10489 Dept. of Argiculture - Pesticide Control Service - Department ...
10489 Dept. of Argiculture - Pesticide Control Service - Department ...
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<strong>10489</strong> <strong>Dept</strong>. <strong>of</strong> <strong>Argiculture</strong> 5/12/2003 12:34 pm Page a<br />
PESTICIDE RESIDUES IN FOOD-2002<br />
__________<br />
BAILE ÁTHA CLIATH:<br />
ARNA FHOILSIÚ AG OIFIG AN tSOLÁTHAIR<br />
__________<br />
Le ceannach díreach ón<br />
OIFIG DHÍOLTA FOILSEACHÁN RIALTAIS,<br />
TEACH SUN ALLIANCE, SRÁID THEACH LAIGHEAN, BAILE ÁTHA CLIATH 2,<br />
nó tríd an bpost ó<br />
FOILSEACHÁIN RIALTAIS, AN RANNÓG POST-TRÁCHTA,<br />
51 FAICHE STIABHNA, BAILE ÁTHA CLIATH 2.<br />
(Teil: 01-647 6834/35/36/37; Fax: 01-647 6843)<br />
nó trí aon díoltóir leabhar.<br />
__________<br />
DUBLIN<br />
PUBLISHED BY THE STATIONERY OFFICE<br />
__________<br />
To be purchased directly from the<br />
GOVERNMENT PUBLICATIONS SALE OFFICE,<br />
SUN ALLIANCE HOUSE, MOLESWORTH STREET, DUBLIN 2,<br />
or by mail order from<br />
GOVERNMENT PUBLICATIONS, POSTAL TRADE SECTION,<br />
51 ST. STEPHEN’S GREEN, DUBLIN 2.<br />
(Tel: 01-647 6834/35/36/37; Fax: 01-647 6843)<br />
or through any bookseller.<br />
Price: €7<br />
DEPARTMENT OF AGRICULTURE & FOOD<br />
PESTICIDE CONTROL SERVICE — AUGUST 2003.<br />
ABBOTSTOWN, CASTLEKNOCK, DUBLIN 15, IRELAND
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- b -
<strong>10489</strong> <strong>Dept</strong>. <strong>of</strong> <strong>Argiculture</strong> 5/12/2003 12:34 pm Page c<br />
© Government <strong>of</strong> Ireland 2003<br />
ISBN (To be supplied)<br />
500 9/03 Brunswick Press Ltd. Spl. (<strong>10489</strong>)
<strong>10489</strong> <strong>Dept</strong>. <strong>of</strong> <strong>Argiculture</strong> 5/12/2003 12:34 pm Page i<br />
FOREWORD<br />
I am very pleased to present the results <strong>of</strong> the national<br />
monitoring programme for pesticide residues in food<br />
carried out in 2002 by the <strong>Department</strong>’s <strong>Pesticide</strong><br />
<strong>Control</strong> <strong>Service</strong> under the terms <strong>of</strong> the service contract<br />
with the Food Safety Authority <strong>of</strong> Ireland. Food safety<br />
is <strong>of</strong> great importance to all involved in the food chain<br />
and, through the residue monitoring programme,<br />
consumers can be assured that they are not exposed to<br />
unacceptable pesticide residue levels and that only<br />
authorized pesticides are applied to food crops. Samples<br />
<strong>of</strong> food are analysed in the <strong>Department</strong>’s <strong>Pesticide</strong><br />
<strong>Control</strong> Laboratory that is accredited by the National<br />
Accreditation Board (NAB) <strong>of</strong> Ireland to the ISO 17025<br />
standard for the analysis <strong>of</strong> selected pesticide residues<br />
in food <strong>of</strong> plant and <strong>of</strong> animal origin. The accreditation<br />
status <strong>of</strong> the laboratory will continue to be extended to<br />
cover additional pesticides and food commodities. This report provides detailed information on the<br />
results <strong>of</strong> the sampling and analysis programmes for residual traces <strong>of</strong> pesticides in both imported and<br />
domestic food for 2002.<br />
Noel Treacy TD<br />
Minister <strong>of</strong> State at the <strong>Department</strong><br />
<strong>of</strong> Agriculture and Food<br />
i
<strong>10489</strong> <strong>Dept</strong>. <strong>of</strong> <strong>Argiculture</strong> 5/12/2003 12:34 pm Page ii<br />
ii
<strong>10489</strong> <strong>Dept</strong>. <strong>of</strong> <strong>Argiculture</strong> 5/12/2003 12:34 pm Page iii<br />
CONTENTS<br />
Page No.<br />
Foreword<br />
i<br />
List <strong>of</strong> Tables<br />
vi<br />
Introduction 1<br />
Monitoring Programmes 1<br />
A Sampling <strong>of</strong> fruit and vegetables 2<br />
B Sampling <strong>of</strong> cereals 3<br />
C Sampling <strong>of</strong> food <strong>of</strong> animal origin 3<br />
D Samples <strong>of</strong> miscellaneous products 3<br />
E Analytical procedures 3<br />
Quality Assurance 4<br />
Results and Discussion 5<br />
A Fruit and Vegetables 5<br />
i Routine monitoring programme 5<br />
ii Targeted sampling programme 23<br />
iii<br />
Sampling <strong>of</strong> vegetable crops produced by growers<br />
participating in the An Bord Glas Quality Programme 24<br />
B Cereals 25<br />
i Routine monitoring programme 25<br />
ii Targeted sampling programme 25<br />
iii
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CONTENTS Continued<br />
Page No.<br />
C Food <strong>of</strong> animal origin 26<br />
1 Bovine meat 26<br />
i Routine monitoring programme 26<br />
ii Targeted sampling programme 27<br />
2 Ovine meat 27<br />
i Routine monitoring programme 27<br />
ii Targeted sampling programme 27<br />
3 Porcine meat 28<br />
i Routine monitoring programme 28<br />
ii Targeted sampling programme 28<br />
4 Dairy products 28<br />
i Routine monitoring programme 28<br />
ii Targeted sampling programme 28<br />
5 Venison 28<br />
6 Poultry 29<br />
7 Eggs 29<br />
8 Honey 29<br />
D Miscellaneous and complaint samples 30<br />
Conclusions 31<br />
A Introduction 31<br />
B Routine monitoring programme 31<br />
C Violation investigation programme 36<br />
D Concluding remarks 37<br />
Annex I<br />
Regulations fixing maximum levels for pesticide residues<br />
in agricultural produce 38<br />
iv
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CONTENTS Continued<br />
Page No.<br />
Annex II<br />
EC Directives fixing maximum levels for pesticide<br />
residues in agricultural produce 40<br />
Annex III Glossary <strong>of</strong> terms 43<br />
Annex IV<br />
Analytical methods and procedures employed for the<br />
determination <strong>of</strong> pesticide residues in foodstuffs 45<br />
Annex V <strong>Pesticide</strong>s determined in fruit, vegetables, cereals and honey 46<br />
Annex VI <strong>Pesticide</strong>s determined in bovine, porcine, ovine, poultry and venison kidney fat 48<br />
Annex VII <strong>Pesticide</strong>s determined in milk 50<br />
Annex VIII<br />
Summary <strong>of</strong> the results <strong>of</strong> the quality assurance<br />
programme for analytical methods 52<br />
1 Fruit and vegetables 52<br />
2 Cereals 56<br />
3 Food <strong>of</strong> animal origin 60<br />
i Meat fat 60<br />
ii Dairy products 63<br />
iii Poultry products 65<br />
Annex IX <strong>Pesticide</strong>s determined in vegetable samples analysed 68<br />
by Analytical Consultants on behalf <strong>of</strong> An Bord Glas<br />
Annex X<br />
Summary <strong>of</strong> the results <strong>of</strong> the analysis <strong>of</strong> Irish<br />
vegetables sampled by An Bord Glas 71<br />
v
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LIST OF TAzBLES<br />
Page No.<br />
Table 1<br />
Fruit and vegetable samples analysed for their pesticide<br />
residues content in 2002 8<br />
Table 2 <strong>Pesticide</strong> residues detected in fruit and vegetables in 2002 10<br />
Table 3<br />
<strong>Pesticide</strong> residues detected in targeted samples <strong>of</strong> fruit and<br />
vegetables in 2002 24<br />
Table 4<br />
Cereal samples analysed for their pesticide residue content<br />
in 2002 25<br />
Table 5 <strong>Pesticide</strong> residues detected in cereals in 2002 25<br />
Table 6 <strong>Pesticide</strong> residues detected in bovine kidney fat in 2002 26<br />
Table 7 <strong>Pesticide</strong> residues detected in ovine kidney fat in 2002 27<br />
Table 8 <strong>Pesticide</strong> residues detected in porcine kidney fat in 2002 28<br />
Table 9 <strong>Pesticide</strong> residues detected in poultry fat in 2002 29<br />
Table 10 <strong>Pesticide</strong> residues detected in miscellaneous and complaint samples 2002 30<br />
Table 11<br />
Samples with pesticide residues exceeding Maximum Residue<br />
Limits (MRLs) in 2002 32<br />
Table 12<br />
Relationship between excessive residue levels found and the<br />
ADI and ARfD levels for humans 36<br />
vi
<strong>10489</strong> <strong>Dept</strong>. <strong>of</strong> <strong>Argiculture</strong> 5/12/2003 12:34 pm Page 1<br />
INTRODUCTION<br />
The monitoring programme for pesticide residues in food undertaken by the <strong>Department</strong><br />
<strong>of</strong> Agriculture and Food through its <strong>Pesticide</strong> <strong>Control</strong> <strong>Service</strong>, at Abbotstown, Dublin 15,<br />
is aimed at ensuring that consumers are not exposed to unacceptable pesticide residue<br />
levels. In addition, it is aimed at ensuring that authorised pesticides are correctly applied<br />
to food crops and that the use <strong>of</strong> unauthorised pesticides is detected.<br />
In accordance with the contractual arrangements between the <strong>Department</strong> and the Food<br />
Safety Authority <strong>of</strong> Ireland (FSAI) 1 , the annual monitoring programme carried out by the<br />
<strong>Pesticide</strong> <strong>Control</strong> <strong>Service</strong> has since 5 July 1999, been agreed with and conducted on behalf<br />
<strong>of</strong> the FSAI.<br />
The monitoring programme in place involves the sampling <strong>of</strong> produce <strong>of</strong> imported and <strong>of</strong><br />
domestic origin. The analytical part <strong>of</strong> the monitoring programme reflects pesticide usage<br />
patterns both in Ireland and abroad. Some 800 active substances are registered for use in<br />
plant protection products around the world, <strong>of</strong> which between 300 and 400 are in common<br />
use.<br />
<strong>Pesticide</strong> residue levels in treated crops and in animal products are regulated through the<br />
establishment <strong>of</strong> Maximum Residue Limits (MRLs). Currently MRLs have been<br />
established in Ireland for some 150 pesticides in fruit and vegetables (including tea), some<br />
130 pesticides in cereals and some 100 pesticides in food <strong>of</strong> animal origin, reflecting<br />
relevant European Union (EU) legislation. Following the adoption <strong>of</strong> changes in EU<br />
procedures for setting MRLs, more rapid progress is being achieved than heret<strong>of</strong>ore in<br />
their elaboration 2, 3 .<br />
When MRLs are exceeded, <strong>of</strong>ficers <strong>of</strong> the <strong>Pesticide</strong> <strong>Control</strong> <strong>Service</strong> can remove the<br />
produce concerned from the market and destroy it at the owner’s expense. The Minister<br />
may also take prosecutions. Where warranted, a “Rapid Alert” 4 can be issued by the FSAI.<br />
A Rapid Alert is issued when residues detected in food are considered to be harmful to the<br />
consumer.<br />
Explanations <strong>of</strong> the various technical terms used in this report are provided in a glossary<br />
at the end <strong>of</strong> this report (Annex III).<br />
MONITORING PROGRAMMES<br />
Monitoring programmes are in place for the three different food groups for which MRLs<br />
have been established, food <strong>of</strong> plant origin (including fruit and vegetables), cereals and<br />
food <strong>of</strong> animal origin (meat, milk, and dairy produce). Officers <strong>of</strong> the <strong>Pesticide</strong> <strong>Control</strong><br />
<strong>Service</strong> carry out the sampling <strong>of</strong> food <strong>of</strong> plant origin and cereals, while members <strong>of</strong> the<br />
Dairy Science and Veterinary Inspectorates <strong>of</strong> the <strong>Department</strong> <strong>of</strong> Agriculture and Food<br />
carry out the sampling <strong>of</strong> food <strong>of</strong> animal origin.<br />
1 <strong>Service</strong> Contract between the Food Safety Authority <strong>of</strong> Ireland and the <strong>Department</strong> <strong>of</strong> Agriculture, Food and Rural Development dated 5th<br />
day <strong>of</strong> July 1999.<br />
2 Council Directive (91/414/EEC) <strong>of</strong> 15 July 1991, concerning the placing <strong>of</strong> plant protection products on the market, OJ No. L 230/1 <strong>of</strong><br />
19.8.1991.<br />
3 Council Directive (97/41) <strong>of</strong> 25 June 1997 amending Directives 76/895/EEC, 86/362/EEC, 86/363/EEC and 90/642/EEC relating to the<br />
fixing <strong>of</strong> maximum levels for pesticide residues in and on, respectively, fruit and vegetables, cereals, foodstuffs <strong>of</strong> animal origin, and certain<br />
products <strong>of</strong> plant origin, including fruit and vegetables OJ No. L 184 <strong>of</strong> 12.7.1997.<br />
4 Regulation (EC) No. 178/2002 <strong>of</strong> the European Parliament and <strong>of</strong> the Council <strong>of</strong> 28th <strong>of</strong> January 2002.<br />
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The monitoring programme for 2002, agreed with the FSAI, takes into consideration -<br />
i the programme recommended by the European Commission 5 ,<br />
ii<br />
iii<br />
dietary intake patterns <strong>of</strong> Irish consumers 6 , and<br />
the residue pr<strong>of</strong>ile <strong>of</strong> commodities as established from the results <strong>of</strong> the<br />
monitoring programme in previous years.<br />
The total number <strong>of</strong> samples analysed at 965, reflected the capacity <strong>of</strong> the laboratory to<br />
process samples submitted and was an increase <strong>of</strong> some 50% over the year 2001. The<br />
capacity <strong>of</strong> the laboratory in 2002 to analyse samples for pesticide residues continues to<br />
reflect the deployment <strong>of</strong> new staff that were recruited to the laboratory towards the end<br />
<strong>of</strong> 2001 and that are now fully trained in the analysis <strong>of</strong> samples for pesticide residues.<br />
Significant resources are deployed within the laboratory to maintain systems and<br />
procedures to support NAB 7 accreditation <strong>of</strong> the laboratory in accordance with the<br />
requirement <strong>of</strong> Council Directive 89/397/EEC 8 and Council Directive 93/99/EEC 9 . The<br />
laboratory is currently accredited to ISO 17025 standard for the analysis <strong>of</strong> pesticide<br />
residues in both food <strong>of</strong> plant and <strong>of</strong> animal origin using gas chromatographic techniques.<br />
The scope <strong>of</strong> this accreditation will continue to be extended in 2003 to include additional<br />
pesticides and food commodities.<br />
The monitoring programme is the prime means <strong>of</strong> ensuring that pesticides are used in<br />
accordance with Good Agricultural Practice. The monitoring programme is essential to<br />
the elimination <strong>of</strong> abuses in the use <strong>of</strong> pesticides, such as use <strong>of</strong> excessive dose rates,<br />
failure to respect the minimum periods specified between last application and harvest (i.e.<br />
pre-harvest intervals) and use for purposes for which they are not authorised (i.e. illegal<br />
uses). When used in accordance with Good Agricultural Practice unacceptable levels <strong>of</strong><br />
pesticide residues should not occur in treated produce.<br />
In accordance with the European Communities (Prohibition <strong>of</strong> Certain Active Substances<br />
in Plant Protection Products) Regulations, 1981 to 1990, the marketing and use <strong>of</strong> certain<br />
plant protection products are prohibited because <strong>of</strong> risks to human health or the<br />
environment associated with their use. The residue monitoring programme serves as an<br />
indicator <strong>of</strong> the level <strong>of</strong> compliance with those provisions.<br />
A<br />
SAMPLING OF FRUIT AND VEGETABLES<br />
Routine sampling is biased in favour <strong>of</strong> food commodities that are <strong>of</strong> greater dietary<br />
importance. Within particular commodity groups, samples are taken at random. As part <strong>of</strong><br />
the violation investigation programme, fruit and vegetables <strong>of</strong> specific origin are targeted<br />
for further special attention, where residues at levels in excess <strong>of</strong> MRLs have been found<br />
following routine sampling. When a crop is encountered which is targeted for statutory<br />
sampling, whether as a result <strong>of</strong> information generated through routine monitoring or<br />
following a Food Alert issued by the FSAI or following a Rapid Alert notification to the<br />
5 Commission Recommendation <strong>of</strong> 27 December 2001, concerning a co-ordinated Community monitoring programme for 2002 to ensure<br />
compliance with maximum levels <strong>of</strong> pesticide residues in and on cereals and certain other products <strong>of</strong> plant origin (2002/1/EC) OJ No L<br />
2/8 <strong>of</strong> 4th <strong>of</strong> January 2002.<br />
6 IUNA, North South Food Consumption Database, 2001.<br />
7 National Accreditation Board.<br />
8 Council Directive <strong>of</strong> 14 June 1989 on the <strong>of</strong>ficial control <strong>of</strong> foodstuffs. (89/397/EEC) OJ No. L 186 <strong>of</strong> 30.6.1989.<br />
9 Council Directive <strong>of</strong> 29 October 1993 on the subject <strong>of</strong> additional measures concerning the <strong>of</strong>ficial control <strong>of</strong> foodstuffs. (93/99/EEC)OJ<br />
No. L 290 <strong>of</strong> 24.11.1993.<br />
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FSAI from the EU Commission, the sampled lot is seized pending analysis. Since<br />
monitoring <strong>of</strong> pesticide residues commenced in 1982, six repeat violations in targeted<br />
crops have been encountered 10 – one <strong>of</strong> which led to prosecution and conviction. Both<br />
domestic and imported produce are sampled, primarily at wholesale level. This approach<br />
ensures that samples taken are representative <strong>of</strong> consumption patterns and allows action to<br />
be taken, where necessary, prior to distribution.<br />
B<br />
SAMPLING OF CEREALS<br />
The main concern with respect to cereals relates to residues that arise as a result <strong>of</strong> postharvest<br />
application <strong>of</strong> plant protection products. The current sampling programme for<br />
cereals is confined, for practical reasons, to the sampling and analysis <strong>of</strong> grain used in the<br />
milling, malting and breakfast cereal industries. Cereals and cereal products <strong>of</strong> both<br />
domestic and imported origin are sampled on a random basis, at point <strong>of</strong> assembly or<br />
storage. Samples analysed are taken at random by authorised <strong>of</strong>ficers <strong>of</strong> the <strong>Pesticide</strong><br />
<strong>Control</strong> <strong>Service</strong>.<br />
C<br />
SAMPLING OF FOOD OF ANIMAL ORIGIN<br />
Random samples <strong>of</strong> bovine, porcine, ovine, poultry and venison fat are taken at a range <strong>of</strong><br />
meat plants around the country. Dairy produce is sampled at production plants or points <strong>of</strong><br />
assembly. The samples analysed relate only to domestic produce. The meat samples<br />
analysed are from individual animals. Each dairy produce sample taken is representative<br />
<strong>of</strong> a particular bulk consignment. Members <strong>of</strong> the Dairy Science and Veterinary<br />
Inspectorates <strong>of</strong> the <strong>Department</strong> <strong>of</strong> Agriculture and Food carry out the sampling <strong>of</strong> meat<br />
and dairy produce.<br />
D<br />
SAMPLES OF MISCELLANEOUS PRODUCTS<br />
Complaint or suspect samples are submitted from time to time for analysis by other<br />
<strong>Service</strong>s <strong>of</strong> the <strong>Department</strong> <strong>of</strong> Agriculture and Food, other State <strong>Service</strong>s, Local<br />
Authorities, concerned consumers and other interested parties.<br />
E<br />
ANALYTICAL PROCEDURES<br />
The methodologies used in the analysis <strong>of</strong> the different food samples involve -<br />
i homogenisation <strong>of</strong> samples,<br />
ii extraction <strong>of</strong> the samples into a suitable organic solvent,<br />
iii clean-up <strong>of</strong> the solvent extract using chromatographic techniques, and<br />
iv analysis <strong>of</strong> the cleaned up extract with capillary GC and HPLC instrumentation,<br />
using specific detectors and GC-mass spectrometry.<br />
The methods used in most cases are multi-residue in nature, an approach that facilitates the<br />
maximisation <strong>of</strong> laboratory output. The detection and confirmation <strong>of</strong> the presence <strong>of</strong><br />
residues in food samples depends on the use <strong>of</strong> chromatography columns <strong>of</strong> different<br />
polarity. Quantitative determinations are made by -<br />
10 1994, 1995 & 1996 <strong>Pesticide</strong> Residues in Food, 1998, 1999, 2000 and 2001 <strong>Pesticide</strong> Residues in Food, <strong>Department</strong> <strong>of</strong> Agriculture, Food<br />
and Rural Development, <strong>Pesticide</strong> <strong>Control</strong> <strong>Service</strong>, Dublin, Ireland. Published by the Stationary Office Available from the Government<br />
Publications Sale Office, Sun Alliance House, Molesworth Street, Dublin 2.<br />
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i(i)<br />
(ii)<br />
comparison with external standards, and<br />
in the case <strong>of</strong> fruit and vegetables, use <strong>of</strong> a 3-point calibration curve <strong>of</strong> matrixmatched<br />
standards.<br />
Due to the wide variety <strong>of</strong> fruit and vegetables analysed, it is not practical to use all<br />
matrices. In 2002, 10 different matrices including peas, beans, carrots, tomatoes,<br />
cucumbers, kiwi, celery, aubergine, potatoes and mushroom were used for the preparation<br />
<strong>of</strong> matrix matched standards when quantifying residues in routine samples. In the case <strong>of</strong><br />
targeted statutory samples, quantitative determinations were made using, where possible,<br />
the matrix <strong>of</strong> the commodity analysed.<br />
In addition to the analysis <strong>of</strong> samples using gas chromatography with specific detectors<br />
confirmation <strong>of</strong> the identity <strong>of</strong> pesticide residues using mass spectrometry is now included<br />
as part <strong>of</strong> the analytical process where pesticides are amenable to this analysis.<br />
Specific rather than multi-residue methods <strong>of</strong> analysis are used for the detection <strong>of</strong><br />
benzimidazole residues. The method <strong>of</strong> analysis for the benzimidazole pesticides was not<br />
an accredited method <strong>of</strong> analysis in 2002.<br />
Further details <strong>of</strong> the methods employed are provided in Annex IV.<br />
QUALITY ASSURANCE.<br />
Routine quality assurance procedures within the laboratory have become much more<br />
involved following the accreditation <strong>of</strong> the laboratory. In 2002 in excess <strong>of</strong> 250 samples<br />
were used in recovery studies to verify that the analytical methods were being used<br />
correctly in the laboratory. This work involved:<br />
i<br />
ii<br />
iii<br />
iv<br />
v<br />
vi<br />
vii<br />
All animal fat samples being spiked with Aldrin as an internal standard.<br />
Each batch <strong>of</strong> 10 samples <strong>of</strong> food <strong>of</strong> animal origin being spiked with reference<br />
pesticide mixtures containing 9 organochlorine pesticides, 9 organophosphorous<br />
pesticides and a PCB mixture containing 7 PCB congeners.<br />
For every 40 samples <strong>of</strong> food <strong>of</strong> animal origin analysed one sample being spiked with<br />
one <strong>of</strong> 3 mixtures <strong>of</strong> organochlorine pesticides containing a total <strong>of</strong> 13 pesticides.<br />
This recovery work is carried out on a rolling basis.<br />
For every 40 samples <strong>of</strong> food <strong>of</strong> animal origin analysed one sample being spiked with<br />
one <strong>of</strong> 3 mixtures <strong>of</strong> organophosphorous pesticides containing a total <strong>of</strong> 15 pesticides.<br />
This recovery work is carried out on a rolling basis.<br />
Each batch <strong>of</strong> 10 dairy product samples being spiked with reference pesticide<br />
mixtures containing 10 organochlorine pesticides, 9 organophosphorous pesticides<br />
and a PCB mixture containing 7 PCB congeners.<br />
For every 40 samples <strong>of</strong> dairy produce analysed one sample being spiked with one <strong>of</strong><br />
3 mixtures <strong>of</strong> organochlorine pesticides containing a total <strong>of</strong> 13 pesticides. This<br />
recovery work is carried out on a rolling basis.<br />
For every 40 samples <strong>of</strong> dairy produce analysed one sample being spiked with one <strong>of</strong><br />
3 mixtures <strong>of</strong> organophosphorous pesticides containing a total <strong>of</strong> 15 pesticides. This<br />
recovery work is carried out on a rolling basis.<br />
viii Each batch <strong>of</strong> 10 cereal samples being spiked with reference pesticide mixtures<br />
containing 14 organochlorine pesticides and 14 organophosphorous pesticides.<br />
ix For every 50 samples <strong>of</strong> cereals analysed one sample being spiked with one <strong>of</strong> 4<br />
mixtures <strong>of</strong> organochlorine pesticides containing a total <strong>of</strong> 32 pesticides. This<br />
recovery work is carried out on a rolling basis.<br />
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x For every 50 samples <strong>of</strong> cereals analysed one sample being spiked with one <strong>of</strong> 5<br />
mixtures <strong>of</strong> organophosphorous pesticides containing a total <strong>of</strong> 27 pesticides. This<br />
recovery work is carried out on a rolling basis.<br />
xi Each batch <strong>of</strong> 10 fruit and vegetable samples being spiked with reference pesticide<br />
mixtures containing 14 organochlorine pesticides and 13 organophosphorous<br />
xii<br />
pesticides.<br />
For every 50 samples <strong>of</strong> fruit and vegetables analysed one sample being spiked with<br />
one <strong>of</strong> 4 mixtures <strong>of</strong> organochlorine pesticides containing a total <strong>of</strong> 32 pesticides.<br />
This recovery work is carried out on a rolling basis.<br />
xiii For every 50 samples <strong>of</strong> fruit and vegetables analysed one sample being spiked with<br />
one <strong>of</strong> 5 mixtures <strong>of</strong> organophosphorous pesticides containing a total <strong>of</strong> 27 pesticides.<br />
This recovery work is carried out on a rolling basis.<br />
Recovery studies were carried out using at least one ‘reference pesticide standard mixture’<br />
representative <strong>of</strong> the range <strong>of</strong> pesticides analysed by the laboratory. These studies were<br />
generally carried out at concentrations equivalent to the lowest calibration level (LCL) or<br />
at 10 times the LCL for the pesticides concerned. Recovery levels are considered<br />
acceptable for routine monitoring samples if they are in the range <strong>of</strong> 60 – 140%.<br />
In addition to the in-house quality assurance programme, the laboratory participated in<br />
seven rounds <strong>of</strong> pr<strong>of</strong>iciency tests during 2002 that were organised and run by the Food<br />
Analysis Performance Assessment Scheme (FAPAS) 11 . The pr<strong>of</strong>iciency testing<br />
undertaken involved the analysis <strong>of</strong> samples <strong>of</strong> apple, orange, carrot, vegetable oil, and<br />
lettuce, spiked with pesticide residues. Up to 80 laboratories participated in the scheme<br />
and the results for the <strong>Pesticide</strong> <strong>Control</strong> <strong>Service</strong> were satisfactory. The laboratory also<br />
participated in a pr<strong>of</strong>iciency study organised on behalf <strong>of</strong> the EU Commission which<br />
involved analysis <strong>of</strong> a sample <strong>of</strong> oranges containing up to 15 different pesticides. 117<br />
laboratories participated in this study from each <strong>of</strong> the EU and accession countries. The<br />
results obtained by the <strong>Pesticide</strong> <strong>Control</strong> Laboratory in these pr<strong>of</strong>iciency studies were<br />
acceptable in all cases.<br />
The methods <strong>of</strong> analysis currently employed by the <strong>Pesticide</strong> <strong>Control</strong> <strong>Service</strong> do not have<br />
the capacity to detect all <strong>of</strong> the pesticides for which MRLs have been established in fruit<br />
and vegetables and in cereals. It is necessary to continue to expand the analytical capacity<br />
<strong>of</strong> the laboratory by increasing the number <strong>of</strong> pesticides included in the analytical screen.<br />
This will be achieved by further developing the scope <strong>of</strong> the current analytical methods<br />
used within the laboratory and by the introduction and use <strong>of</strong> new analytical methods.<br />
RESULTS AND DISCUSSION<br />
A<br />
i<br />
FRUIT AND VEGETABLES<br />
Routine Monitoring Programme<br />
The results <strong>of</strong> the 2002 monitoring programme are summarised in Table 1 below while the<br />
details on samples which were analysed and found to contain pesticide residues are<br />
presented in Table 2.<br />
11 FAPAS is a registered trade mark <strong>of</strong> the UK <strong>Department</strong> <strong>of</strong> the Environment, Food and Rural Affairs [DEFRA].<br />
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In 2002, some 559 samples <strong>of</strong> 72 different types <strong>of</strong> fruit and vegetables were analysed for<br />
their pesticide residue content, <strong>of</strong> which 18% were <strong>of</strong> domestic origin, and 82% were <strong>of</strong><br />
imported produce or <strong>of</strong> unknown origin. Details are provided in Table 1. Samples were<br />
analysed for residues <strong>of</strong> up to 89 pesticides and metabolites (Annex V). MRLs have been<br />
established for an additional 93 compounds which are not yet included in the monitoring<br />
programme. 52% <strong>of</strong> samples analysed contained detectable quantities <strong>of</strong> pesticide residues<br />
<strong>of</strong> which 4.7% contained residues in excess <strong>of</strong> the MRLs.<br />
Details <strong>of</strong> the residues detected are provided in Table 2. In all, residues <strong>of</strong> 46 different<br />
pesticides were detected in 2002. MRL’s exist for 39 <strong>of</strong> these compounds but have not yet<br />
been set for the remaining 7 pesticides.<br />
Thiabendazole (17.7% <strong>of</strong> samples), carbendazim (10.4% <strong>of</strong> samples), captan (6.4% <strong>of</strong><br />
samples), chlorpyrifos (5.2% <strong>of</strong> samples), methidathion (5% <strong>of</strong> samples), iprodione (4.8%<br />
<strong>of</strong> samples), folpet (4.1% <strong>of</strong> samples), bromopropylate (3.9% <strong>of</strong> samples), tolyfluanid (3%<br />
<strong>of</strong> samples) and chlorothalonil (2.3% <strong>of</strong> samples) were the most commonly detected<br />
pesticides in the routine monitoring programme. Other pesticides detected in samples<br />
analysed were acephate, azinphos-methyl, bifenthrin, binapacryl, chlorfenvinphos,<br />
chlorpyrifos-methyl, cypermethrin, deltamethrin, demeton-S-me-sulphone, diazinon,<br />
dichl<strong>of</strong>luanid, dic<strong>of</strong>ol, dieldrin, dimethoate, endosulfan, fenitrothion, fenvalerate, lambdacyhalothrin,<br />
lindane, malathion, methamidophos, mevinphos, omethoate, parathion,<br />
parathion-methyl, phosalone, phosmet, phosphamidon, procymidone, DDT, propyzamide,<br />
quintozene, tecnazene, tetradifon, tolcophos-methyl and vinclozolin. The frequency <strong>of</strong><br />
detection <strong>of</strong> particular pesticide residues in 2002 is similar to that for 2001 with the<br />
exception that dimethoate was detected on far fewer occasions during 2002 (0.9%) as<br />
opposed to 3.3% in 2001. The reduction in the use <strong>of</strong> dimethoate may be related to EU<br />
decisions to modify the MRL’s for dimethoate during 2002.<br />
Residues <strong>of</strong> thiabendazole were detected mainly in citrus and bananas but were also found<br />
in apples, pears, kumquats, mangoes, and potatoes; residues <strong>of</strong> carbendazim were mainly<br />
detected in citrus, apples, pears and stone fruit but were also detected in grapes,<br />
strawberries, avocado, passion fruit, litchi and courgettes; residues <strong>of</strong> captan were detected<br />
mainly in apples but were also found in pears, apricots, nectarines, peaches, grapes and<br />
strawberries; chlorpyrifos was detected mainly in citrus but was also found in pears,<br />
peaches, plums, grapes and strawberries; methidathion was detected in citrus only;<br />
residues <strong>of</strong> iprodione were found in the widest range <strong>of</strong> crops, being detected in fifteen<br />
different fruit and vegetables [ pome fruit, stone fruit, berries and small fruit, kiwi, passion<br />
fruit, carrots, tomatoes and lettuce] ; folpet was found most commonly in citrus, apples and<br />
pears but was also found in bananas, lettuce and celery; bromopropylate was detected most<br />
frequently in citrus but was also found in apples, red currants and parsnips. ; residues <strong>of</strong><br />
tolyfluanid were found in citrus, apples, strawberries, red currants, figs and tomatoes ;<br />
chlorothalonil was found in strawberries, blueberries, kiwano, papaya, tamarillos,<br />
tomatoes, cucumbers, head cabbage, lettuce, parsley and celery.<br />
In all, some 72 samples (12.9%) contained residues <strong>of</strong> two pesticides, 32 samples (5.7%)<br />
contained residues <strong>of</strong> three pesticides, 13 samples (2.3%) contained residues <strong>of</strong> four<br />
pesticides, 5 samples (0.9%) contained residues <strong>of</strong> five pesticides and 1 sample (0.2%)<br />
contained residues <strong>of</strong> six pesticides.<br />
Twenty six samples <strong>of</strong> fruit and vegetables, from the routine monitoring programme, were<br />
found to contain pesticide residues in excess <strong>of</strong> an MRL. Three <strong>of</strong> these samples were<br />
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produce <strong>of</strong> Irish origin (parsley, strawberry and swede), ten were from other EU countries<br />
and the remaining thirteen were from outside <strong>of</strong> the EU. Of the 102 samples <strong>of</strong> domestic<br />
origin analysed 3 (2.9 %) contained residues in excess <strong>of</strong> an MRL, while in the case <strong>of</strong> the<br />
457 samples <strong>of</strong> imported origin analysed 23 (5 %) contained residues in excess <strong>of</strong> an<br />
MRL. 21 <strong>of</strong> the 26 samples containing pesticide residues that exceeded an MRL involved<br />
MRLs that have been established at the limit <strong>of</strong> determination. Thirteen <strong>of</strong> the samples<br />
found to contain pesticide residues levels in excess <strong>of</strong> MRLs were <strong>of</strong> food commodities<br />
that are <strong>of</strong> limited dietary importance (peach x2, blueberry, red currant, avocado, kiwano,<br />
kumquat, litchi, papaya, passion fruit, tamarillo, parsnip and parsley). The remaining<br />
fourteen samples (grapes x3, strawberries x2, carrots x1, swede x1, pepper x1, lettuce x1,<br />
spinach x2, celery x1 and potatoes x1) which contained residues in excess <strong>of</strong> an MRL are<br />
more widely consumed. The calculated dietary intake for the pesticides found in these<br />
crops is presented in Table 12. The estimated intake figures indicate that the residues<br />
present do not pose a threat to the health <strong>of</strong> Irish adult consumers.<br />
In the case <strong>of</strong> pesticides which are not used in the European Union but which may be used<br />
in other countries, MRLs are generally established at the limit <strong>of</strong> determination (LOD),<br />
reflecting non use within the EU. The occurrence <strong>of</strong> residues in excess <strong>of</strong> such MRLs in<br />
imported produce (i.e. they are technical breaches <strong>of</strong> MRLs), in most cases, do not present<br />
risks for consumers. Such anomalies should be resolved in due course by the World Trade<br />
Organisation (WTO) and by continuing co-operation between the EU and producer groups<br />
in third countries. In 2002 twelve <strong>of</strong> the thirteen MRL exceedances in produce imported<br />
from outside the EU related to situations where the EU MRL was established at the LOD.<br />
There were nine instances in 2002 <strong>of</strong> the occurrence <strong>of</strong> residues, in excess <strong>of</strong> the MRL,<br />
following unauthorised use <strong>of</strong> pesticides in Ireland and in other EU countries. The residues<br />
detected may have resulted in some cases from use on crops for which the particular<br />
pesticides are not authorised and in other cases from improper use <strong>of</strong> the pesticide.<br />
Improper use can involve non-compliance with the pre-harvest intervals specified, use <strong>of</strong><br />
excessive rates or numbers <strong>of</strong> applications and/or the use <strong>of</strong> an inappropriate method <strong>of</strong><br />
application. The instances <strong>of</strong> such excessive residues that did not involve risks for<br />
consumers, were: –<br />
■ dic<strong>of</strong>ol in peaches (Spain)<br />
■ carbendazim in strawberry (Ireland)*<br />
■ endosulfan in carrot (Spain)<br />
■ chlorpyrifos in swedes (Ireland)*<br />
■ chlorothalonil in lettuce (Spain)<br />
■ chlorpyrifos in spinach (Spain)<br />
■ chlorpyrifos in parsley (Ireland)<br />
■ cypermethrin in celery (Spain)<br />
■ acephate in potato (Italy).<br />
* In these instances the residues arose from the use <strong>of</strong> an old plant protection product<br />
whose label did not reflect the changed MRL and associated change in GAP.<br />
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Table 1: Fruit and vegetables samples analysed for their pesticide residue content in 2002<br />
Commodity No. No. No. Residues<br />
Samples Domestic Imported<br />
Analysed Samples Samples > MRL ≤ MRL ND<br />
Apple 67 67 47 20<br />
Apricot 3 3 2 1<br />
Asparagus 2 2 2<br />
Aubergine 3 3 3<br />
Avocado 4 4 1 3<br />
Banana 12 12 11 1<br />
Bean+pod 12 12 2 10<br />
Beansprout 1 1 1<br />
Blackberry 3 3 1 2<br />
Blackcurrant 2 2 2<br />
Blueberry 3 1 2 1 2<br />
Broccoli 2 2 1 1<br />
Cabbage 7 4 3 2 5<br />
Carrot 26 9 17 1 7 18<br />
Cauliflower 3 2 1 3<br />
Celery 15 6 9 1 6 8<br />
Cherry 2 2 2 0<br />
Clementine 31 31 26 5<br />
Courgette 5 1 4 1 4<br />
Cranberry 1 1 1<br />
Cucumber 11 8 3 2 9<br />
Fennel 1 1 1 0<br />
Fig 1 1 1 0<br />
Grape 16 16 3 7 6<br />
Grapefruit 11 11 6 5<br />
Kiwano 2 2 1 0 1<br />
Kiwi 11 11 4 7<br />
Kumquat 1 1 1 0 0<br />
Leek 1 1 1<br />
Lemon 4 4 3 1<br />
Lemongrass 1 1 1 0<br />
Lettuce 23 11 12 1 6 16<br />
Lime 1 1 1<br />
Litchi 3 3 1 2<br />
Mandarin 2 2 2 0<br />
Mandora 3 3 3 0<br />
Mango 6 6 2 4<br />
Melon 6 6 3 3<br />
Mineola 2 2 2 0<br />
Mushroom 6 5 1 1 5<br />
Nectarine 13 13 4 9<br />
Onion 1 1 1 0<br />
Orange 36 36 32 4<br />
Papaya 2 2 1 1<br />
Parlsey 5 4 1 1 3 1<br />
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Table 1:<br />
Continued<br />
Commodity No. No. No. Residues<br />
Samples Domestic Imported<br />
Analysed Samples Samples > MRL ≤ MRL ND<br />
Parsnip 10 7 3 1 7 2<br />
Passion Fruit 2 2 1 1<br />
Peach 8 8 2 4 2<br />
Pear 24 24 12 12<br />
Peas (+pod) 1 1 1<br />
Pepper 10 10 1 2 7<br />
Physalis 1 1 1<br />
Pineapple 2 2 2<br />
Plum 12 12 8 4<br />
Potato 25 12 13 1 3 21<br />
Radish 1 1 1<br />
Raspberry 7 1 6 1 6<br />
Redcurrant 1 1 1 0<br />
Rhubarb 1 1 1<br />
Rocket 1 1 1<br />
Satsuma 20 20 20 0<br />
Spinach 12 12 2 1 9<br />
Spring onion 1 1 1<br />
Star Fruit 2 2 2<br />
Strawberry 16 11 5 2 7 7<br />
Swede 7 7 1 1 5<br />
Sweet potato 1 1 1<br />
Sweetcorn 1 1 1<br />
Tangarine 1 1 1 0<br />
Tomato 16 8 8 4 12<br />
Tamarillo 2 2 1 1<br />
Turnip 1 1 1<br />
TOTAL 559 102 457 26 263 270<br />
ND = no pesticide residue detected.<br />
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Table 2: <strong>Pesticide</strong> residues detected in fruit and vegetables in 2002<br />
Sample Country <strong>of</strong> Residue detected Residue MRL<br />
number origin (mg/kg) (mg/kg)<br />
1. Fruit 1.1 Citrus Fruit 1.1.2. Clementines<br />
61525 Spain chlorpyrifos 0.12 2<br />
dic<strong>of</strong>ol 0.09 2<br />
61526 Spain dic<strong>of</strong>ol 0.08 2<br />
chlorpyrifos 0.11 2<br />
61529 Spain thiabendazole 4.7 5<br />
dic<strong>of</strong>ol 0.07 2<br />
methidathion 0.06 2<br />
61549 Morocco methidathion 0.47 2<br />
61627 Morocco methidathion 0.35 2<br />
61784 S. Africa thiabendazole 0.87 5<br />
61815 S. Africa folpet 0.01 0.1<br />
61830 S. Africa bromopropylate 0.45 5<br />
61854 S. Africa bromopropylate 0.05 5<br />
61876 S. Africa thiabendazole 0.18 5<br />
61888 S. Africa methidathion 0.12 2<br />
61914 S. Africa thiabendazole 0.39 5<br />
carbendazim 0.39 5<br />
61926 S. Africa folpet 0.02 0.1<br />
methidathion 0.16 2<br />
bromopropylate 0.04 5<br />
61955 S. Africa methidathion 0.46 2<br />
thiabendazole 1.4 5<br />
61981 Chile chlorpyrifos 0.24 2<br />
thiabendazole 3.3 5<br />
61986 S. Africa carbendazim 0.46 5<br />
thiabendazole 0.26 5<br />
61989 S. Africa carbendazim 0.43 5<br />
methidathion 0.84 2<br />
tetradifon 0.06 No MRL<br />
malathion 0.06 2<br />
thiabendazole 0.29 5<br />
61991 S. Africa methidathion 0.03 2<br />
62004 Canary Islands thiabendazole 0.25 5<br />
62009 S. Africa bromopropylate 0.09 5<br />
thiabendazole 1.6 5<br />
carbendazim 0.46 5<br />
malathion 0.07 2<br />
62033 Chile thiabendazole 0.85 5<br />
chlorpyrifos 0.11 2<br />
chlorpyrifos-me 0.03 1<br />
62034 Chile thiabendazole 3.1 5<br />
chlorpyrifos 0.12 2<br />
62044 Chile thiabendazole 0.27 5<br />
62051 S. Africa thiabendazole 1.3 5<br />
chlorpyrifos 0.07 2<br />
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Table 2:<br />
Continued<br />
Sample Country <strong>of</strong> Residue detected Residue MRL<br />
number origin (mg/kg) (mg/kg)<br />
62083 Spain folpet 0.06 0.1<br />
62083 Spain tolyfluanid 0.03 No MRL<br />
62083 Spain thiabendazole 3.1 5<br />
62106 Spain thiabendazole 4.0 5<br />
chlorpyrifos 0.20 2<br />
malathion 0.29 2<br />
methidathion 0.08 2<br />
dic<strong>of</strong>ol 0.04 2<br />
1.1.3. Grapefruit<br />
61528 Cyprus bromopropylate 0.67 5<br />
thiabendazole 0.86 5<br />
chlorpyrifos 0.23 0.3<br />
61673 Turkey thiabendazole 1.8 5<br />
chlorpyrifos 0.24 0.3<br />
61708 Turkey chlorpyrifos 0.05 0.3<br />
tetradifon 0.08 No MRL<br />
thiabendazole 0.14 5<br />
61786 Cyprus bromopropylate 0.72 5<br />
tetradifon 0.05 No MRL<br />
chlorpyrifos 0.03 0.3<br />
61828 Greece Bromopropylate 0.13 5<br />
chlorpyrifos 0.06 0.3<br />
thiabendazole 3.3 5<br />
malathion 0.40 2<br />
tetradifon 0.07 No MRL<br />
62081 Cuba bromopropylate 0.04 5<br />
62081 Cuba thiabendazole 3.3 5<br />
1.1.4. Lemons<br />
61866 Spain carbendazim 0.29 5<br />
tolyfluanid 0.01 No MRL<br />
thiabendazole 4.5 5<br />
61906 Spain tolyfluanid 0.08 No MRL<br />
methidathion 0.24 2<br />
62058 S. Africa tolyfluanid 0.04 No MRL<br />
methidathion 0.04 2<br />
bromopropylate 0.23 5<br />
folpet 0.04 0.1<br />
1.1.6. Mandarins<br />
61957 Argentina thiabendazole 3.6 5<br />
62085 Argentina thiabendazole 0.21 5<br />
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Table 2:<br />
Continued<br />
Sample Country <strong>of</strong> Residue detected Residue MRL<br />
number origin (mg/kg) (mg/kg)<br />
1.1.7. Mandora<br />
61636 Cyprus methidathion 0.40 2<br />
thiabendazole 2.5 5<br />
malathion 0.10 2<br />
bromopropylate 0.17 5<br />
61701 Cyprus bromopropylate 0.61 5<br />
chlorpyrifos 0.20 0.3<br />
thiabendazole 3.5 5<br />
61714 Cyprus chlorpyrifos 0.14 0.3<br />
bromopropylate 1.1 5<br />
thiabendazole 2.09 5<br />
1.1.8. Mineola<br />
62022 Peru thiabendazole 0.13 5<br />
methidathion 0.12 2<br />
62057 Peru methidathion 0.15 2<br />
carbendazim 0.08 5<br />
thiabendazole 0.15 5<br />
1.1.9. Orange<br />
61539 Spain thiabendazole 0.79 5<br />
methidathion 0.18 2<br />
61548 Turkey thiabendazole 3.0 5<br />
61569 Spain dimethoate 0.11 1<br />
chlorpyrifos 0.09 0.3<br />
61583 Turkey thiabendazole 4.5 5<br />
61600 Spain chlorpyrifos 0.20 0.3<br />
carbendazim 0.06 5<br />
methidathion 0.04 2<br />
61635 Israel methidathion 0.17 2<br />
thiabendazole 1.2 5<br />
bromopropylate 0.37 5<br />
61700 Israel thiabendazole 2.4 5<br />
61706 Egypt thiabendazole 0.95 5<br />
61748 Morocco methidathion 0.40 2<br />
61826 Spain dic<strong>of</strong>ol 0.22 2<br />
methidathion 0.35 2<br />
61827 Greece parathion-me 0.16 0.2<br />
61859 Morocco carbendazim 0.07 5<br />
methidathion 0.41 2<br />
61865 Cyprus thiabendazole 3.8 5<br />
bromopropylate 0.64 5<br />
methidathion 0.41 2<br />
chlorpyrifos 0.14 0.3<br />
61904 S. Africa folpet 0.04 0.1<br />
thiabendazole 1.5 5<br />
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Table 2:<br />
Continued<br />
Sample Country <strong>of</strong> Residue detected Residue MRL<br />
number origin (mg/kg) (mg/kg)<br />
61913 S. Africa methidathion 0.04 2<br />
bromopropylate 0.14 5<br />
61933 Morocco methidathion 1.9 2<br />
carbendazim 0.08 5<br />
61956 S. Africa bromopropylate 0.17 5<br />
thiabendazole 1.4 5<br />
parathion 0.04 1<br />
61979 Morocco methidathion 0.49 2<br />
carbendazim 0.13 5<br />
folpet 0.06 0.1<br />
61982 S. Africa folpet 0.02 0.1<br />
61990 Zimbabwe thiabendazole 4.2 5<br />
61996 S. Africa binapacryl 0.05 0.05<br />
62007 S. Africa bromopropylate 0.04 5<br />
thiabendazole 2.2 5<br />
62011 Uruguay thiabendazole 1.7 5<br />
62020 S. Africa thiabendazole 0.17 5<br />
62026 S. Africa thiabendazole 0.38 5<br />
62027 S. Africa thiabendazole 1.2 5<br />
62049 Uruguay folpet 0.03 0.1<br />
62055 S. Africa folpet 0.03 0.1<br />
thiabendazole 0.09 5<br />
62056 S. Africa folpet 0.05 0.1<br />
bromopropylate 0.19 5<br />
62079 S. Africa endosulfan-2 0.06 0.5<br />
62080 S. Africa carbendazim 0.27 5<br />
62107 Spain methidathion 0.06 2<br />
1.1.10. Satsuma<br />
61582 Spain chlorpyrifos 0.14 0.3<br />
dic<strong>of</strong>ol 0.42 2<br />
61646 Argentina carbendazim 0.08 5<br />
thiabendazole 0.83 5<br />
61682 Argentina thiabendazole 0.77 5<br />
carbendazim 0.10 5<br />
malathion 0.53 2<br />
61687 S. Africa thiabendazole 4.2 5<br />
61707 S. Africa thiabendazole 3.0 5<br />
61719 S. Africa parathion 0.18 1<br />
carbendazim 0.50 5<br />
thiabendazole 0.52 5<br />
61731 S. Africa methidathion 0.32 2<br />
carbendazim 0.05 5<br />
61749 S. Africa malathion 0.10 2<br />
carbendazim 0.06 5<br />
61756 S. Africa tolyfluanid 0.04 No MRL<br />
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Table 2:<br />
Continued<br />
Sample Country <strong>of</strong> Residue detected Residue MRL<br />
number origin (mg/kg) (mg/kg)<br />
61757 Argentina malathion 0.11 2<br />
61785 S. Africa thiabendazole 0.43 5<br />
bromopropylate 0.34 5<br />
61807 S. Africa thiabendazole 0.09 5<br />
61853 Uruguay malathion 0.11 2<br />
thiabendazole 0.82 5<br />
61862 Uruguay thiabendazole 0.76 5<br />
methidathion 0.14 2<br />
61887 Peru carbendazim 0.27 5<br />
thiabendazole 4.2 5<br />
61915 Peru carbendazim 0.08 5<br />
thiabendazole 3.3 5<br />
61932 Peru thiabendazole 0.67 5<br />
61963 S. Africa thiabendazole 1.7 5<br />
62002 S. Africa malathion 0.04 2<br />
thiabendazole 0.48 5<br />
parathion 0.23 1<br />
62082 Spain methidathion 0.12 2<br />
malathion 0.38 2<br />
thiabendazole 2.4 5<br />
chlorpyrifos 0.12 0.3<br />
1.1.11. Tangarine<br />
62030 Brazil thiabendazole 0.29 5<br />
1.3. Pome Fruit 1.3.1. Apple<br />
61520 France phosalone 0.13 2<br />
thiabendazole 1.0 5<br />
61522 France captan 0.08 3<br />
tolyfluanid 0.12 No MRL<br />
61524 France tolyfluanid 0.07 No MRL<br />
captan 0.09 3<br />
carbendazim 0.12 2<br />
61527 Italy captan 0.08 3<br />
61532 France captan 0.02 3<br />
61551 France l-cyhalothrin 0.02 0.1<br />
thiabendazole 0.37 5<br />
61552 The Netherlands captan 0.08 3<br />
61566 United Kingdom carbendazim 0.09 2<br />
61579 Italy captan 0.11 3<br />
61580 France carbendazim 0.12 2<br />
thiabendazole 0.28 5<br />
61581 France thiabendazole 0.58 5<br />
phosalone 0.12 2<br />
61589 France thiabendazole 1.1 5<br />
- 14 -
<strong>10489</strong> <strong>Dept</strong>. <strong>of</strong> <strong>Argiculture</strong> 5/12/2003 12:34 pm Page 15<br />
Table 2:<br />
Continued<br />
Sample Country <strong>of</strong> Residue detected Residue MRL<br />
number origin (mg/kg) (mg/kg)<br />
61594 France carbendazim 0.07 2<br />
61614 Portugal folpet 0.12 3<br />
captan 0.18 3<br />
phosalone 0.27 2<br />
61633 Italy captan 0.06 3<br />
thiabendazole 0.26 5<br />
61634 France carbendazim 0.08 2<br />
thiabendazole 0.40 5<br />
61638 France carbendazim 0.05 2<br />
tolyfluanid 0.01 No MRL<br />
61666 France thiabendazole 0.36 5<br />
61669 France carbendazim 0.06 2<br />
thiabendazole 0.20 5<br />
folpet 0.11 3<br />
bifenthrin 0.05 No MRL<br />
61686 France carbendazim 0.23 2<br />
captan 0.27 3<br />
61698 Brazil dimethoate 0.05 1<br />
carbendazim 0.05 2<br />
captan 0.08 3<br />
61699 France bromopropylate 0.12 5<br />
carbendazim 0.15 2<br />
thiabendazole 0.30 5<br />
captan 0.04 3<br />
61710 France carbendazim 0.12 2<br />
thiabendazole 0.55 5<br />
61711 France thiabendazole 0.33 5<br />
61760 Brazil carbendazim 0.05 2<br />
folpet 0.09 3<br />
61763 New Zealand captan 0.03 3<br />
61783 Brazil captan 0.06 3<br />
61789 New Zealand captan 0.13 3<br />
61811 Chile thiabendazole 0.64 5<br />
61814 Argentina thiabendazole 0.06 5<br />
azinphos-me 0.14 1<br />
61850 France captan 0.37 3<br />
carbendazim 0.07 2<br />
61858 New Zealand captan 0.01 3<br />
61871 France thiabendazole 0.15 5<br />
61884 France thiabendazole 0.15 5<br />
61894 France thiabendazole 0.70 5<br />
61895 S. Africa phosmet 0.26 No MRL<br />
61896 France thiabendazole 0.37 5<br />
61916 New Zealand thiabendazole 0.08 5<br />
61929 Argentina carbendazim 0.46 1<br />
captan 1.2 3<br />
- 15 -
<strong>10489</strong> <strong>Dept</strong>. <strong>of</strong> <strong>Argiculture</strong> 5/12/2003 12:34 pm Page 16<br />
Table 2:<br />
Continued<br />
Sample Country <strong>of</strong> Residue detected Residue MRL<br />
number origin (mg/kg) (mg/kg)<br />
61937 France carbendazim 0.07 2<br />
captan 0.05 3<br />
phosalone 0.21 2<br />
thiabendazole 0.70 5<br />
61953 S. Africa iprodione 0.74 10<br />
61954 New Zealand captan 0.04 3<br />
61970 New Zealand captan 0.04 3<br />
61995 France tolyfluanid 0.05 No MRL<br />
62001 S. Africa iprodione 0.79 10<br />
62016 France parathion-me 0.04 0.2<br />
tolyfluanid 0.02 No MRL<br />
62045 France captan 0.02 3<br />
1.3.2. Pear<br />
61521 The Netherlands carbendazim 0.08 2<br />
61533 Portugal phosmet 0.14 No MRL<br />
folpet 0.19 3<br />
captan 0.34 3<br />
chlorpyrifos 0.07 0.5<br />
61564 Portugal phosmet 0.10 No MRL<br />
thiabendazole 0.05 5<br />
captan 0.15 3<br />
folpet 1.5 3<br />
61565 Portugal captan 0.14 3<br />
phosmet 0.12 No MRL<br />
folpet 0.46 3<br />
61585 Portugal thiabendazole 2.0 5<br />
captan 0.05 3<br />
folpet 0.02 3<br />
61597 Portugal omethoate 0.06 0.5<br />
captan 0.08 3<br />
phosmet 0.12 No MRL<br />
dimethoate 0.09 1<br />
carbendazim 0.13 2<br />
61688 Portugal phosmet 0.18 No MRL<br />
captan 0.68 3<br />
folpet 0.46 3<br />
61787 S. Africa iprodione 0.11 10<br />
61907 Argentina captan 0.44 3<br />
folpet 1.1 3<br />
carbendazim 0.45 2<br />
thiabendazole 1.1 5<br />
61927 The Netherlands carbendazim 0.11 2<br />
captan 0.03 3<br />
procymidone 0.24 1<br />
61969 S. Africa phosmet 0.17 No MRL<br />
62010 Portugal phosmet 0.09 No MRL<br />
- 16 -
<strong>10489</strong> <strong>Dept</strong>. <strong>of</strong> <strong>Argiculture</strong> 5/12/2003 12:34 pm Page 17<br />
Table 2:<br />
Continued<br />
Sample Country <strong>of</strong> Residue detected Residue MRL<br />
number origin (mg/kg) (mg/kg)<br />
1.4. Stone Fruit 1.4.1. Apricot<br />
61903 Greece captan 0.18 2<br />
61910 France captan 0.09 2<br />
l-cyhalothrin 0.04 0.1<br />
1.4.2. Cherry<br />
61912 United States endosulfan-2 0.03 0.05<br />
endosulfate 0.03 0.05<br />
carbendazim 0.09 0.1<br />
61940 Turkey diazinon 0.07 0.3<br />
1.4.3. Nectarine<br />
61598 Chile iprodione 1.1 5<br />
61891 Spain phosalone 0.09 1<br />
61905 France captan 0.03 2<br />
61959 France iprodione 0.14 5<br />
1.4.4. Peach<br />
61806 Spain Captan 0.20 2<br />
61835 Spain carbendazim 0.06 1<br />
61860 Spain endosulfan-1 0.00 0.5<br />
endosulfan-2 0.01 0.5<br />
endosulfate 0.01 0.5<br />
carbendazim 0.26 1<br />
61863 France captan 0.01 2<br />
methamidophos 0.07 0.05<br />
chlorpyrifos 0.04 0.2<br />
carbendazim 0.12 1<br />
61902 France carbendazim 0.07 1<br />
iprodione 0.57 5<br />
61935 Spain dic<strong>of</strong>ol 0.06 0.02<br />
1.4.5. Plum<br />
61615 S. Africa acephate 0.05 2<br />
61679 Chile chlorpyrifos 0.07 0.2<br />
iprodione 0.32 5<br />
61702 Chile carbendazim 0.09 0.5<br />
iprodione 0.23 5<br />
61761 Chile iprodione 2.6 5<br />
61788 Chile iprodione 1.5 5<br />
61799 Spain carbendazim 0.05 0.5<br />
methamidophos 0.11 0.3<br />
acephate 0.44 2<br />
61832 Spain dimethoate 0.17 1<br />
61877 Spain acephate 0.26 2<br />
- 17 -
<strong>10489</strong> <strong>Dept</strong>. <strong>of</strong> <strong>Argiculture</strong> 5/12/2003 12:34 pm Page 18<br />
Table 2:<br />
Continued<br />
Sample Country <strong>of</strong> Residue detected Residue MRL<br />
number origin (mg/kg) (mg/kg)<br />
1.5. Berries & Small Fruit 1.5.1.1. Grapes<br />
61601 S. Africa iprodione 0.22 10<br />
61623 S. Africa iprodione 0.15 10<br />
61704 India carbendazim 0.88 2<br />
61759 India fenvalerate 0.08 0.1<br />
acephate 0.06 0.02<br />
61772 India chlorpyrifos 0.14 0.5<br />
carbendazim 1.4 2<br />
captan 0.03 3<br />
methamidophos 0.30 0.01<br />
omethoate 0.06 0.5<br />
acephate 1.4 0.02<br />
61944 Egypt iprodione 0.23 10<br />
carbendazim 0.08 2<br />
61964 Spain carbendazim 0.24 2<br />
chlorpyrifos 0.16 0.5<br />
61980 Spain chlorpyrifos 0.84 0.5<br />
carbendazim 0.16 2<br />
61983 Spain carbendazim 0.36 2<br />
chlorpyrifos 0.06 0.5<br />
62032 Greece parathion-me 0.07 0.2<br />
fenitrothion 0.03 0.5<br />
carbendazim 0.05 2<br />
iprodione 0.07 10<br />
vinclozolin 0.31 5<br />
1.5.2.1. Strawberry<br />
61570 Morocco carbendazim 0.34 0.1<br />
captan 1.1 3<br />
dichl<strong>of</strong>luanid 0.97 10<br />
61781 Ireland iprodione 0.25 10<br />
61825 Ireland tolyfluanid 0.77 No MRL<br />
61841 Ireland chlorothalonil 0.08 3<br />
carbendazim 0.12 0.1<br />
61844 Ireland iprodione 1.1 10<br />
61882 Ireland tolyfluanid 0.76 No MRL<br />
61941 Ireland tolyfluanid 0.77 No MRL<br />
62024 Ireland iprodione 1.7 10<br />
1.5.3.1. Blackberry<br />
61845 The Netherlands iprodione 1.3 5<br />
1.5.3.2. Raspberry<br />
61843 Ireland iprodione 0.10 5<br />
- 18 -
<strong>10489</strong> <strong>Dept</strong>. <strong>of</strong> <strong>Argiculture</strong> 5/12/2003 12:34 pm Page 19<br />
Table 2:<br />
Continued<br />
Sample Country <strong>of</strong> Residue detected Residue MRL<br />
number origin (mg/kg) (mg/kg)<br />
1.5.4.2. Blueberry<br />
61621 Chile chlorothalonil 0.15 0.01<br />
carbendazim 0.13 0.1<br />
iprodione 0.24 0.02<br />
1.5.4.3. Red Currant<br />
61974 Belgium vinclozolin 0.03 10<br />
phosalone 8.5 1<br />
tolyfluanid 0.04 No MRL.<br />
bromopropylate 0.03 0.05<br />
1.6. Miscellaneous Fruit 1.6.1. Avocado<br />
61727 S. Africa carbendazim 0.14 0.1<br />
1.6.2. Banana<br />
61591 Costa Rica thiabendazole 0.11 5<br />
61717 Costa Rica vinclozolin 0.02 0.05<br />
61735 Mexico thiabendazole 1.7 5<br />
61925 Costa Rica thiabendazole 0.24 5<br />
61962 Windward Isles thiabendazole 1.1 5<br />
61985 Belize thiabendazole 0.50 5<br />
62029 Costa Rica thiabendazole 0.26 5<br />
62035 Belize thiabendazole 0.07 5<br />
62067 Honduras thiabendazole 0.49 5<br />
62068 Belize thiabendazole 0.68 5<br />
62084 Belize folpet 0.01 0.1<br />
62084 Belize thiabendazole 0.44 5<br />
1.6.3. Fig<br />
61775 Brazil tolyfluanid 0.02 No MRL<br />
1.6.4. Kiwano<br />
61596 New Zealand chlorothalonil 0.06 0.01<br />
1.6.5. Kiwi<br />
61613 Italy vinclozolin 4.1 10<br />
61716 Italy vinclozolin 5.9 10<br />
61813 Italy vinclozolin 2.5 10<br />
61833 Chile Iprodione 0.05 5<br />
1.6.6. Kumquat<br />
61918 S. Africa malathion 0.04 0.5<br />
thiabendazole 0.22 0.05<br />
- 19 -
<strong>10489</strong> <strong>Dept</strong>. <strong>of</strong> <strong>Argiculture</strong> 5/12/2003 12:34 pm Page 20<br />
Table 2:<br />
Continued<br />
Sample Country <strong>of</strong> Residue detected Residue MRL<br />
number origin (mg/kg) (mg/kg)<br />
1.6.7. Litchi<br />
61852 Thialand cypermethrin 0.13 0.05<br />
carbendazim 0.53 0.1<br />
1.6.8. Mango<br />
61553 Brazil thiabendazole 2.6 5<br />
61978 Brazil thiabendazole 0.12 5<br />
1.6.9. Papaya<br />
61776 Brazil chlorothalonil 0.04 0.01<br />
1.6.10. Passion Fruit<br />
61796 Kenya iprodione 0.16 0.02<br />
carbendazim 0.11 0.1<br />
1.6.14. Tamarillo<br />
62047 Chile chlorothalonil 0.03 0.01<br />
2. Vegetables 2.1. Root & Tuber Vegetables 2.1.1. Carrots<br />
61577 Ireland iprodione 0.12 0.3<br />
61663 Spain binapacryl 0.03 0.05<br />
61674 Spain endosulfate 0.06 0.05<br />
61766 Spain binapacryl 0.01 0.05<br />
61823 France binapacryl 0.02 0.05<br />
61909 Spain binapacryl 0.01 0.05<br />
61977 France ppdde 0.03 0.05<br />
quintozene 0.04 No MRL<br />
62069 Ireland chlorfenvinphos 0.10 0.5<br />
2.1.2. Parsnip<br />
61517 Ireland chlorfenvinphos 0.35 0.5<br />
61546 Ireland chlorfenvinphos 0.11 0.5<br />
61555 Ireland chlorfenvinphos 0.21 0.5<br />
61605 Ireland chlorfenvinphos 0.18 0.5<br />
61648 Ireland dieldrin 0.08 No MRL<br />
chlorfenvinphos 0.24 0.5<br />
bromopropylate 0.02 1<br />
61693 Ireland chlorfenvinphos 0.29 0.5<br />
61820 Israel endosulfan-2 0.19 0.05<br />
62071 Ireland chlorfenvinphos 0.17 0.5<br />
2.1.4. Swede<br />
61930 Ireland chlorpyrifos 0.09 0.05<br />
62061 Ireland mevinphos 0.06 0.1<br />
- 20 -
<strong>10489</strong> <strong>Dept</strong>. <strong>of</strong> <strong>Argiculture</strong> 5/12/2003 12:34 pm Page 21<br />
Table 2:<br />
Continued<br />
Sample Country <strong>of</strong> Residue detected Residue MRL<br />
number origin (mg/kg) (mg/kg)<br />
2.2.2. Bulb Onion<br />
62111 Spain phosphamidon 0.07 0.2<br />
2.3. Fruiting Vegetables 2.3.1. Solanacea 2.3.1.2. Pepper<br />
61535 Spain endosulfate 0.05 1<br />
procymidone 0.07 2<br />
endosulfate 0.05 1<br />
61620 Morocco endosulfan-1 0.50 1<br />
endosulfate 0.75 1<br />
endosulfan-2 0.61 1<br />
61653 Spain vinclozolin 0.11 3<br />
procymidone 0.08 2<br />
2.3.1.3. Tomato<br />
61530 Canary Islands procymidone 0.07 2<br />
61572 Spain procymidone 0.19 2<br />
61751 Ireland tolyfluanid 0.10 No MRL<br />
62066 Ireland chlorothalonil 0.00 2<br />
iprodione 0.02 5<br />
tolyfluanid 0.07 No MRL<br />
2.3.2. Cucurbits(edible peel.) 2.3.2.1. Courgette<br />
61519 Spain carbendazim 0.08 0.3<br />
2.3.2.2. Cucumber<br />
61531 Spain endosulfate 0.01 0.05<br />
61560 Spain chlorothalonil 0.04 1<br />
procymidone 0.10 1<br />
2.3.3. Cucurbits(inedible peel.) 2.3.3.1. Melon<br />
61730 Spain endosulfate 0.02 0.3<br />
61758 Morocco endosulfate 0.16 0.3<br />
61769 Spain endosulfate 0.10 0.3<br />
2.4. Brassica Vegetables 2.4.1. Flowering Brassicas 2.4.1.1. Broccoli<br />
61768 Spain lindane 0.03 1<br />
2.4.2. Head Brassicas. 2.4.2.1. Head Cabbage<br />
61658 Ireland chlorothalonil 0.05 3<br />
61745 Spain lindane 0.22 1<br />
2.5. Leafy Vegetables 2.5.1. Lettuce and Similar 2.5.1.1. Lettuce<br />
61515 Ireland iprodione 7.2 10<br />
demeton-s-me-sulfone 0.14 0.5<br />
propyzamide 0.06 1<br />
- 21 -
<strong>10489</strong> <strong>Dept</strong>. <strong>of</strong> <strong>Argiculture</strong> 5/12/2003 12:34 pm Page 22<br />
Table 2:<br />
Continued<br />
Sample Country <strong>of</strong> Residue detected Residue MRL<br />
number origin (mg/kg) (mg/kg)<br />
61536 Spain procymidone 0.18 5<br />
vinclozolin 0.27 5<br />
61540 Spain procymidone 0.12 5<br />
chlorothalonil 0.05 0.01<br />
folpet 0.04 2<br />
61680 France procymidone 0.09 5<br />
61737 Italy deltamethrin 0.07 0.5<br />
61740 Ireland cypermethrin 0.16 2<br />
deltamethrin 0.06 0.5<br />
iprodione 1.9 10<br />
61922 Ireland iprodione 0.89 10<br />
2.5.2. Spinach and Similar 2.5.2.1. Spinach<br />
61642 Spain cypermethrin 0.60 0.5<br />
61746 Italy deltamethrin 0.22 0.5<br />
61803 Spain chlorpyrifos 0.42 0.05<br />
Cypermethrin 0.29 0.5<br />
2.5.5. Herbs 2.5.5.1. Lemongrass<br />
61976 Thailand propyzamide 0.17 1<br />
2.5.5.2. Parsley<br />
61649 Ireland chlorpyrifos 0.19 0.05<br />
61723 Ireland chlorothalonil 2.02 5<br />
61742 Ireland bifenthrin 0.09 No MRL<br />
61765 Italy bifenthrin 0.12 No MRL<br />
2.6. Legume Vegetables 2.6.1. Beans 2.6.1.1. Green Beans<br />
61616 Kenya dimethoate 0.04 1<br />
61911 Kenya bifenthrin 0.05 No MRL<br />
2.7. Stem vegetables 2.7.2. Celery<br />
61514 Spain dichl<strong>of</strong>luanid 0.08 5<br />
61537 Spain fenitrothion 0.30 0.5<br />
cypermethrin 0.13 0.05<br />
61563 Spain fenitrothion 0.05 0.5<br />
chlorothalonil 0.06 10<br />
61607 Spain folpet 0.07 0.1<br />
61654 Spain chlorothalonil 0.10 10<br />
61822 Ireland chlorothalonil 0.29 10<br />
62086 Ireland folpet 0.00 0.1<br />
2.7.3. Fennel<br />
61733 The Netherlands tolcl<strong>of</strong>os-me 0.06 No MRL<br />
- 22 -
<strong>10489</strong> <strong>Dept</strong>. <strong>of</strong> <strong>Argiculture</strong> 5/12/2003 12:34 pm Page 23<br />
Table 2:<br />
Continued<br />
Sample Country <strong>of</strong> Residue detected Residue MRL<br />
number origin (mg/kg) (mg/kg)<br />
2.8. Fungii 2.8.1. Mushroom<br />
61947 Ireland lindane 0.02 1<br />
2.11. Potato 2.11.1. Potato<br />
61544 France tecnazene 0.07 No MRL.<br />
61661 Ireland thiabendazole 0.07 15<br />
61836 Ireland thiabendazole 0.12 15<br />
61885 Italy acephate 0.10 0.02<br />
ii<br />
Targeted Sampling Programme<br />
Eleven samples <strong>of</strong> fruit and vegetables were taken during 2002 as a follow up to MRL<br />
exceedances which occurred in 2001 and 2002. Five <strong>of</strong> the samples were taken as statutory<br />
samples. The results from the analysis <strong>of</strong> these samples is presented in Table 3 below.<br />
Three <strong>of</strong> the samples taken were <strong>of</strong> Irish origin while the remainder were imports from<br />
either EU or third countries. The samples analysed did not contain any pesticide residue in<br />
excess <strong>of</strong> a statutory MRL so no further enforcement action was required.<br />
Samples <strong>of</strong> fruit and vegetables which were found to contain pesticide residues in excess<br />
<strong>of</strong> the MRL from the 2002 sampling programme will be targeted for sampling in 2003.<br />
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Table 3: <strong>Pesticide</strong> residues detected in targeted samples <strong>of</strong> fruit and vegetables, 2002<br />
Commodity Sample Follow up Country Residue Residue MRL<br />
number to sample <strong>of</strong> origin detected (mg/kg) (mg/kg)<br />
number<br />
Strawberry 61797 61338 from 2001 Ireland Iprodione 0.06 10<br />
Vinclozolin 0.1 5.0<br />
Tolyfluanid 1.56 No MRL<br />
Strawberry** 61824 61338 from 2001 Ireland Vinclozolin 0.07 5.0<br />
Kiwano** 61639 61596 from 2002 New Zealand No residue detected<br />
Kumquat** 61578 61513 from 2001 Israel Malathion 0.46 0.5<br />
Passion Fruit 61831 61220 from 2001 South Africa No residue detected<br />
Carrots 62132 69077 from 2002 Ireland Chlorfenvinphos 0.48 0.5<br />
Carrots 62133 61499 from 2001 Ireland Chlorfenvinphos 0.09 0.5<br />
Triazophos 0.02 0.02<br />
Pepper 61798 61620 from 2002 Morocco Endosulfan-1 0.06 1.0<br />
Endosulfate 0.05<br />
Endosulfan-2 0.07<br />
Lettuce** 61641 61540 from 2002 Spain No residue detected<br />
Spinach 61732 61642 from 2002 Spain Cypermethrin 0.01 0.5<br />
Celery** 61640 61537 from 2002 Spain No residue detected<br />
**= these samples were taken as statutory samples.<br />
iii<br />
Sampling <strong>of</strong> vegetable crops produced by growers participating in the An Bord<br />
Glas Quality Programme<br />
The An Bord Glas Quality Programme is targeted at both growers and pre-packers <strong>of</strong> fresh<br />
produce. It encompasses all the main sectors <strong>of</strong> production, including field vegetables,<br />
mushrooms, s<strong>of</strong>t and top fruit, protected crops and potatoes. Participation involves<br />
implementation <strong>of</strong> quality systems designed to ensure that horticultural produce is<br />
produced and handled in accordance with best practices and procedures and complies with<br />
current regulatory requirements. The standards established are outlined in a series <strong>of</strong><br />
Quality Manuals tailored to the specific needs <strong>of</strong> the individual sectors <strong>of</strong> the horticultural<br />
industry.<br />
Participants in the An Bord Glas Quality Programme are independently audited to assess<br />
compliance with the standards specified in the relevant Quality Manual(s).<br />
During 2002 some 144 samples <strong>of</strong> mainly vegetables, but including one strawberry and 2<br />
apple samples, were taken by An Bord Glas personnel from crops grown by or pre-packed<br />
by participants in the An Bord Glas Quality Programme. The samples were taken<br />
following harvest at point <strong>of</strong> packaging or assembly and were dispatched using a courier<br />
service to an accredited laboratory for analysis. The samples were analysed for 89<br />
pesticides and metabolites (Annex IX). The results obtained (Annex X) demonstrate that<br />
vegetables produced by Irish growers participating in the An Bord Glas Quality<br />
Programme have a lower pesticide residue content than those found in the general<br />
monitoring programme which includes both domestic and imported produce. 15.2% <strong>of</strong><br />
samples submitted for analysis were found to contain pesticide residues. None <strong>of</strong> these<br />
samples contained a pesticide residue in excess <strong>of</strong> an MRL.<br />
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B<br />
i<br />
CEREALS<br />
Routine Monitoring Programme<br />
In 2002, 47 cereal samples (19 barley, 17 wheat, 5 oats, 3 processed oats, 2 processed<br />
wheat and 1 processed barley) <strong>of</strong> both domestic and imported origin were analysed for<br />
residues <strong>of</strong> 89 pesticides and metabolites (Annex V). One <strong>of</strong> the samples analysed, a<br />
French wheat sample, contained detectable residues <strong>of</strong> malathion while the remainder<br />
contained no detectable pesticide residues (Tables 4 and 5). MRLs are currently in place<br />
for 127 different pesticides 64 <strong>of</strong> which are not yet included in the monitoring programme.<br />
Table 4: Cereal samples analysed for their pesticide residue content in 2002<br />
Commodity No. Samples No. Domestic No. Residues<br />
Analysed Samples Imported*<br />
Samples > MRL ≤ MRL ND<br />
Wheat grain 17 5 12 0 1 16<br />
Barley grain 19 19 0 0 0 19<br />
Oat grain 5 5 0 0 0 05<br />
Wheat flakes 2 2 0 0 02<br />
Oat flakes 1 1 0 0 01<br />
Oat bran. 2 1 1 0 0 02<br />
Barley flakes 1 1 0 0 01<br />
Totals 47 31 16 0 1 46<br />
*ND = No residue detected<br />
Table 5: <strong>Pesticide</strong> residues detected in cereals in 2002<br />
Sample Country Residue Residue MRL<br />
number <strong>of</strong> origin detected (mg/kg) (mg/kg)<br />
Cereals<br />
1.0 Wheat<br />
62098 French Malathion. 0.09 8<br />
ii<br />
Targeted Sampling Programme<br />
As there were no violations <strong>of</strong> MRLs in the years 1997 through 2001, targeted sampling<br />
<strong>of</strong> cereals and cereal products was not undertaken in 2002.<br />
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C<br />
FOOD OF ANIMAL ORIGIN<br />
The monitoring programme in place is restricted to the sampling and analysis <strong>of</strong> fresh<br />
meat, milk, dairy products, eggs and honey <strong>of</strong> Irish origin. Bovine meat (130 fat samples),<br />
ovine meat (48 fat samples), porcine meat (52 fat samples), venison meat (2 fat samples),<br />
poultry meat (36 fat samples) and 13 samples <strong>of</strong> eggs were analysed for residues <strong>of</strong> 55<br />
pesticides, metabolites and for residues <strong>of</strong> polychlorinated biphenyl (PCB) congeners<br />
[no’s 28, 52, 101, 118, 138, 153 and 180] (Annex VI). 54 samples <strong>of</strong> dairy produce were<br />
analysed for 55 pesticides and metabolites (Annex VII) and polychlorinated biphenyl<br />
(PCB) congeners [no’s 28, 52, 101, 118, 138, 153 and 180] while 14 samples <strong>of</strong> honey<br />
were analysed for 89 pesticide and metabolite residues.<br />
MRLs have been established for 104 pesticides <strong>of</strong> which 34 were included in the 2002<br />
monitoring programme. Samples are also analysed, as indicated above, for residues <strong>of</strong> the<br />
environmental contaminants polychlorinated biphenyls (PCBs). PCBs are persistent<br />
organochlorine compounds which, in the past, were released into the environment from<br />
industrial sources but whose use has since largely been discontinued. These are included<br />
in the residue monitoring programme due to concerns associated with their presence in<br />
food and due to their links with polychlorinated dibenzodioxins.<br />
1 Bovine Meat<br />
i<br />
Routine Monitoring Programme<br />
Details <strong>of</strong> the analytical results are presented in Table 6. Overall some 5.4% <strong>of</strong> the bovine<br />
samples analysed contained detectable pesticide or PCB residues. Some 4.6% <strong>of</strong> samples<br />
analysed contained detectable residues <strong>of</strong> DDT (as metabolite ppDDE) and 0.8% <strong>of</strong><br />
samples contained a detectable residue <strong>of</strong> dieldrin. The residue levels detected were in<br />
trace amounts and were not considered significant from a consumer safety viewpoint. The<br />
origin <strong>of</strong> these trace organochlorine pesticide residues detected are considered to result<br />
from either background levels in soil as a consequence <strong>of</strong> the former use or intake through<br />
residual traces present in feeding stuffs. Generally, the quantities detected and reported<br />
reflect the sensitivity <strong>of</strong> the analytical methodologies currently used. No residues <strong>of</strong><br />
PCB’s were detected in any <strong>of</strong> the samples analysed.<br />
Table 6: <strong>Pesticide</strong> residues detected in bovine kidney fat in 2002<br />
Sample Country Residue Residue MRL<br />
number <strong>of</strong> origin detected (mg/kg fat) (mg/kg fat)<br />
65952 Ireland ppdde 0.015 1<br />
66029 Ireland ppdde 0.017 1<br />
66061 Ireland ppdde 0.004 1<br />
66073 Ireland ppdde 0.006 1<br />
66074 Ireland ppdde 0.008 1<br />
66153 Ireland ppdde 0.006 1<br />
66164 Ireland Dieldrin 0.007 0.2<br />
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ii<br />
Targeted Sampling Programme<br />
As there were no violations <strong>of</strong> MRLs in the past number <strong>of</strong> years, targeted sampling <strong>of</strong><br />
samples <strong>of</strong> bovine meat was not undertaken in 2002.<br />
2 Ovine Meat<br />
i<br />
Routine Monitoring Programme<br />
Details <strong>of</strong> the analytical results obtained are presented in Table 7. Some 7.6% <strong>of</strong> samples<br />
contained detectable residues. Residues <strong>of</strong> 2 different pesticides, DDT and HCB were<br />
detected. MRLs have been established for both <strong>of</strong> these compounds. Two <strong>of</strong> the samples<br />
containing detectable pesticide residues had a residue <strong>of</strong> a single pesticide while the<br />
remaining two each contained residues <strong>of</strong> 2 pesticides. The residues were not considered<br />
to be significant from a consumer safety viewpoint. The quantities detected and reported<br />
reflect the sensitivity <strong>of</strong> the analytical methodologies currently used.<br />
The residues detected were DDT (7.6% <strong>of</strong> samples) and HCB (3.8% <strong>of</strong> samples). Three<br />
<strong>of</strong> the DDT residues levels found reflect background levels present in soil while a fourth<br />
at 0.074mg/kg is consistent with contamination through the animal feed as it is higher than<br />
normally encountered. The two residues <strong>of</strong> HCB detected are at background levels. As<br />
HCB was never approved for use in Ireland so it is likely to have come from residual<br />
traces present in the imported constituents <strong>of</strong> animal feed.<br />
Table 7: <strong>Pesticide</strong> residues detected in ovine kidney fat in 2002<br />
Sample Country Residue Residue MRL<br />
number <strong>of</strong> origin detected (mg/kg fat) (mg/kg fat)<br />
65920 Ireland ppdde 0.074 1<br />
66084 ppdde 0.003 1<br />
Ireland HCB 0.003 0.2<br />
66102 ppdde 0.003 1<br />
Ireland HCB 0.004 0.2<br />
66117 Ireland ppdde 0.003 1<br />
ii<br />
Targeted Sampling Programme<br />
As there were no violations <strong>of</strong> MRLs in the past number <strong>of</strong> years, targeted sampling <strong>of</strong><br />
samples <strong>of</strong> ovine meat was not undertaken in 2002.<br />
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3 Porcine Meat<br />
i<br />
Routine Monitoring Programme<br />
Details <strong>of</strong> the analytical results obtained are presented in Table 8. Some 3.8% <strong>of</strong> samples<br />
contained detectable pesticide residues. Residues <strong>of</strong> 2 different pesticides, DDT (1.9% <strong>of</strong><br />
samples) and dieldrin (1.9% <strong>of</strong> samples) were detected. MRLs have been established<br />
for both <strong>of</strong> these compounds. The residues were not considered to be significant from<br />
a consumer safety viewpoint. The quantities detected and reported reflect the sensitivity <strong>of</strong><br />
the analytical methodologies currently used in the laboratory.<br />
Uses <strong>of</strong> both DDT and dieldrin have not occurred in Ireland for many years and residues<br />
<strong>of</strong> these pesticides generally arise from environmental contamination <strong>of</strong> soil due to former<br />
use. As pig production, in the main, takes place indoors it is likely that the residues <strong>of</strong> both<br />
DDT and dieldrin detected reflect background levels present in the animal feed.<br />
Table 8: <strong>Pesticide</strong> residues detected in porcine kidney fat in 2002<br />
Sample Country Residue Residue MRL<br />
number <strong>of</strong> origin detected (mg/kg fat) (mg/kg fat)<br />
65927 Ireland dieldrin 0.028 0.2<br />
66065 Ireland pp-dde 0.004 1<br />
ii<br />
Targeted Sampling Programme<br />
There were no violations <strong>of</strong> MRL’s in 1999, 2000 orin 2001. No samples were targeted for<br />
analysis in 2002.<br />
4 Dairy Products<br />
i<br />
Routine Monitoring Programme<br />
54 samples <strong>of</strong> milk were analysed. None <strong>of</strong> the samples analysed contained detectable<br />
pesticide residues.<br />
ii<br />
Targeted Sampling Programme<br />
As there were no violations <strong>of</strong> MRLs for a number <strong>of</strong> years, targeted sampling <strong>of</strong> dairy<br />
produce was not undertaken in 2002.<br />
5 Venison<br />
2 samples <strong>of</strong> venison were analysed. Neither <strong>of</strong> the samples contained detectable pesticide<br />
residues.<br />
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ii<br />
Targetted Sampling Programme<br />
As there were no violations <strong>of</strong> venison MRLs encountered in the past no targeting<br />
sampling was under taken in 2002.<br />
6 Poultry<br />
Details <strong>of</strong> the analytical results obtained are presented in Table 9. Thirty six samples<br />
<strong>of</strong> poultry fat were analysed for pesticide residues. Three samples (8.3 %) were found to<br />
contain detectable residues <strong>of</strong> lindane the only residue detected in the samples analysed.<br />
There was no residue present in excess <strong>of</strong> an MRL.<br />
Table 9: <strong>Pesticide</strong> residues detected in poultry fat in 2002<br />
Sample Country Residue Residue MRL<br />
number <strong>of</strong> origin detected (mg/kg fat) (mg/kg fat)<br />
66075 Ireland lindane 0.004 1<br />
66076 Ireland lindane 0.003 1<br />
66105 Ireland lindane 0.004 1<br />
These lindane residues were considered to have derived from trace contamination <strong>of</strong><br />
poultry feed and were not considered to be significant from a consumer safety point <strong>of</strong><br />
view.<br />
7 Eggs<br />
Eggs were analysed for the first time for pesticide residues during 2002. 13 samples <strong>of</strong><br />
eggs were analysed. None <strong>of</strong> the samples contained detectable pesticide residues.<br />
ii<br />
Targetted Sampling Programme<br />
As egg MRL’s had not been exceeded no targeted sampling programme took place in<br />
2002.<br />
8 Honey<br />
Honey was analysed for the first time for pesticide residues in 2002. 14 samples <strong>of</strong> honey<br />
were analysed. None <strong>of</strong> the samples contained detectable pesticide residues from the<br />
current screen.<br />
ii Targeted Sampling Programme<br />
As honey MRL’s had not been exceeded no targeted sampling for honey took place in<br />
2002.<br />
D MISCELLANEOUS AND COMPLAINT SAMPLES<br />
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There were five miscellaneous and three complaint samples analysed during 2002. The<br />
five miscellaneous samples were <strong>of</strong> flour and were submitted by Teagasc for pesticide<br />
residue analysis. Three complaint samples were submitted by consumers for analysis. The<br />
results <strong>of</strong> these analyses are presented in Table 10. All <strong>of</strong> the samples were free <strong>of</strong> residues<br />
with the exception <strong>of</strong> a carrot sample which was found to contain residues <strong>of</strong><br />
chlorfenvinphos and diazinon. A follow up statutory sample <strong>of</strong> carrots was taken from the<br />
relevant grower to check the quality <strong>of</strong> the produce on sale. The statutory sample showed<br />
that the residues present were in compliance with statutory MRLs.<br />
Table 10: <strong>Pesticide</strong> residues detected in miscellaneous and complaint samples 2002<br />
Sample Country Residue Residue MRL<br />
number <strong>of</strong> origin detected (mg/kg fat) (mg/kg fat)<br />
Miscellaneous Samples<br />
69078 (wheat flour) Unknown none<br />
69079 (wheat flour) Unknown none<br />
69080 (wheat flour) Unknown none<br />
69081 (wheat flour) Unknown none<br />
69082 (wheat flour) Unknown none<br />
Complaint Samples<br />
69073 (kiwi) Unknown none<br />
69075 (Red pepper) Netherlands none<br />
69077 (carrot)** Ireland Chlorfenvinphos 1.2 0.5<br />
Diazinon. 0.21 0.2<br />
**= This sample consisted <strong>of</strong> a single carrot which does not consitute a proper sample. A<br />
subsequent statutory sample was taken to determine the residue levels present in these<br />
carrots.<br />
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CONCLUSIONS<br />
A INTRODUCTION<br />
When assessing the impact for consumers <strong>of</strong> exposure through diet to pesticide residues,<br />
it is appropriate to consider the effects <strong>of</strong> both chronic exposure and acute exposure. For<br />
the purposes <strong>of</strong> assessing the effects <strong>of</strong> chronic exposure, the level <strong>of</strong> exposure over a<br />
lifetime and the likely effects on health <strong>of</strong> such exposure must be considered. The<br />
techniques necessary for such assessments are well developed and involve consideration<br />
<strong>of</strong> the mean levels <strong>of</strong> exposure likely in relation to the acceptable daily intake (ADI) values<br />
established for individual pesticides. ADI values, which are a measure <strong>of</strong> the maximum<br />
level <strong>of</strong> intake over a lifetime adjudged to result in no adverse toxicological effects, include<br />
a safety factor to ensure that the elderly, infants and children, and those whose systems are<br />
under stress because <strong>of</strong> illness are protected.<br />
For the purposes <strong>of</strong> assessing the effects <strong>of</strong> acute exposure, the highest levels <strong>of</strong> exposure<br />
likely (97.5th percentile exposure) over a single day and the effects on health <strong>of</strong> such<br />
exposure must be considered. The techniques necessary for such assessments are less well<br />
developed than those relating to chronic exposure. For commodities consisting <strong>of</strong> large<br />
sized units (e.g. melons) or medium sized units (e.g. citrus and pome fruit), it is necessary<br />
that the variability <strong>of</strong> residues in individual commodity units be taken into account due to<br />
the possibility that all <strong>of</strong> the sample residue was present in one unit, e.g. in one apple. For<br />
that purpose a variability factor “v” is applied to the maximum residue limits detected in<br />
the composite samples analysed to take account <strong>of</strong> the worst possible situation which may<br />
be encountered 12 . In assessing the effects <strong>of</strong> acute exposure, the level <strong>of</strong> exposure must be<br />
considered in relation to the acute reference dose (ARfD) value established for individual<br />
pesticides. ARfD values, which are a measure <strong>of</strong> the maximum level <strong>of</strong> intake over a day,<br />
judged to result in no adverse toxicological effects, include a safety factor to ensure that<br />
the elderly, infants and children and those whose systems are under stress because <strong>of</strong><br />
illness are protected. To date ARfD values have been established for a limited number <strong>of</strong><br />
pesticides. Procedures are still under development particularly at the FAO/WHO Joint<br />
Meeting for <strong>Pesticide</strong> Residues (JMPR) and at EU level with a view to improving the<br />
methodology used to establish ARfD’s.<br />
B ROUTINE MONITORING PROGRAMME<br />
Inspection <strong>of</strong> the monitoring results for the year, which involved the analysis <strong>of</strong> some 949<br />
routine samples, 10 targeted samples, 5 miscellaneous samples, 3 complaint samples and<br />
10 variabiltiy samples, shows that some 32% <strong>of</strong> samples analysed contained quantifiable<br />
pesticide residues. 2.8% <strong>of</strong> these routine samples contained residues in excess <strong>of</strong> the<br />
statutory MRLs (Table 11). The levels present in most samples found to contain residues<br />
were extremely low. The presence <strong>of</strong> residues at such low levels reflects the sensitivity <strong>of</strong><br />
current analytical techniques. The 2002 results, like those obtained in previous years,<br />
continue to show that while a significant proportion <strong>of</strong> the samples analysed contain<br />
pesticide residues the residue levels present are generally very low.<br />
An assessment <strong>of</strong> the relationship between ADIs and the level <strong>of</strong> residues in samples<br />
exceeding established MRLs (Table 12) demonstrates the extent <strong>of</strong> the risks associated<br />
12 Food consumption and exposure assessment <strong>of</strong> chemicals. Report <strong>of</strong> a FAO/WHO consultation, Geneva, Switzerland, 10-14 February<br />
1997, WHO/FSF/FOS/97.5.<br />
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with dietary intake <strong>of</strong> such residues. The intake figures used for individual commodities<br />
are derived from the 96-98 IUNA dietary survey. The dietary intake assessment for<br />
chronically toxic pesticides was carried out using the mean consumption data while the<br />
intake assessment for the acutely toxic pesticides was carried out using the higher 97.5th<br />
percentile intake. Through use <strong>of</strong> such intake figures, all but the most extreme intake<br />
figures likely to arise have been taken into account when estimating the acute dietary<br />
impact <strong>of</strong> these residues for the consumer.<br />
Table 11:<br />
Samples containing pesticide residues exceeding Maximum Residue Limits (MRLs)<br />
in 2002<br />
Commodity Sample Country Residue Residue MRL<br />
number <strong>of</strong> origin detected (mg/kg) (mg/kg)<br />
Lettuce 61540 Spain chlorothalonil 0.05 0.01<br />
Celery 61537 Spain cypermethrin 0.14 0.05<br />
Strawberry 61570 Morocco carbendazim 0.34 0.1<br />
Kiwano 61596 South Africa chlorothalonil 0.06 0.01<br />
Pepper 61620 Morocco endosulfan 1.9 1<br />
Blueberry 61621 Chile carbendazim 0.13 0.1<br />
chlorothalonil 0.15 0.01<br />
iprodione 0.24 0.02<br />
Spinach 61642 Spain cypermethrin 0.6 0.5<br />
Parsley 61649 Ireland chloropyriphos 0.19 0.05<br />
Carrot 61674 Spain endosulfan 0.06 0.05<br />
Avocado 61727 South Africa carbendazim 0.14 0.1<br />
Grapes 61759 India acephate 0.06 0.02<br />
Grapes 61772 India acephate 1.35 0.02<br />
methamidophos 0.3 0.01<br />
Passion Fruit. 61796 Kenya iprodione 0.16 0.02<br />
Papaya 61776 Brazil chlorothalonil 0.04 0.01<br />
Parsnip 61820 Israel endosulfan 0.19 0.05<br />
Spinach 61803 Spain chlorpyrifos 0.42 0.05<br />
Peach 61863 France methamidophos 0.07 0.05<br />
Litchi 61852 Thialand cypermethrin 0.13 0.05<br />
Strawberry 61841 Ireland carbendazim 0.12 0.1<br />
Potato 61885 Italy acephate 0.1 0.02<br />
Kumquat 61918 South Africa thiabendazole 0.22 0.05<br />
Swede 61930 Ireland chlorpyrifos 0.09 0.05<br />
Peach 61935 Spain dic<strong>of</strong>ol 0.06 0.02<br />
Red Currant 61974 Belgium phosalone 8054 1<br />
Grapes 61980 Spain chlorpyrifos 0.84 0.5<br />
Tamarillo 62047 Chile chlorothalonil 0.03 0.01<br />
Carrot** 60977 Ireland chlorfenvinphos 1.21 0.5<br />
diazinon 0.16 0.5<br />
**= This sample was submitted as a complaint sample. The sample however consisted <strong>of</strong><br />
one carrot only and as such did not meet the sampling requirements. Sample number<br />
62132 (Table 3) was a follow up sample, taken in the correct manner, which was used<br />
to check if the carrots complied with the statutory MRL’s for chlorfenvinphos. No<br />
MRL exceedance was found.<br />
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In the case <strong>of</strong> consumers exposed to residues <strong>of</strong> chronically toxic pesticides their health<br />
would only be at risk if their dietary intake exceeded the ADI every day for an extended<br />
period <strong>of</strong> time. Nevertheless, the fact that abuses occur and that residue levels in excess <strong>of</strong><br />
the MRL continue to be detected, points to the need for the continuation and strengthening<br />
<strong>of</strong> the monitoring and violation investigation programmes.<br />
There was only one case in 2002 where the calculated chronic intake associated with an<br />
MRL exceedance exceeded the ADI. This occurred with a carrot complaint sample which<br />
was submitted for analysis by a consumer. In this case the ADI was only marginally<br />
exceeded. This carrot sample consisted <strong>of</strong> a single carrot and did not comply with the EU<br />
sampling requirements in terms <strong>of</strong> sample size. Produce from the carrot grower was re<br />
sampled according to the <strong>of</strong>ficial sampling procedures and the follow-up sample (sample<br />
no. 62132, Table 3) when analysed was found to be compliant with the statutory MRL.<br />
There were no cases during 2002 when the estimated acute intakes associated with MRL<br />
exceedances were greater than the relevant ARfD toxicological end point.<br />
An evaluation <strong>of</strong> the monitoring results shows that the number <strong>of</strong> samples analysed in 2002<br />
has increased by 52% over the numbers analysed in 2001. The residue results obtained in<br />
2002 are still quite comparable to those <strong>of</strong> 2001.<br />
In cereals and in food <strong>of</strong> animal origin samples the number and levels <strong>of</strong> pesticide residues<br />
found are marginally lower than those found in 2001 but overall the pattern is considered<br />
to be comparable.<br />
The pesticide residue pattern in fruit and vegetables from 2002 is different in a number <strong>of</strong><br />
ways to that found in 2001 in that,<br />
— a larger variety <strong>of</strong> fruit and vegetables were analysed, 72 in 2002 as opposed<br />
to 62 in 2001;<br />
— a larger number <strong>of</strong> pesticide residues were detected, 46 in 2002 as opposed to<br />
37 in 2001;<br />
— the % <strong>of</strong> imported produce sampled and analysed in 2002 monitoring<br />
programme was 81% while it was 71% in 2001;<br />
— the % <strong>of</strong> fruit and vegetables containing pesticide residues at 52% in 2002 is<br />
marginally higher than the 49.5% found in 2001. This difference is not<br />
considered to be significant;<br />
— the % <strong>of</strong> samples <strong>of</strong> fruit and vegetables containing pesticide residues greater<br />
than the MRL for 2002 at 4.8% is greater than that for 2001 where MRL<br />
exceedances were at 3.3% <strong>of</strong> samples analysed. This increase reflects the larger<br />
proportion <strong>of</strong> imported produce analysed. Imported fruit and vegetables have a<br />
higher % <strong>of</strong> MRL exceedances when compared to Irish produced produce;<br />
— the frequency at which pesticide residues were detected in fruit and vegetables<br />
during 2002 correspond with the pattern for 2001 where the most commonly<br />
detected pesticides were thiabendazole, carbendazim, captan and chlorpyrifos.<br />
Some changes noted in the 2002 results were that the use <strong>of</strong> methidathion on<br />
citrus has increased while residues <strong>of</strong> dimethoate were detected less frequently<br />
when compared to 2001. The use <strong>of</strong> dimethoate may have been affected by<br />
decisions taken in 2002 to modify the MRL’s for this pesticide.<br />
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As part <strong>of</strong> the programme <strong>of</strong> work in 2002 a limited study was carried out to study the<br />
variability <strong>of</strong> pesticide residues present in individual sample units. This is important when<br />
dealing with acutely toxic pesticides as it is assumed that a high level <strong>of</strong> variability exists<br />
between the amounts <strong>of</strong> residue present in individual sample units. The normal variability<br />
factor used, at present, when assessing acute dietary intake is 7x. (e.g. a laboratory sample<br />
<strong>of</strong> apples consists <strong>of</strong> 10 individual apples. These apples are homogenised, analysed and the<br />
result is the mean <strong>of</strong> the residues present in all <strong>of</strong> the apples. Each apple is a unit and if<br />
analysed individually it is possible to determine the variability <strong>of</strong> the residues between<br />
apples. Variability = Ratio <strong>of</strong> mean unit residue: highest individual unit residue.). In 2002<br />
a sample <strong>of</strong> peaches were found to contain the acutely toxic pesticide methamidophos. 10<br />
individual peaches were taken from the same consignment and analysed individually. The<br />
results are presented in Table 13. Comparison <strong>of</strong> the mean residue with the highest residue<br />
found indicates that the variability applying to this sample was a factor <strong>of</strong> 2.3x. This result<br />
is in line with the results found by monitoring authorities in other Member States. This<br />
factor is considerably lower that the variability factor <strong>of</strong> 7x which would normally be<br />
applied to peaches in the event <strong>of</strong> an MRL exceedance. It is possible to conclude that the<br />
use <strong>of</strong> a variability factor <strong>of</strong> 7x, when carrying out acute dietary intake assessments is<br />
likely to overestimate the expected intake.<br />
The pesticide monitoring programme is considered to be limited with regard to the number<br />
<strong>of</strong> samples being taken for analysis and the number <strong>of</strong> pesticide residues being sought in<br />
these samples. Steps are being taken to increase the capacity <strong>of</strong> the monitoring programme<br />
and the 2003 programme will see the numbers <strong>of</strong> samples analysed increase by 33% over<br />
the number analysed during 2002. It is also planned to increase the number <strong>of</strong> pesticides<br />
being determined in samples during 2004.<br />
The current plans for the <strong>Pesticide</strong> <strong>Control</strong> Laboratory are<br />
i to increase the number <strong>of</strong> samples scheduled for analysis in 2003 to 1300.<br />
ii<br />
to increase the number <strong>of</strong> pesticides included in the monitoring programme from<br />
2004 onwards.<br />
iii to continue extend the range <strong>of</strong> pesticides for which MRLs are established.<br />
iv to reduce the time period between sample receipt in the laboratory and the results<br />
<strong>of</strong> the analysis.<br />
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Table 12 : Relationship between excessive residue levels found and the ADI and ARfD levels for Irish Adults<br />
Sample Commodity Country <strong>Pesticide</strong> Residue. MRL ADI. ARfD Mean 97.5%ile Intake as Intake as<br />
no. <strong>of</strong> origin (mg/kg) (mg/kg) (mg/kg (mg/kg commodity diet a % <strong>of</strong> a % <strong>of</strong><br />
bw/day) bw/day) Intake (kg/day) (kg/day) ADI ARfD.<br />
61540 Lettuce Spain Chlorothalonil 0.05 0.01 0.03 None required 0.007 0.026 0.02 Not required<br />
61537 Celery Spain Cypermethrin 0.14 0.05 0.05 None required 0.004 0.021 0.02 Not required<br />
61570 Strawberry Morocco Carbendazim 0.34 0.1 0.03 None required 0.014 0.086 0.26 Not required<br />
61596 kiwano South Africa Chlorothalonil 0.06 0.01 0.03 None required 0.003 0.01 0.01 Not required<br />
61620 Pepper Morocco Endosulfan 1.9 1 0.006 0.02 0.013 0.053 7 58<br />
61621 Blueberry Chile Carbendazim 0.13 0.1 0.03 None required 0.003 0.01 0.02 Not required<br />
Chlorothalonil 0.15 0.01 0.03 None required 0.003 0.01 0.03 Not required<br />
Iprodione 0.24 0.02 0.06 None required 0.003 0.01 0.02 Not required<br />
61642 Spinach Spain Cypermethrin 0.60 0.5 0.05 None required 0.0094 0.0393 0.19 Not required<br />
61649 Parsley Ireland Chlorpyrifos 0.19 0.05 0.01 0.1 0.0004 0.0024 0.01 0.05<br />
61674 Carrot Spain Endosulfan 0.06 0.05 0.006 0.02 0.0270 0.083 0.45 2.91<br />
61727 Avocado South Africa Carbendazim 0.14 0.1 0.03 None required 0.0123 0.03186 0.10<br />
61759 Grapes India Acephate 0.06 0.02 0.03 0.1 0.0195 0.14 0.07 1<br />
61772 grapes India Acephate 1.35 0.02 0.03 0.1 0.0195 0.14 1.5 3<br />
methamidophos 0.30 0.01 0.004 0.004 0.0195 0.14 2.4 18<br />
61796 passion fruit Kenya iprodione 0.16 0.02 0.06 None required 0.0030 0.01<br />
61776 papaya Brazil chlorothalonil 0.04 0.01 0.03 None required 0.0030 0.01<br />
61820 parsnip Israel endosulfan 0.19 0.05 0.006 0.02 0.0126 0.0475 0.67 5<br />
61803 Spinach Spain Chlorpyrifos 0.42 0.05 0.01 0.1 0.0094 0.0393 0.66 2<br />
61863 Peach France methamidophos 0.07 0.05 0.004 0.004 0.0428 0.205 1.19 40<br />
61852 Litchii Thailand cypermethrin 0.13 0.05 0.05 None required 0.0030 0.01 0.01<br />
61841 Strawberry Ireland Carbendazim 0.12 0.1 0.03 None required 0.0140 0.086 0.10<br />
61885 Potato Italy Acephate 0.10 0.02 0.03 0.1 0.1429 0.597 0.83 7<br />
61918 Kumquat S. Africa thiabendazole 0.22 0.05 0.1 None required 0.0030 0.01 0.01<br />
61930 Swede Ireland Chlorpyrifos 0.09 0.05 0.01 0.1 0.0200 0.064 0.29 1<br />
61935 Peach Spain Dic<strong>of</strong>ol 0.06 0.02 0.002 0.015 0.0430 0.205 2.29 10<br />
61974 Red currant Belgium phosalone 8.54 1 0.02 0.3 0.0030 0.01 2.14 0.5<br />
61980 grapes Spain chlorpyrifos 0.84 0.5 0.01 0.1 0.0195 0.14 2.72 2.0<br />
62047 Tamarillo Chile chlorothalonil 0.03 0.01 0.03 None required 0.0030 0.01 0.01<br />
60977 Carrot ** Ireland chlorfenvinphos 1.21 0.5 0.0005 0.002 0.0270 0.083 108.90 83.7<br />
Diazinon 0.16 0.2 0.002 0.03 0.0270 0.083 3.60 0.7<br />
Comment: The intake calculations for chronic toxicity, for the above pesticide/crops, does not indicate an unacceptable risk to the consumer.<br />
In the case <strong>of</strong> passion fruit, papaya, Kiwano and blueberry the mean consumption was estimated to be 3 g/person/day as a default diet while the default 97.5th % diet was estimated to be 10g.<br />
In the case <strong>of</strong> celery the UK toddler 97.5th percentile consumption is determined to be 0.0088 kg/person/day. In the calculation the use <strong>of</strong> this dietary consumption figure would give an endosulfan intake which<br />
was 23.5% <strong>of</strong> the ARfD.<br />
In the case <strong>of</strong> cherry tomatoes the consumption data for “tomatoes” was used which overestimates the dietary intake for cherry tomatoes.<br />
**= A complaint sample which consisted <strong>of</strong> one single carrot. As the sample was a single carrot it does not comply with the definition <strong>of</strong> a sample and it is not possible to apply the MRL to the sample. A follow<br />
up sample, sample number 62132 (see Table 3), was taken to determine if the carrots complied with the statutory MRL. Sample number 62132 complied with the MRL.<br />
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Table 13:<br />
Variability <strong>of</strong> methamidophos residues in peaches<br />
Variabilty <strong>of</strong> methamidophos residues in peaches<br />
Results (mg/kg)<br />
Individual peaches<br />
0.019 peach 1<br />
0.046 peach 2<br />
Highest residue detected 0.088 peach 3<br />
0.065 peach 4<br />
0.018 peach 5<br />
0.023 peach 6<br />
0.047 peach 7<br />
Lowest residue detected 0.013 peach 8<br />
0.043 peach 9<br />
0.017 peach 100<br />
Mean residue level 0.038<br />
Ratio <strong>of</strong> highest residue: mean residue 2.3<br />
Ratio <strong>of</strong> highest residue detected: lowest<br />
residue detected 5.2<br />
Calculated sample variability factor for<br />
methamidophos in peaches 2.3x<br />
This sample was taken as a follow up to sample number 61863 which contained a methamidophos residue <strong>of</strong><br />
0.07 mg/kg.<br />
The <strong>Pesticide</strong> <strong>Control</strong> <strong>Service</strong> <strong>of</strong> the <strong>Department</strong> <strong>of</strong> Agriculture and Food and the Food<br />
Safety Authority will continue to have an ongoing dialogue, as part <strong>of</strong> the service contract<br />
between both organisations, with a view to optimising the annual monitoring programme<br />
for pesticide residues in food. This programme will continue to take account <strong>of</strong> the<br />
recommendations from the European Commission with respect to the range <strong>of</strong> crops and<br />
pesticides to be included in the programme.<br />
C VIOLATION INVESTIGATION PROGRAMME<br />
Targeted sampling <strong>of</strong> produce found to be in breach <strong>of</strong> established MRLs is the prime<br />
means <strong>of</strong> determining whether violations that occur result from the systematic misuse <strong>of</strong><br />
pesticides or are isolated incidents. The repeated occurrence <strong>of</strong> excessive residue levels in<br />
particular food commodities, which would result in consumer safety being prejudiced, is<br />
clearly unacceptable. The violation investigation programme is geared to eliminate any<br />
such abuses. The programme is also designed to ensure that incidents where pesticide<br />
MRLs are exceeded are not repeated.<br />
In 2002 eleven targeted samples <strong>of</strong> fruit and vegetables were taken as part <strong>of</strong> the violation<br />
investigation programme. Samples <strong>of</strong> strawberry x2, kiwano, kumquat, passion fruit,<br />
carrots x2, pepper, lettuce, spinach and celery were taken for analysis. None <strong>of</strong> the samples<br />
analysed contained residues in excess <strong>of</strong> the MRL so no additional follow-on action was<br />
required.<br />
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An examination <strong>of</strong> the results <strong>of</strong> the monitoring programmes for 2002 shows that the MRL<br />
exceedances for the 2002 were, in 21 out <strong>of</strong> the 27 samples found to exceed the MRL,<br />
associated with MRLs which have been set at the limit <strong>of</strong> determination. When MRLs are<br />
established at the limit <strong>of</strong> determination it signifies that there is either no legal use <strong>of</strong> the<br />
pesticide on that crop or that the legal use will not result in detectable residues being<br />
present in the harvested food. For those commodities that exceeded an MRL and were<br />
produced within the European Union the MRL breaches confirm that the pesticide was<br />
used illegally. In the case <strong>of</strong> 13 <strong>of</strong> the samples which exceeded the MRL and which were<br />
produced outside <strong>of</strong> the European Union no application has been made to modify the<br />
relevant European Union MRLs that were exceeded. The situation where EU MRLs are<br />
established which do not take account <strong>of</strong> 3 rd country GAP will continue to create problems<br />
for produce imported into the European Union. When such produce are found to contain<br />
pesticide residues which exceed the EU MRL they will be considered to be illegal and will<br />
be subject to penalty under the pesticide residue legislation. Ongoing consultations<br />
between the European Union and 3 rd countries are attempting to resolve these issues.<br />
An assessment <strong>of</strong> the dietary intake associated with the pesticide MRL exceedances<br />
detected in 2002 indicates that they did not present an unacceptable risk for Irish<br />
consumers.<br />
D CONCLUDING REMARKS<br />
The <strong>Department</strong> <strong>of</strong> Agriculture and Food and the Food Safety Authority <strong>of</strong> Ireland<br />
continue to be committed to the strengthening <strong>of</strong> the pesticide residue monitoring<br />
programmes in food, thereby, ins<strong>of</strong>ar as pesticide residues are concerned, ensuring the<br />
safety <strong>of</strong> food for consumers and ensuring the quality <strong>of</strong> produce <strong>of</strong>fered for sale.<br />
This report was compiled through the efforts <strong>of</strong> J. Acton, J. Garvey, M. Lynch and D. O’Sullivan.<br />
The sampling and violation programme was effected by P. Carey, P. Killarney, M. B. Dolan,<br />
D. Murphy and members <strong>of</strong> the Dairy Science and Veterinary Inspectorates. The analytical<br />
results were generated by J. Acton, J. Garvey, Brid McHugh, J. McGannon, D. Carr, F. Morrin,<br />
M. Kelly, T. Walsh, D. Smyth, E. Connolly, J. Coloe, W. Cummins, E. Corbett, M. Graham,<br />
A. Ryan, D. Harris and T. Fuller.<br />
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ANNEX I<br />
REGULATIONS FIXING MAXIMUM LEVELS FOR PESTICIDE RESIDUES IN<br />
AGRICULTURAL PRODUCE<br />
11 European Communities (<strong>Pesticide</strong> Residues) (Fruit and Vegetables) Regulations<br />
1989, S.I. No. 105 <strong>of</strong> 1989<br />
12 European Communities (<strong>Pesticide</strong> Residues) (Fruit and Vegetables) (Amendment)<br />
Regulations 1997, S.I. No. 218 <strong>of</strong> 1997<br />
13 European Communities (<strong>Pesticide</strong> Residues) (Fruit and Vegetables) (Amendment)<br />
Regulations 1998, S.I. No. 563 <strong>of</strong> 1998<br />
14 European Communities (<strong>Pesticide</strong> Residues) (Fruit and Vegetables) (Amendment)<br />
Regulations 2002, S.I. No. 526 <strong>of</strong> 2002<br />
15 European Communities (<strong>Pesticide</strong> Residues) (Feeding stuffs) Regulations 1992, S.I.<br />
No. 40 <strong>of</strong> 1992<br />
16 European Communities (<strong>Pesticide</strong> Residues) (Products <strong>of</strong> Plant Origin, including<br />
Fruit and Vegetables) Regulations 1999, S.I. No. 179 <strong>of</strong> 1999<br />
17 European Communities (<strong>Pesticide</strong> Residues) (Products <strong>of</strong> Plant Origin, including<br />
Fruit and Vegetables) (Amendment) Regulations 1999, S.I. No. 458 <strong>of</strong> 1999<br />
18 European Communities (<strong>Pesticide</strong> Residues) (Products <strong>of</strong> Plant Origin, including<br />
Fruit and Vegetables) (Amendment) Regulations 2000, S.I. No. 461 <strong>of</strong> 2000<br />
19 European Communities (<strong>Pesticide</strong> Residues) (Products <strong>of</strong> Plant Origin, including<br />
Fruit and Vegetables) (Amendment) Regulations 2000, S.I. No. 462 <strong>of</strong> 2000<br />
10 European Communities (<strong>Pesticide</strong> Residues) (Products <strong>of</strong> Plant Origin, including<br />
Fruit and Vegetables) (Amendment) Regulations 2001, S.I. No. 256 <strong>of</strong> 2001<br />
11 European Communities (<strong>Pesticide</strong> Residues) (Products <strong>of</strong> Plant Origin, including<br />
Fruit and Vegetables) (Amendment) Regulations 2001, S.I. No. 621 <strong>of</strong> 2001<br />
12 European Communities (<strong>Pesticide</strong> Residues) (Products <strong>of</strong> Plant Origin, including<br />
Fruit and Vegetables) (Amendment) Regulations 2002, S.I. No. 535 <strong>of</strong> 2002<br />
13 European Communities (<strong>Pesticide</strong> Residues) (Foodstuffs <strong>of</strong> Animal Origin)<br />
Regulations 1999, S.I. No. 180 <strong>of</strong> 1999<br />
14 European Communities (<strong>Pesticide</strong> Residues) (Foodstuffs <strong>of</strong> Animal Origin)<br />
(Amendment) Regulations 1999, S.I. No. 460 <strong>of</strong> 1999<br />
15 European Communities (<strong>Pesticide</strong> Residues) (Foodstuffs <strong>of</strong> Animal Origin)<br />
(Amendment) Regulations 2000, S.I. No. 460 <strong>of</strong> 2000<br />
16 European Communities (<strong>Pesticide</strong> Residues) (Foodstuffs <strong>of</strong> Animal Origin)<br />
(Amendment) Regulations 2000, S.I. No. 249 <strong>of</strong> 2001<br />
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17 European Communities (<strong>Pesticide</strong> Residues) (Foodstuffs <strong>of</strong> Animal Origin)<br />
(Amendment) Regulations 2000, S.I. No. 620 <strong>of</strong> 2001<br />
18 European Communities (<strong>Pesticide</strong> Residues) (Foodstuffs <strong>of</strong> Animal Origin)<br />
(Amendment) Regulations 2002, S.I. No. 534 <strong>of</strong> 2002<br />
19 European Communities (<strong>Pesticide</strong> Residues) (Cereals) Regulations 1999, S.I. No.<br />
181 <strong>of</strong> 1999<br />
20 European Communities (<strong>Pesticide</strong> Residues) (Cereals) (Amendment) Regulations<br />
1999, S.I. No. 459 <strong>of</strong> 1999<br />
21 European Communities (<strong>Pesticide</strong> Residues) (Cereals) (Amendment) Regulations<br />
2000, S.I. No. 459 <strong>of</strong> 2000<br />
22 European Communities (<strong>Pesticide</strong> Residues) (Cereals) (Amendment) Regulations<br />
2001, S.I. No. 250 <strong>of</strong> 2001<br />
23 European Communities (<strong>Pesticide</strong> Residues) (Cereals) (Amendment) Regulations<br />
2001, S.I. No. 622 <strong>of</strong> 2001<br />
24 European Communities (<strong>Pesticide</strong> Residues) (Cereals) (Amendment) Regulations<br />
2002, S.I. No. 533 <strong>of</strong> 2002<br />
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ANNEX II EC DIRECTIVES FIXING MAXIMUM LEVELS FOR PESTICIDE RESIDUES IN<br />
AGRICULTURAL PRODUCE<br />
1 Council Directive <strong>of</strong> 23 November 1976 relating to the fixing <strong>of</strong> maximum levels for<br />
pesticide residues in and on fruit and vegetables. (76/895/EEC) OJ No. L340 <strong>of</strong><br />
9.12.1976,<br />
and amending Directives -<br />
79/700/EEC <strong>of</strong> 24 July 1979 OJ No. L207 <strong>of</strong> 15.8.1979<br />
80/428/EEC <strong>of</strong> 28 March 1980 OJ No. L102 <strong>of</strong> 19.4.1980<br />
81/36/EEC <strong>of</strong> 9 February 1981 OJ No. L46 <strong>of</strong> 19.2.1981<br />
82/528/EEC <strong>of</strong> 19 July 1982 OJ No. L234 <strong>of</strong> 9.8.1982<br />
88/298/EEC <strong>of</strong> 16 May 1988 OJ No. L126 <strong>of</strong> 20.5.1988<br />
89/186/EEC <strong>of</strong> 6 March 1989 OJ No. L66 <strong>of</strong> 10.3.1989<br />
93/58/EEC <strong>of</strong> 29 June 1993 OJ No. L211 <strong>of</strong> 23.8.1993<br />
Corrigendum to 93/58/EEC OJ No. L219 <strong>of</strong> 24.8.1994<br />
96/32/EC <strong>of</strong> 21 May 1996 OJ No. L144 <strong>of</strong> 18.6.1996<br />
97/41/EC <strong>of</strong> 25 June 1997 OJ No. L184 <strong>of</strong> 12.7.1997<br />
2000/24/EC <strong>of</strong> 28 <strong>of</strong> April 2000 OJ No. L107 <strong>of</strong> 04.05.2000<br />
2000/42/EC <strong>of</strong> 22 <strong>of</strong> June 2000 OJ No. L158 <strong>of</strong> 30.06.2000<br />
2000/48/EC <strong>of</strong> 25 <strong>of</strong> July 2000 OJ No. L197 <strong>of</strong> 03.08.2000<br />
2000/57/EC <strong>of</strong> 22 <strong>of</strong> Sept 2000 OJ No. L244 <strong>of</strong> 29.09.2000<br />
2000/82/EC <strong>of</strong> 20 <strong>of</strong> Dec. 2000 OJ No. L3 <strong>of</strong> 06.01.2001<br />
2002/66/EC <strong>of</strong> 16 <strong>of</strong> July 2002 OJ No. L192 <strong>of</strong> 20.07.2002<br />
2 Council Directive <strong>of</strong> 24 July 1986 on the fixing <strong>of</strong> maximum levels for pesticide<br />
residues in and on cereals. (86/362/EEC) OJ No. 221 <strong>of</strong> 7.8.1986<br />
and amending Directives -<br />
88/298/EEC <strong>of</strong> 16 May 1988 OJ No. L126 <strong>of</strong> 20.5.1988<br />
93/57/EEC <strong>of</strong> 29 June 1993 OJ No. L211 <strong>of</strong> 23.8.1993<br />
94/29/EC <strong>of</strong> 23 June 1994 OJ No. L189 <strong>of</strong> 23.7.1994<br />
95/39/EC <strong>of</strong> 17 July 1995 OJ No. L197 <strong>of</strong> 22.8.1995<br />
Corrigendum to 95/39/EC OJ No. L164 <strong>of</strong> 3.7.1996<br />
96/33/EC <strong>of</strong> 21 May 1996 OJ No. L144 <strong>of</strong> 18.6.1996<br />
97/41/EC <strong>of</strong> 25 June 1997 OJ No. L184 <strong>of</strong> 12.7.1997<br />
97/71/EC <strong>of</strong> 15 December 1997 OJ No. L347 <strong>of</strong> 18.12.1997<br />
98/82/EC <strong>of</strong> 27 October 1998 OJ No. L290 <strong>of</strong> 29.10.1998<br />
1999/65/EC <strong>of</strong> 24 June 1999 OJ No. L172 <strong>of</strong> 8.7.1999<br />
1999/71/EC <strong>of</strong> 14 July 1999 OJ No. L194 <strong>of</strong> 27.7.1999<br />
2000/24/EC <strong>of</strong> 28 <strong>of</strong> April 2000 OJ No. L107 <strong>of</strong> 04.05.2000<br />
2000/42/EC <strong>of</strong> 22 <strong>of</strong> June 2000 OJ No. L158 <strong>of</strong> 30.06.2000<br />
2000/48/EC <strong>of</strong> 25 <strong>of</strong> July 2000 OJ No. L197 <strong>of</strong> 03.08.2000<br />
2000/58/EC <strong>of</strong> 22 <strong>of</strong> Sept 2000 OJ No. L244 <strong>of</strong> 29.09.2000<br />
2000/82/EC <strong>of</strong> 20 <strong>of</strong> Dec 2000 OJ No. L3 <strong>of</strong> 06.01.2001<br />
2001/39/EU <strong>of</strong> 23 <strong>of</strong> May 2001 OJ No. L148 <strong>of</strong> 01.05.2001<br />
2001/48/EU <strong>of</strong> 28 <strong>of</strong> June 2001 OJ No. L180 <strong>of</strong> 03.07.2001<br />
2001/57/EU <strong>of</strong> 25 <strong>of</strong> July 2001 OJ No. L208 <strong>of</strong> 01.08.2001<br />
2002/23/EU <strong>of</strong> 26 <strong>of</strong> Feb 2002 OJ No. L64 <strong>of</strong> 07.03.2002<br />
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ANNEX II Continued<br />
3 Council Directive <strong>of</strong> 24 July 1986 on the fixing <strong>of</strong> maximum levels for pesticide<br />
residues in and on foodstuffs <strong>of</strong> animal origin. (86/363/EEC) OJ No. L221 <strong>of</strong><br />
7.8.1986<br />
and amending Directives -<br />
93/57/EEC <strong>of</strong> 29 June 1993 OJ No. L211 <strong>of</strong> 23.8.1993<br />
94/29/EC <strong>of</strong> 23 June 1994 OJ No. L189 <strong>of</strong> 23.7.1994<br />
95/39/EC <strong>of</strong> 17 July 1995 OJ No. L197 <strong>of</strong> 22.8.1995<br />
Corrigendum <strong>of</strong> 95/39/EC OJ No. L164 <strong>of</strong> 3.7.1996<br />
96/33/EC <strong>of</strong> 21 May 1996 OJ No. L144 <strong>of</strong> 18.6.1996<br />
97/41/EC <strong>of</strong> 25 June 1997 OJ No. L184 <strong>of</strong> 12.7.1997<br />
97/71/EC <strong>of</strong> 15 December 1997 OJ No. L347 <strong>of</strong> 18.12.1997<br />
98/82/EC <strong>of</strong> 27 October 1998 OJ No. L290 <strong>of</strong> 29.10.1998<br />
1999/71/EC <strong>of</strong> 14 July 1999 OJ No. L194 <strong>of</strong> 27.7.1999<br />
2000/24/EC <strong>of</strong> 28 <strong>of</strong> April 2000 OJ No. L107 <strong>of</strong> 04.05.2000<br />
2000/42/EC <strong>of</strong> 22 <strong>of</strong> June 2000 OJ No. L158 <strong>of</strong> 30.06.2000<br />
2000/58/EC <strong>of</strong> 22 <strong>of</strong> Sept 2000 OJ No. L244 <strong>of</strong> 29.09.2000<br />
2000/82/EC <strong>of</strong> 20 <strong>of</strong> Dec 2000 OJ No. L3 <strong>of</strong> 06.01.2001<br />
2001/39/EU <strong>of</strong> 23 <strong>of</strong> May 2001 OJ No. L148 <strong>of</strong> 01.05.2001<br />
2001/57/EU <strong>of</strong> 25 <strong>of</strong> July 2001 OJ No. L208 <strong>of</strong> 01.08.2001<br />
2002/23/EU <strong>of</strong> 26 <strong>of</strong> Feb 2002 OJ No. L64 <strong>of</strong> 07.03.2002<br />
4 Council Directive <strong>of</strong> 27 November 1990 on the fixing <strong>of</strong> maximum levels for<br />
pesticide residues in an on certain products <strong>of</strong> plant origin, including fruit and<br />
vegetables. (90/642/EEC) OJ No. L350 <strong>of</strong> 14.12.1990<br />
and amending Directives -<br />
93/58/EEC <strong>of</strong> 29 June 1993 OJ No. L211 <strong>of</strong> 23.8.1993<br />
Corrigendum to 93/58 EEC OJ No. L219 <strong>of</strong> 24.8.1994<br />
94/30/EC <strong>of</strong> 23 June 1994 OJ No. L189 <strong>of</strong> 23.7.1994<br />
95/38/EC <strong>of</strong> 17 July 1995 OJ No. L197 <strong>of</strong> 22.8.1995<br />
Corrigendum to 95/38/EEC OJ No. L155 <strong>of</strong> 28.6.1996<br />
95/61/EC <strong>of</strong> 29 November 1995 OJ No. L292 <strong>of</strong> 7.12.1995<br />
96/32/EC <strong>of</strong> 21 May 1996 OJ No. L144 <strong>of</strong> 18.6.1996<br />
97/41/EC <strong>of</strong> 25 June 1997 OJ No. L184 <strong>of</strong> 12.7.1997<br />
97/71/EC <strong>of</strong> 15 December 1997 OJ No. L347 <strong>of</strong> 18.12.1997<br />
98/82/EC <strong>of</strong> 27 October 1998 OJ No. L290 <strong>of</strong> 29.10.1998<br />
1999/65/EC <strong>of</strong> 24 June 1999 OJ No. L172 <strong>of</strong> 8.7.1999<br />
1999/71/EC <strong>of</strong> 14 July 1999 OJ No. L194 <strong>of</strong> 27.7.1999<br />
2000/24/EC <strong>of</strong> 28 <strong>of</strong> April 2000 OJ No. L107 <strong>of</strong> 04.05.2000<br />
2000/42/EC <strong>of</strong> 22 <strong>of</strong> June 2000 OJ No. L158 <strong>of</strong> 30.06.2000<br />
2000/48/EC <strong>of</strong> 25 <strong>of</strong> July 2000 OJ No. L197 <strong>of</strong> 03.08.2000<br />
2000/57/EC <strong>of</strong> 22 <strong>of</strong> Sept 2000 OJ No. L244 <strong>of</strong> 29.09.2000<br />
2000/58/EC <strong>of</strong> 22 <strong>of</strong> Sept 2000 OJ No. L244/78 <strong>of</strong> 29.09.2000<br />
2000/82/EC <strong>of</strong> 20 <strong>of</strong> Dec 2000 OJ No. L3/18 <strong>of</strong> 06.01.2001<br />
2001/35/EU <strong>of</strong> 11 <strong>of</strong> May 2001 OJ No. L136 <strong>of</strong> 18.05.2001<br />
2001/39/EU <strong>of</strong> 23 <strong>of</strong> May 2001 OJ No. L148 <strong>of</strong> 01.05.2001<br />
2001/48/EU <strong>of</strong> 28 <strong>of</strong> June 2001 OJ No. L180 <strong>of</strong> 03.07.2001<br />
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ANNEX II Continued<br />
2001/57/EU <strong>of</strong> 25 <strong>of</strong> July 2001 OJ No. L208 <strong>of</strong> 01.08.2001<br />
2002/5/EU <strong>of</strong> 30 <strong>of</strong> Jan 2002 OJ No. L34 <strong>of</strong> 05.02.2002<br />
2002/23/EU <strong>of</strong> 26 <strong>of</strong> Feb 2002 OJ No. L64 <strong>of</strong> 07.03.2002<br />
5 Council Directive <strong>of</strong> 4 March 1991, amending Directive 74/63/EEC on undesirable<br />
substances and products in animal nutrition. (91/132/EEC) OJ No. L66 <strong>of</strong> 13.3.1991<br />
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ANNEX III<br />
GLOSSARY OF TERMS<br />
Acceptable Daily Intake (ADI)<br />
An ADI is an estimate <strong>of</strong> the amount <strong>of</strong> a residue in food or<br />
drinking water, expressed on a body weight basis, that can be<br />
ingested daily over a lifetime without appreciable health risk.<br />
The particular vulnerability <strong>of</strong> infants, children, the elderly and<br />
those whose systems are under stress because <strong>of</strong> ill-health, are<br />
taken into account, through application <strong>of</strong> a safety factor, when<br />
ADI values are established.<br />
ADI values are based on the no-adverse-effect level in the most<br />
sensitive animal species used in the toxicological experiments,<br />
or if appropriate data are available, in humans. Invariably, a<br />
safety factor to account for inter-species and intra-species<br />
variations is applied. Studies used as a basis for the identification<br />
<strong>of</strong> the relevant no-adverse-effect levels and hence for deriving<br />
ADI values, are conducted using active substance as<br />
manufactured. Accordingly the toxicological effects <strong>of</strong><br />
impurities present in active substances are included in the<br />
assessment. Account is also taken <strong>of</strong> metabolites that may<br />
influence the toxicological significance <strong>of</strong> the residue reaching<br />
the consumer.<br />
Acute Reference Dose (ARfD)<br />
An ARfD is similar in nature to an ADI but it relates to intake <strong>of</strong><br />
residues at one meal or on one day.<br />
The particular vulnerability <strong>of</strong> infants, children, the elderly and<br />
those whose systems are under stress because <strong>of</strong> ill-health, are<br />
taken into account, through application <strong>of</strong> a safety factor, when<br />
ARfD values are established.<br />
ARfD values are based on the no-adverse effect level in the most<br />
sensitive animal species used in the toxicological<br />
experimentation, or if appropriate data are available, in humans.<br />
ARfD values are derived from the results <strong>of</strong> those toxicological<br />
studies that are most relevant to short term exposure.<br />
Good Agricultural Practice (GAP)<br />
Lowest Calibrated Level (LCL)<br />
GAP in the use <strong>of</strong> a plant protection product (pesticide) includes<br />
authorized use under practical conditions necessary for effective<br />
control <strong>of</strong> harmful organisms. It encompasses a range <strong>of</strong> levels<br />
<strong>of</strong> application up to the highest level authorized, applied in a<br />
manner that leaves a residue that is the smallest amount<br />
practicable.<br />
The lowest concentration <strong>of</strong> a pesticide residue with which the<br />
detection system is calibrated for the purposes <strong>of</strong> determining<br />
the presence or absence <strong>of</strong> measurable residues. It normally also<br />
serves to define the reporting limit for individual pesticide<br />
residues.<br />
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ANNEX III Continued<br />
Limit <strong>of</strong> Determination (LOD)<br />
Matrix Matched Calibration<br />
The LOD is the lowest concentration <strong>of</strong> a pesticide residue o<br />
contaminant that can be identified and quantitatively measured<br />
in a specified food, agricultural commodity or animal feed, with<br />
an acceptable degree <strong>of</strong> certainty by a method <strong>of</strong> analysis.<br />
A system involving use <strong>of</strong> calibration solutions to ensure that all<br />
constituents (other than the analyte) are similar to, or produce the<br />
same effect on analytical response as the equivalent solutions<br />
generated from the samples to be analyzed.<br />
The objectives <strong>of</strong> matrix-matched calibration are to compensate<br />
for analyte response enhancement or suppression effects induced<br />
by sample co-extractives and to provide a chromatogram that has<br />
underlying interference comparable to that <strong>of</strong> the sample.<br />
Matrix blanks are prepared using solvents, reagents and clean-up<br />
procedures similar to those used for analysis <strong>of</strong> samples to be<br />
analyzed. In practice the pesticide is added to a blank extract <strong>of</strong><br />
a matrix similar to that to be analyzed. The matrix used may<br />
differ from that <strong>of</strong> the samples if it is shown to achieve the stated<br />
objectives.<br />
Maximum Residue Limits (MRLs)<br />
An MRL is the maximum concentration <strong>of</strong> a pesticide residue,<br />
expressed in milligrams per kilogram, legally permitted in or on<br />
food commodities and animal feeds. MRLs are based on<br />
supervised residues trials data that reflect Good Agricultural<br />
Practice (GAP). MRLs established for particular food<br />
commodities are such that potential consumer exposure to<br />
residues is judged to be toxicologically acceptable.<br />
MRLs are fixed at or about the limit <strong>of</strong> determination, where<br />
there are no approved uses.<br />
MRLs are established on the basis <strong>of</strong> sound scientific<br />
knowledge. They are only established for those pesticides for<br />
which acceptable daily intake (ADI) values exist<br />
No-adverse-effect Level<br />
<strong>Pesticide</strong> Residue<br />
The no-adverse-effect level is the highest level <strong>of</strong> continual<br />
exposure to a chemical that causes no significant adverse effect<br />
on morphology, biochemistry, functional capacity, growth,<br />
development, or life span <strong>of</strong> individuals <strong>of</strong> the target species that<br />
may be animal or human.<br />
Any trace <strong>of</strong> a pesticide found in a sample, including any<br />
specified derivatives such as degradation and conversion<br />
products, metabolites and impurities, which are considered to be<br />
<strong>of</strong> toxicological significance and are included in the residue<br />
definition.<br />
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ANNEX IV<br />
ANALYTICAL METHODS AND PROCEDURES EMPLOYED FOR THE<br />
DETERMINATION OF PESTICIDE RESIDUES IN FOODSTUFFS<br />
The methods <strong>of</strong> analysis currently used in the pesticide residue laboratory include<br />
those described hereunder.<br />
ii(i)<br />
Multi residue method 1, Analytical Methods for <strong>Pesticide</strong> Residues in<br />
Foodstuffs, 6th edition, 1996, General Inspectorate for Health Problems,<br />
Ministry <strong>of</strong> Public Health, Welfare and Sport, The Netherlands. The method is<br />
used to determine residues <strong>of</strong> organophosphorous, organochlorine and<br />
benzimidazole pesticides in food <strong>of</strong> plant origin.<br />
Note: A variation <strong>of</strong> the method is used. The variation involves addition <strong>of</strong><br />
sodium sulphate at the time <strong>of</strong> sample extraction to facilitate the extraction <strong>of</strong><br />
polar organophosphorous pesticides.<br />
i(ii)<br />
(iii)<br />
(iv)<br />
Multi residue method 1, Analytical Methods for <strong>Pesticide</strong> Residues in<br />
Foodstuffs, 6th edition, 1996, General Inspectorate for Health Problems,<br />
Ministry <strong>of</strong> Public Health, Welfare and Sport, The Netherlands. The variation <strong>of</strong><br />
the method uses ethyl acetate as the extraction solvent and is used for the<br />
analysis <strong>of</strong> residues <strong>of</strong> organophosphorous, organochlorine and benzimidazole<br />
pesticides in cereals.<br />
The Becker method, A multi residue method for the simultaneous determination<br />
<strong>of</strong> plant protection chemicals in plant material, Dtsch. Lebensm. Rundsch. 75,<br />
148-152, 1979, using a gel permeation column instead <strong>of</strong> the silica gel/activated<br />
charcoal column specified.<br />
The method in use for the determination <strong>of</strong> organochlorine and organophosphorous<br />
residues in samples <strong>of</strong> fat is based on clean-up method number 5<br />
<strong>of</strong> the German Manual <strong>of</strong> <strong>Pesticide</strong> Residue Analysis (Volume 1 <strong>of</strong> 1987) and<br />
involves extraction with a mixture <strong>of</strong> acetonitrile and acetone, followed by<br />
clean-up using gel permeation chromatography column and alumina/silver<br />
nitrate micro columns (for organochlorine pesticides only).<br />
The method for the analysis <strong>of</strong> benzimidazole compounds in use is based on that<br />
developed by Hiemstra, M., J.A. Joosten and A. de Kok, J. AOAC Int. 78, 1267 -1274,<br />
1995. A fully automated solid-phase extraction cleanup and an on-line liquid<br />
chromatographic system, using a UV detector, is used for the determination <strong>of</strong> the<br />
benzimidazole fungicides carbendazim, benomyl and thiophanate-methyl (determined<br />
as carbendazim) and thiabendazole, in fruit and vegetables.<br />
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Annex V<br />
<strong>Pesticide</strong>s determined in Fruit, Vegetables, Cereals and Honey.<br />
Organochlorine<br />
Lowest Calibrated Level (LCL)<br />
Compounds.<br />
(in milligrams per kilogram – ppm)<br />
aldrin 0.03<br />
bifenthrin 0.06<br />
binapacryl 0.03<br />
bromopropylate 0.03<br />
captafol 0.02<br />
captan** 0.03<br />
α-chlordane 0.02<br />
γ-chlordane 0.02<br />
chlorothalonil** 0.02<br />
cyfluthrin 0.04<br />
λ-cyhalothrin 0.02<br />
cypermethrin 0.07<br />
deltamethrin 0.05<br />
pp’DDT 0.02<br />
op’DDT 0.02<br />
pp’DDE 0.02<br />
op’DDE 0.03<br />
pp’DDD 0.02<br />
op’DDD 0.03<br />
dichl<strong>of</strong>luanid 0.03<br />
dic<strong>of</strong>ol 0.05<br />
dieldrin 0.02<br />
α-endosulfan** 0.02<br />
β-endosulfan 0.03<br />
endosulfate 0.02<br />
endrin 0.02<br />
fenarimol 0.05<br />
fenvalerate 0.06<br />
folpet 0.02<br />
HCB 0.02<br />
α-HCH 0.02<br />
β-HCH 0.04<br />
δ-HCH 0.02<br />
heptachlor 0.02<br />
heptachlor-epoxide 0.02<br />
iprodione 0.07<br />
lindane (γ-HCH) 0.02<br />
methoxychlor 0.04<br />
permethrin ** 0.2<br />
procymidone 0.1<br />
propyzamide 0.09<br />
quintozene 0.02<br />
tecnazene 0.03<br />
tetradifon 0.03<br />
tolyfluanid 0.03<br />
vinclozolin 0.02<br />
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ANNEX V<br />
Continued<br />
Organophosphorous<br />
Lowest Calibrated Level (LCL)<br />
and other Compounds.<br />
(in milligrams per kilogram – ppm)<br />
Acephate 0.05<br />
Azinphos-methyl 0.1<br />
Azinphos-ethyl 0.1<br />
Bromophos-ethyl 0.05<br />
Bromophos-methyl 0.05<br />
Chlorfenvinphos 0.06<br />
Chlorpyrifos 0.06<br />
Chlorpyrifos-methyl 0.05<br />
Demeton-S-Me-sulfone 0.06<br />
Diazinon 0.05<br />
Dichlorvos 0.04<br />
Dimethoate 0.05<br />
Ethion 0.05<br />
Etrimfos 0.04<br />
Fenchlorphos 0.02<br />
Fenitrothion 0.04<br />
Fon<strong>of</strong>os 0.05<br />
Heptenophos 0.05<br />
Iod<strong>of</strong>enphos 0.03<br />
Is<strong>of</strong>enphos 0.05<br />
Malaoxon 0.05<br />
Malathion 0.04<br />
Methacrifos 0.04<br />
Methamidophos ** 0.04<br />
Methidathion 0.04<br />
Mevinphos 0.04<br />
Monocrotophos 0.05<br />
Omethoate ** 0.05<br />
Paraoxon 0.05<br />
Paraoxon-methyl 0.04<br />
Parathion 0.05<br />
Parathion-methyl 0.05<br />
Phosalone 0.1<br />
Phosmet 0.11<br />
Phosphamidon 0.04<br />
Pirimifos-ethyl 0.05<br />
Pirimifos-methyl 0.05<br />
Propetamphos 0.05<br />
Quinalphos 0.04<br />
Tolcl<strong>of</strong>os-methyl 0.05<br />
Triazophos 0.03<br />
Thiabendazole ** 0.05<br />
Carbendazim ** 0.05<br />
**= These pesticides are not included in the scope <strong>of</strong> the accreditation granted by NAB<br />
in 2000.<br />
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Annex VI<br />
<strong>Pesticide</strong>s determined in Bovine, Porcine, Ovine, Poultry and Venison Kidney Fat.<br />
Organochlorine<br />
Lowest Calibrated Level (LCL)<br />
compounds & PCB<br />
(in milligrams per kilogram <strong>of</strong> fat – ppm)<br />
congeners<br />
Aldrin 0.006<br />
α-Chlordane 0.006<br />
β-Chlordane 0.006<br />
pp’DDT 0.005<br />
op’DDT 0.005<br />
pp’DDE 0.005<br />
op’DDE 0.005<br />
pp’DDD 0.005<br />
op’DDD 0.006<br />
Dieldrin 0.005<br />
Dic<strong>of</strong>ol 0.01<br />
α-Endosulfan 0.005<br />
β-Endosulfan 0.006<br />
Endrin 0.005<br />
HCB 0.005<br />
α-HCH 0.005<br />
β-HCH 0.008<br />
δ-HCH 0.005<br />
Heptachlor 0.005<br />
Heptachlor-epoxide 0.005<br />
Lindane (γ-HCH) 0.005<br />
PCB 28 0.01<br />
PCB 52 0.01<br />
PCB 101 0.01<br />
PCB 118 0.01<br />
PCB 138 0.01<br />
PCB 153 0.01<br />
PCB 180 0.01<br />
Permethrin 0.04<br />
Quintozene 0.005<br />
Tecnazene 0.005<br />
Organophosphorous<br />
Compounds.<br />
Lowest Calibrated Level (LCL)<br />
(in milligrams per kilogram <strong>of</strong> fat – ppm)<br />
Azinphos-Ethyl 0.2<br />
Azinphos-Methyl 0.2<br />
Bromophos-Ethyl 0.1<br />
Bromophos-Methyl 0.1<br />
Chlorfenvinphos 0.1<br />
Chlorpyrifos 0.1<br />
Chlorpyrifos-Methyl 0.1<br />
Diazinon 0.1<br />
Dichlorvos 0.1<br />
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Annex VI<br />
Continued<br />
Organophosphorous<br />
Compounds.<br />
Lowest Calibrated Level (LCL)<br />
(in milligrams per kilogram <strong>of</strong> fat – ppm)<br />
Dimethoate 0.1<br />
Ethion 0.1<br />
Fenchlorphos 0.04<br />
Fon<strong>of</strong>os 0.1<br />
Iod<strong>of</strong>enphos 0.08<br />
Malathion 0.1<br />
Methidathion 0.08<br />
Mevinphos 0.08<br />
Parathion 0.1<br />
Parathion-methyl 0.1<br />
Phosalone 0.2<br />
Pirimifos-ethyl 0.1<br />
Pirimifos-methyl 0.1<br />
Propetamphos 0.1<br />
Triazophos 0.06<br />
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Annex VII<br />
<strong>Pesticide</strong>s determined in Milk<br />
Organochlorine<br />
Compounds and PCB<br />
Congeners.<br />
Lowest Calibrated Level (LCL)<br />
(in milligrams per kilogram – ppm)<br />
Aldrin 0.006<br />
α-Chlordane 0.006<br />
γ-Chlordane 0.006<br />
Dieldrin 0.005<br />
pp’DDT 0.005<br />
op’DDT 0.005<br />
pp’DDE 0.005<br />
op’DDE 0.005<br />
pp’DDD 0.005<br />
op’DDD 0.006<br />
Dic<strong>of</strong>ol 0.01<br />
α-Endosulfan 0.005<br />
β-Endosulfan 0.006<br />
Endrin 0.005<br />
HCB 0.005<br />
α-HCH 0.005<br />
β-HCH 0.008<br />
γ-HCH 0.005<br />
Heptachlor 0.005<br />
Heptachlor-epoxide 0.005<br />
Lindane (γ-HCH) 0.005<br />
PCB 28 0.01<br />
PCB 52 0.01<br />
PCB 101 0.01<br />
PCB 118 0.01<br />
PCB 138 0.01<br />
PCB 153 0.01<br />
PCB 180 0.01<br />
Permethrin 0.04<br />
Quintozene 0.005<br />
Tecnazene 0.005<br />
Organophosphorous<br />
Compounds.<br />
Lowest Calibrated Level (LCL)<br />
(in milligrams per kilogram – ppm)<br />
Azinphos-Ethyl 0.2<br />
Azinphos-Methyl 0.2<br />
Bromophos-Ethyl 0.1<br />
Bromophos-Methyl 0.1<br />
Chlorfenvinphos 0.1<br />
Chlorpyrifos 0.1<br />
Chlorpyrifos-Methyl 0.1<br />
Diazinon 0.1<br />
Dichlorvos 0.1<br />
Dimethoate 0.1<br />
Ethion 0.1<br />
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Annex VII<br />
Continued.<br />
Organophosphorous<br />
Compounds.<br />
Lowest Calibrated Level (LCL)<br />
(in milligrams per kilogram – ppm)<br />
Fenchlorphos 0.04<br />
Fon<strong>of</strong>os 0.1<br />
Iod<strong>of</strong>enphos 0.08<br />
Malathion 0.1<br />
Methidathion 0.08<br />
Mevinphos 0.08<br />
Parathion 0.1<br />
Parathion-Methyl 0.1<br />
Phosalone 0.2<br />
Pirimifos-ethyl 0.1<br />
Pirimifos-methyl 0.1<br />
Propetamphos 0.1<br />
Triazophos 0.06<br />
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ANNEX VIII SUMMARY OF THE RESULTS OF THE QUALITY ASSURANCE<br />
PROGRAMME FOR ANALYTICAL METHODS<br />
1. Fruit and Vegetables<br />
Organochlorine <strong>Pesticide</strong>s<br />
The results <strong>of</strong> the recovery studies carried out are presented in terms <strong>of</strong> percentage<br />
mean recovery, standard deviation <strong>of</strong> the mean recovery and co-efficient <strong>of</strong> variation:<br />
63 samples [ Courgette (1), Strawberry (5), Carrot (6), Bean (6), Pea (1), Tomato (4),<br />
Lemon (1), Melon (3), Kiwi (3), Broccoli (2), Raspberry (1), Mango (1), Swede (1),<br />
Celery (2), Cucumber (6), Lettuce (2), Aubergine (2), Grape (1), Potato (2), Mushroom<br />
(1), Pepper (1), Spinach (2), Rhubarb (1), Pineapple (2), Apple (2), Plum (2),<br />
Blueberry (1), Honey (1)] were spiked with an organochlorine mixture (Mix 1)<br />
containing 14 different pesticides and metabolites.<br />
Mix 1 Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery (%) Deviation <strong>of</strong> Variation<br />
Aldrin 0.03 - 0.2 92.0 12.5 13.6<br />
Captan 0.03 - 0.2 98.8 15.9 16.6<br />
Chlorothalonil 0.02 - 0.13 93.5 16.9 18.1<br />
Cypermethrin 0.07 - 0.5 96.2 10.3 10.7<br />
Deltamethrin 0.05 - 0.34 95.4 11.4 11.9<br />
pp-DDD 0.02 - 0.14 93.6 11.2 11.9<br />
pp-DDE 0.02 - 0.12 94.0 13.5 14.4<br />
pp- DDT 0.02 - 0.14 93.4 10.7 11.5<br />
α- Endosulfan 0.02 - 0.13 90.9 14.2 15.6<br />
Endrin 0.02 - 0.13 95.0 10.8 11.4<br />
HCB 0.02 - 0.13 89.7 12.1 13.5<br />
Lindane 0.02 - 0.12 93.7 14.5 15.5<br />
Methoxychlor 0.04 - 0.26 94.0 10.3 10.9<br />
Permethrin 0.2 - 1.3 93.2 14.5 15.6<br />
17 Samples [Tomato (1), Bean (2), Cabbage (1), Melon (2), Raspberry (1), Mango (1),<br />
Tomato (1), Aubergine (2), Carrot (1), Spinach (1), Cucumber (1), Strawberry (2)]<br />
were spiked with a second organochlorine pesticide mixture (Mix 2) containing 12<br />
different pesticides and metabolites.<br />
Mix 2 Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery Deviation <strong>of</strong> Variation<br />
op-DDD 0.03 – 0.21 91.1 6.9 7.5<br />
op-DDE 0.03 – 0.20 95.1 4.4 4.7<br />
op-DDT 0.02 – 0.13 91.9 9.1 9.9<br />
Dieldrin 0.02 – 0.14 86.2 13.7 15.9<br />
Endosulfate 0.02 – 0.13 94.6 5.7 6.0<br />
Fenvalerate 0.06 – 0.40 96.5 6.9 7.1<br />
α-HCH 0.02 – 0.13 92.5 6.1 6.6<br />
Heptachlor 0.02 – 0.14 101.2 21.6 21.3<br />
Heptachlorepoxide<br />
0.02 – 0.13 93.5 4.6 5.0<br />
Iprodione 0.07 – 0.50 97.1 5.8 5.9<br />
Quintozene<br />
Tetradifon<br />
0.02 – 0.14<br />
0.03 – 0.2<br />
92.3<br />
92.3<br />
4.4<br />
4.3<br />
4.8<br />
4.6<br />
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13 samples [Pea (1), Potato (3), Carrot (1), Tomato (2), Bean (1), Celery (1), Lettuce<br />
(1), Spinach (1), Cucumber (1), Pineapple (1)] were spiked with a third organochlorine<br />
mixture (Mix 3) containing 8 different pesticides and metabolites.<br />
Mix 3 Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery Deviation <strong>of</strong> Variation<br />
Captafol 0.02 – 0.13 90.3 9.2 10.1<br />
Dic<strong>of</strong>ol 0.05 – 0.33 84.9 9.5 11.2<br />
b-Endosulfan 0.03 – 0.20 92.7 8.7 9.4<br />
Fenarimol 0.05 – 0.33 95.9 8.4 8.8<br />
β-HCH 0.04 – 0.13 85.8 10.0 11.7<br />
δ-HCH 0.02 – 0.30 91.8 12.9 14.1<br />
Procymidone 0.10 – 0.66 96.4 14.5 15.0<br />
Tecnazene 0.02 – 0.13 80.6 14.1 17.5<br />
16 samples [ Strawberry (2), Bean (1), Kiwi (2), Grape (1), Raspberry (1), Tomato (1),<br />
Celery (1), Melon (2), Aubergine (1), Pepper (1), Rhubarb (1), Cucumber (1), Honey<br />
(1)] were spiked with a fourth organochlorine mixture (Mix 4) containing 9 different<br />
pesticides.<br />
Mix 4 Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery Deviation <strong>of</strong> Variation<br />
Bifenthrin 0.06 – 0.40 95.9 4.1 4.3<br />
Binapacryl 0.03 – 0.20 95.2 5.3 5.6<br />
Bromopropylate 0.03 – 0.21 96.8 4.1 4.3<br />
Cyfluthrin 0.04 – 0.27 99.8 10.2 10.2<br />
λ-Cyhalothrin 0.02 – 0.15 94.7 4.6 4.9<br />
Dicl<strong>of</strong>luanid 0.03 – 0.21 96.4 5.3 5.3<br />
Folpet 0.02 – 0.11 99.5 4.8 4.8<br />
Propyzamide 0.10 – 0.60 102.5 9.9 9.7<br />
Vinclozolin 0.02 – 0.11 96.8 4.9 5.1<br />
11 Samples [Courgette (1), Bean (1), Carrot (4), Strawberry (1), Broccoli (1), Spinach<br />
(1), Pineapple (1), Apple (1)] were spiked with a fifth organochlorine mixture (Mix 5)<br />
containing 3 different pesticides.<br />
Mix 5 Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery Deviation <strong>of</strong> Variation<br />
α-Chlordane 0.02 – 0.13 94.5 9.2 9.7<br />
γ-Chlordane 0.02 – 0.13 94.0 9.6 10.3<br />
Tolyfluanid 0.02 – 0.13 93.2 9.6 10.3<br />
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Organophosphorous <strong>Pesticide</strong>s<br />
The results <strong>of</strong> the recovery studies carried out are presented in terms <strong>of</strong> percentage<br />
mean recovery, standard deviation <strong>of</strong> the mean recovery and co-efficient <strong>of</strong> variation:<br />
66 samples [Courgette (1), Strawberry (6), Tomato (4), Lemon (1), Bean (6), Pea (1),<br />
Mangetout (1), Melon (3), Raspberry (1), Carrot (10), Potato (2), Kiwi (2), Broccoli<br />
(2), Mango (1), Cucumber (4), Swede (1), Celery (1), Lettuce (2), Aubergine (3),<br />
Mushroom (1), Sweet Potato (1), Grape (1), Pepper (1), Spinach (2), Rhubarb (1),<br />
Pineapple (2), Apple (2), Plum (1), Honey (1)] <strong>of</strong> fruit and vegetables were spiked with<br />
an organophosphorous pesticide mixture (Mix 20) containing 13 different pesticides.<br />
Mix 20 Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery Deviation <strong>of</strong> Variation<br />
Azinphos-Me 0.10 – 0.60 97.6 10.4 10.6<br />
Chlorpyrifos 0.06 – 0.30 95.6 8.5 8.9<br />
Chlorfenvinphos 0.06 – 0.32 95.3 10.7 11.2<br />
Diazinon 0.05 – 0.26 97.9 9.7 10.0<br />
Dimethoate 0.05 – 0.27 99.0 11.0 11.2<br />
Ethion 0.05 – 0.26 99.1 10.3 10.4<br />
Malathion 0.05 – 0.26 96.3 9.3 9.6<br />
Metamidaphos 0.04 – 0.20 92.2 44.1 47.8<br />
Methidathion 0.04 – 0.21 97.3 10.6 10.9<br />
Omethoate 0.05 – 0.27 86.0 17.0 19.8<br />
Phosmet 0.11 – 0.56 96.5 11.8 12.1<br />
Tolcl<strong>of</strong>os-Me 0.05 – 0.25 94.9 8.7 9.2<br />
Triazophos 0.03 – 0.16 98.4 11.0 11.2<br />
16 samples [Tomato (2), Bean (2), Cabbage (1), Melon (2), Raspberry (1), Mango (1),<br />
Aubergine (2), Carrot (1), Spinach (1), Cucumber (1), Strawberry (1)] were spiked<br />
with a second organophosphorous pesticide mixture (Mix 21) containing 11 different<br />
pesticides and metabolites.<br />
Mix 21 Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery Deviation <strong>of</strong> Variation<br />
Azinphos-et 0.10 – 0.47 96.4 5.8 6.0<br />
Dichlorvos 0.04 – 0.20 79.1 12.8 16.2<br />
Heptenophos 0.05 – 0.24 92.5 9.1 9.9<br />
Iod<strong>of</strong>enphos 0.03 – 0.16 92.9 6.3 6.8<br />
Mevinphos 0.04 – 0.19 91.1 9.4 10.3<br />
Paraoxon 0.05 – 0.24 92.2 6.8 7.3<br />
Paraoxon-me 0.04 – 0.18 91.7 5.9 6.4<br />
Parathion 0.05 – 0.24 95.6 6.6 6.9<br />
Phosphamidon 0.04 – 0.20 93.4 6.3 6.7<br />
Phosalone 0.10 – 0.50 95.9 6.0 6.2<br />
Quinalphos 0.04 – 0.19 96.8 5.4 5.5<br />
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19 samples [Strawberry (2), Pea (1), Potato (1), Carrot (2), Tomato (2), Celery (1),<br />
Cabbage (1), Aubergine (1), Bean (3), Lettuce (1), Mushroom (1), Apple (2), Honey<br />
(1)] were spiked with a third organophosphorous mixture (Mix 22) containing 6<br />
different pesticides.<br />
Mix 22 Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery Deviation <strong>of</strong> Variation<br />
Acephate 0.05 – 0.25 83.9 16.8 20.0<br />
Bromophos-me 0.05 – 0.25 95.2 10.6 11.1<br />
Is<strong>of</strong>enphos 0.05 – 0.23 125.1 53.4 42.7<br />
Fenchlorphos 0.02 – 0.10 96.1 6.9 7.2<br />
Malaoxon 0.05 – 0.23 96.8 8.2 8.4<br />
Propetamphos 0.05 – 0.24 1110.1 14.0 12.7<br />
Note: the information generated indicates that the pesticide Is<strong>of</strong>enphos is not easy to analyse and if<br />
encountered in samples special care should be taken when interpreting results.<br />
14 samples [Mangetout (1), Kiwi (2), Plum (1), Carrot (2), Sweet Potato (1), Pepper<br />
(1), Potato (1), Spinach (1), Cucumber (1), Strawberry (1), Pineapple (1)] were spiked<br />
with a fourth organophosphorous pesticide mixture (Mix 23) containing 6 different<br />
pesticides.<br />
Mix 23 Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery Deviation <strong>of</strong> Variation<br />
Bromophos-Et 0.05 – 0.24 96.7 7.0 7.2<br />
Chlorpyrifos-Me 0.05 – 0.23 96.6 7.9 8.2<br />
Methacrifos 0.01 – 0.21 90.1 11.1 12.3<br />
Pirimphos-Et 0.05 – 0.23 100.3 7.9 7.9<br />
Pirimphos-Me 0.05 – 0.23 96.7 6.4 6.6<br />
13 samples [Courgette (1), Broccoli (2), Carrot (2), Lettuce (1), Bean (2), Grape (1),<br />
Melon (1), Cucumber (1), Rhubarb (1), Pineapple (1)] were spiked with a fifth<br />
organophosphorous pesticide mixture (M24) containing 5 different pesticides.<br />
Mix 24 Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery Deviation <strong>of</strong> Variation<br />
Demeton-S-Me-Sulfone 0.05 – 0.25 100.4 10.6 10.6<br />
Fenithrothion 0.04 – 0.22 99.0 8.7 8.8<br />
Fon<strong>of</strong>os 0.05 – 0.25 309.4 446.7 144.4<br />
Monocrotophos 0.05 – 0.27 97.3 8.0 8.2<br />
Parathion-Me 0.05 – 0.25 97.2 5.0 5.2<br />
Note: As in the case <strong>of</strong> Is<strong>of</strong>enphos the recover data for Fonophos indicates that if residues <strong>of</strong> this pesticide<br />
are detected in samples special care should be taken when interpreting the results.<br />
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Benzimidazole <strong>Pesticide</strong>s<br />
117 samples <strong>of</strong> different crop matrices were spiked with a mixture containing the 2<br />
benzimidazole pesticides.<br />
Mix 25 Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery Deviation <strong>of</strong> Variation<br />
Carbendazim 0.01 – 2.0 97.0 19.5 20.0<br />
Thiabendazole 0.01 – 2.0 99.3 13.9 14.0<br />
2. Cereals<br />
Organochlorine <strong>Pesticide</strong>s<br />
The results <strong>of</strong> the recovery studies carried out are presented in terms <strong>of</strong> percentage<br />
mean recovery, standard deviation <strong>of</strong> the mean recovery and co-efficient <strong>of</strong> variation:<br />
6 samples [Wheat (4), Barley (1), Barley flakes (1)] were spiked with an<br />
organochlorine pesticide mixture (Mix 1) containing 14 different pesticides and<br />
metabolites.<br />
Mix 1 Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery (%) Deviation <strong>of</strong> Variation<br />
Aldrin 0.03- 0.2 92.0 12.5 13.6<br />
Captan 0.03- 0.2 98.8 15.9 16.6<br />
Chlorothalonil 0.02- 0.13 93.5 16.9 18.1<br />
Cypermethrin 0.07- 0.5 96.2 10.3 10.7<br />
Deltamethrin 0.05- 0.34 95.4 11.4 11.9<br />
pp-DDD 0.02- 0.14 93.6 11.2 11.9<br />
pp-DDE 0.02- 0.12 94.0 13.5 14.4<br />
pp- DDT 0.02- 0.14 93.4 10.7 11.5<br />
α- Endosulfan 0.02- 0.13 90.9 14.2 15.6<br />
Endrin 0.02- 0.13 95.0 10.8 11.4<br />
HCB 0.02- 0.13 89.7 12.1 13.5<br />
Lindane 0.02- 0.12 93.7 14.5 15.5<br />
Methoxychlor 0.04- 0.26 94.0 10.3 10.9<br />
Permethrin 0.2- 1.3 93.2 14.5 15.6<br />
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2 samples [Barley (1), Wheat (1)] were spiked with a second organochlorine pesticide<br />
mixture (Mix 2) containing 12 different pesticides and metabolites.<br />
Mix 2 Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery Deviation <strong>of</strong> Variation<br />
op-DDD 0.03 – 0.21 97.5 12.9 13.2<br />
op-DDE 0.03 – 0.20 102.3 8.4 8.2<br />
op-DDT 0.02 – 0.13 103.3 10.1 9.8<br />
Dieldrin 0.02 – 0.14 100.0 7.9 7.9<br />
Endosulfate 0.02 – 0.13 102.6 9.7 9.4<br />
Fenvalerate 0.06 – 0.40 103.9 10.9 10.5<br />
α-HCH 0.02 – 0.13 97.4 18.1 18.5<br />
Heptachlor 0.02 – 0.14 99.3 14.1 14.2<br />
Heptachlor<br />
-epoxide 0.02 – 0.13 99.8 12.4 12.4<br />
Iprodione 0.07 – 0.50 104.7 9.9 9.5<br />
Quintozene 0.02 – 0.14 98.1 18.1 18.5<br />
Tetradifon 0.03 – 0.2 101.7 11.0 10.8<br />
1 sample [Barley flakes (1) ] was spiked with a third organochlorine pesticide mixture<br />
(Mix 3) containing 8 different pesticides and metabolites.<br />
Mix 3 Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery Deviation <strong>of</strong> Variation<br />
Captafol 0.02 – 0.13 67.8<br />
Dic<strong>of</strong>ol 0.05 – 0.33 83.9<br />
β-Endosulfan 0.03 – 0.20 85.2<br />
Fenarimol 0.05 – 0.33 97.3<br />
β-HCH 0.04 – 0.13 88.3<br />
δ-HCH 0.02 – 0.30 85.1<br />
Procymidone 0.10 – 0.66 83.4<br />
Tecnazene 0.02 – 0.13 81.6<br />
1 sample [Wheat (1)] was spiked with a fourth organochlorine pesticide mixture (Mix<br />
4) containing 9 different pesticides.<br />
Mix 4 Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery (%) Deviation <strong>of</strong> Variation<br />
Bifenthrin 0.06 – 0.40 93.4<br />
Binapacryl 0.03 – 0.20 85.9<br />
Bromopropylate 0.03 – 0.21 95.4<br />
Cyfluthrin 0.04 – 0.27 109.7<br />
λ-Cyhalothrin 0.02 – 0.15 110.7<br />
Dicl<strong>of</strong>luanid 0.03 – 0.21 75.0<br />
Folpet 0.02 – 0.11 86.6<br />
Propyzamide 0.10 – 0.60 93.9<br />
Vinclozolin 0.02 – 0.11 96.4<br />
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1 sample [Wheat (1)] was spiked with a fifth organochlorine pesticide mixture (Mix 5)<br />
containing 3 pesticides and metabolites.<br />
Mix 5 Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery Deviation <strong>of</strong> Variation<br />
α-Chlordane 0.02 – 0.13 91.6<br />
γ-Chlordane 0.02 – 0.13 90.2<br />
Tolyfluanid 0.02 – 0.13 92.3<br />
Organophosphorous <strong>Pesticide</strong>s<br />
The results <strong>of</strong> the recovery studies carried out are presented in terms <strong>of</strong> percentage<br />
mean recovery, standard deviation <strong>of</strong> the mean recovery and co-efficient <strong>of</strong> variation:<br />
6 samples [Wheat (4), Barley (1), Barley flakes (1)] were spiked with an<br />
organophosphorous pesticide mixture (Mix 20) containing 13 different pesticides and<br />
metabolites.<br />
Mix 20 Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery Deviation <strong>of</strong> Variation<br />
Acephate 0.05 – 0.25 82.2 11.4 13.8<br />
Azinphos-Me 0.10 – 0.60 97.8 15.9 16.3<br />
Chlorpyrifos 0.06 – 0.30 93.7 5.4 5.8<br />
Chlorfenvinphos 0.06 – 0.32 95.5 5.3 5.5<br />
Diazinon 0.05 – 0.26 94.1 6.5 6.9<br />
Dimethoate 0.05 – 0.27 90.9 7.4 8.1<br />
Ethion 0.05 – 0.26 95.8 5.0 5.2<br />
Malathion 0.05 – 0.26 94.8 6.2 6.6<br />
Methidathion 0.04 – 0.21 93.0 6.4 6.9<br />
Omethoate 0.05 – 0.27 88.1 15.3 17.4<br />
Phosmet 0.11 – 0.56 92.1 5.9 6.4<br />
Tolcl<strong>of</strong>os-Me 0.05 – 0.25 93.8 6.1 6.6<br />
Triazophos 0.03 – 0.16 97.6 5.4 5.6<br />
2 samples [Barley (1), Wheat (1)] were spiked with a second organophosphorous<br />
pesticide mixture (Mix 21) containing 11 different pesticides and metabolites.<br />
Mix 21 Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery Deviation <strong>of</strong> Variation<br />
Azinphos-Et 0.10 – 0.47 129.2 25.3 19.6<br />
Dichlorvos 0.04 – 0.20 105.5 24.2 22.9<br />
Heptenophos 0.05 – 0.24 122.3 20.7 16.9<br />
Iod<strong>of</strong>enphos 0.03 – 0.16 125.3 25.0 20.0<br />
Mevinphos 0.04 – 0.19 106.5 26.8 25.1<br />
Paraoxon 0.05 – 0.24 119.6 20.2 16.9<br />
Paraoxon-Me 0.04 – 0.18 109.2 20.2 18.5<br />
Parathion 0.05 – 0.24 126.5 24.0 19.0<br />
Phosphamidon 0.04 – 0.20 123.5 21.1 17.0<br />
Phosalone 0.10 – 0.50 132.0 24.7 18.7<br />
Quinalphos 0.04 – 0.19 128.4 23.3 18.2<br />
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1 sample [Barley flakes (1)] was spiked with a third organophosphorous pesticide<br />
mixture (Mix 22) containing 6 different pesticides and metabolites.<br />
Mix 22 Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery Deviation <strong>of</strong> Variation<br />
Bromophos-Me 0.05 – 0.25 86.8<br />
Is<strong>of</strong>enphos 0.05 – 0.23 104.6<br />
Fenchlorphos 0.02 – 0.10 85.7<br />
Malaoxon 0.05 – 0.23 84.8<br />
Metamidaphos 0.04 – 0.20 52.6<br />
Propetamphos 0.05 – 0.24 91.5<br />
1 sample [Wheat (1)] was spiked with a fourth organophosphorous pesticide mixture<br />
(Mix 23) containing 5 different pesticides.<br />
Mix 23 Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery Deviation <strong>of</strong> Variation<br />
Bromophos-Et 0.05 – 0.24 92.1<br />
Chlorpyrifos-Me 0.05 – 0.23 92.4<br />
Methacrifos 0.01 – 0.21 87.4<br />
Pirimphos-Et 0.05 – 0.23 100.7<br />
Pirimphos-Me 0.05 – 0.23 92.7<br />
1 sample [Wheat (1)] was spiked with a fifth organophosphorous pesticide mixture<br />
(Mix 24) containing 5 pesticides.<br />
Mix 24 Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery Deviation <strong>of</strong> Variation<br />
Demeton-S-Me-Sulfone 0.05 – 0.25 85.8<br />
Fenithrothion 0.04 – 0.22 89.2<br />
Fon<strong>of</strong>os 0.05 – 0.25 90.1<br />
Monocrotophos 0.05 – 0.27 95.9<br />
Parathion-Me 0.05 – 0.25 87.4<br />
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3 Food <strong>of</strong> Animal Origin<br />
i. Meat Fat<br />
Organochlorine <strong>Pesticide</strong>s (OC)<br />
The results <strong>of</strong> the recovery studies carried out are presented in terms <strong>of</strong> percentage<br />
mean recovery, standard deviation <strong>of</strong> the mean recovery and co-efficient <strong>of</strong> variation:<br />
33 samples [Bovine (16), Porcine (4), Ovine (6), Avian (7)] were spiked with an<br />
organochlorine pesticide mixture (Mix A) containing 9 different pesticides and<br />
metabolites.<br />
Mix A Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery (%) Deviation <strong>of</strong> Variation<br />
pp-DDD 0.02- 0.14 85.9 11.4 13.3<br />
pp-DDE 0.02- 0.12 90.7 11.4 12.6<br />
pp- DDT 0.02- 0.14 88.1 11.0 12.5<br />
α - Endosulfan 0.02- 0.13 88.3 9.9 11.2<br />
Endrin 0.02- 0.13 95.7 15.7 16.4<br />
HCB 0.02- 0.13 85.4 10.7 12.6<br />
Lindane 0.02- 0.12 91.2 10.7 12.6<br />
Methoxychlor 0.04- 0.26 90.3 13.2 11.3<br />
Permethrin 0.2- 1.3 90.0 13.2 14.7<br />
12 samples [Bovine (6), Porcine (1) Ovine (2), Avian (3)] were spiked with a second<br />
organochlorine pesticide mixture (Mix B) containing 8 different pesticides and<br />
metabolites.<br />
Mix B Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery Deviation <strong>of</strong> Variation<br />
op-DDD 0.006 – 0.042 85.9 11.1 12.4<br />
op-DDE 0.006 – 0.040 89.3 11.0 12.3<br />
op-DDT 0.005 – 0.026 87.9 11.0 12.5<br />
α-HCH 0.005 – 0.026 88.6 14.3 16.1<br />
Dieldrin 0.005 – 0.028 94.4 12.8 13.5<br />
Heptachlor 0.005 – 0.028 68.7 15.9 23.1<br />
Heptachlor<br />
-epoxide 0.005 – 0.026 90.8 13.3 14.7<br />
Quintozene 0.005 – 0.028 88.4 14.3 16.2<br />
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27 samples [Bovine (9), Porcine (7) Ovine (5), Avian (5), Venison (1)] were spiked with<br />
a third organochlorine pesticide mixture (Mix C) containing 5 different pesticides and<br />
metabolites.<br />
Mix C Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery Deviation <strong>of</strong> Variation<br />
Dic<strong>of</strong>ol 0.005 – 0.026 27.8 16.3 58.7<br />
β-Endosulfan 0.006 – 0.038 58.5 26.4 45.2<br />
β-HCH 0.008 – 0.052 88.4 4.71 5.33<br />
δ-HCH 0.005 – 0.026 71.7 14.5 20.2<br />
Tecnazene 0.005 – 0.026 89.6 8.0 8.9<br />
Note: Due to the high RSD’s for dic<strong>of</strong>ol and β-endosulfan any results for these pesticides found in food <strong>of</strong><br />
animal origin samples would have to be interpreted with care. No residues were found in 2002.<br />
Organophosphorous <strong>Pesticide</strong>s<br />
The results <strong>of</strong> the recovery studies carried out are presented in terms <strong>of</strong> percentage<br />
mean recovery, standard deviation <strong>of</strong> the mean recovery and co-efficient <strong>of</strong> variation:<br />
43 samples [Bovine (22), Porcine (4), Ovine (8), Avian (8), Venison (1)] were spiked<br />
with an organophosphorous pesticide mixture (Mix E) containing 9 different pesticides.<br />
Mix E Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery Deviation <strong>of</strong> Variation<br />
Azinphos-Me 0.22 – 1.10 92.4 14.7 15.9<br />
Chlorpyrifos 0.10 – 0.47 89.5 11.7 13.1<br />
Chlorfenvinphos 0.10 – 0.54 90.0 11.9 13.2<br />
Diazinon 0.10 – 0.52 85.1 16.8 19.7<br />
Dimethoate 0.10 – 0.53 92.6 14.0 15.2<br />
Ethion 0.10 – 0.51 87.1 8.9 10.2<br />
Malathion 0.11 – 0.56 88.3 8.7 9.9<br />
Methidathion 0.08 – 0.34 92.5 11.8 12.8<br />
Triazophos 0.03 – 0.15 89.4 11.8 13.1<br />
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29 samples [Bovine (13), Porcine (6) Ovine (3), Avian (7)] were spiked with a second<br />
organophosphorous pesticide mixture (Mix F) containing 10 pesticides.<br />
Mix F Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery Deviation <strong>of</strong> Variation<br />
Azinphos-Et 0.20 – 0.94 82.0 14.1 17.2<br />
Dichlorvos 0.08 – 0.40 87.1 19.4 22.3<br />
Fenchlorophos 0.04 – 0.20 86.5 11.6 13.4<br />
Iod<strong>of</strong>enphos 0.06 – 0.31 85.9 11.2 13.0<br />
Mevinphos 0.08 – 0.38 92.8 14.8 16.0<br />
Parathion 0.10 – 0.48 87.2 13.1 15.0<br />
Parathion-Me 0.10 – 0.50 88.4 13.0 14.7<br />
Pirimphos-Et 0.10 – 0.45 86.4 10.8 12.5<br />
Propetamphos 0.10 – 0.47 90.6 16.0 17.7<br />
Phosalone 0.20 – 0.94 82.2 13.9 16.9<br />
19 samples [Bovine (8), Porcine (7) Ovine (1), Avian (3)] were spiked with a third<br />
organophosphorous pesticide mixture (Mix G) containing 5 pesticides.<br />
Mix G Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery Deviation <strong>of</strong> Variation<br />
Bromophos-et 0.10 – 0.47 85.0 10.0 11.8<br />
Bromophos-Me 0.10 – 0.49 86.4 11.0 12.8<br />
Chlorpyrifos-Me 0.09 – 0.45 87.4 10.8 12.4<br />
Fon<strong>of</strong>os 0.10 – 0.50 106.4 17.5 16.4<br />
Pirimphos-Me 0.08 – 0.44 85.5 10.7 12.5<br />
11 samples [Bovine (5), Porcine (4), Ovine (1), Avian (1)] were spiked with PCB<br />
mixture 3 containing 7 different PCB congeners.<br />
PCB Mix 3 Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery (%) Deviation <strong>of</strong> Variation<br />
PCB 28 0.01 – 0.05 95.2 21.8 22.9<br />
PCB 52 0.01 – 0.05 91.6 17.6 19.3<br />
PCB 101 0.01 – 0.05 89.2 15.5 17.3<br />
PCB 118 0.01 – 0.05 87.7 17.9 20.4<br />
PCB 153 0.01 – 0.05 85.2 16.0 18.8<br />
PCB 138 0.01 – 0.05 86.3 17.7 20.5<br />
PCB 180 0.01 – 0.05 81.9 16.8 20.5<br />
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ii<br />
Milk<br />
Dairy Produce<br />
The results <strong>of</strong> the recovery studies carried out are presented in terms <strong>of</strong> percentage<br />
mean recovery, standard deviation <strong>of</strong> the mean recovery and co-efficient <strong>of</strong> variation:<br />
11 samples <strong>of</strong> milk were spiked with an organochlorine pesticide mixture (Mix A)<br />
containing 9 pesticides and metabolites.<br />
Mix A Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery (%) Deviation <strong>of</strong> Variation<br />
Aldrin 0.005-0.02 75.8 5.1 6.7<br />
pp-DDD 0.005-0.026 79.9 5.8 7.3<br />
pp-DDE 0.005-0.024 83.2 6.7 8.0<br />
pp- DDT 0.005-0.028 79.6 7.5 9.5<br />
α - Endosulfan 0.005-0.026 79.8 5.6 7.0<br />
Endrin 0.005-0.026 90.4 13.8 15.3<br />
HCB 0.005-0.026 71.4 9.2 12.9<br />
Lindane 0.005-0.024 78.6 5.5 7.0<br />
Methoxychlor 0.008-0.052 84.1 7.5 9.5<br />
Permethrin 0.05-0.26 74.4 11.7 17.7<br />
1 sample <strong>of</strong> milk was spiked with organochlorine mixture, Mix B, containing 8<br />
different pesticides and metabolites.<br />
Mix B Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery (%) Deviation <strong>of</strong> Variation<br />
op-DDD 0.006 – 0.042 79.6<br />
op-DDE 0.006 – 0.040 78.0<br />
op-DDT 0.005 – 0.026 78.7<br />
α -HCH 0.005 – 0.026 77.1<br />
Dieldrin 0.005 – 0.028 78.9<br />
Heptachlor 0.005 – 0.028 60.4<br />
Heptachlor-epoxide 0.005 – 0.026 75.4<br />
Quintozene 0.005 – 0.028 74.9<br />
1 sample <strong>of</strong> milk was spiked with the organochlorine pesticide mixture, Mix C,<br />
containing 5 different pesticides and metabolites.<br />
Mix C Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery Deviation <strong>of</strong> Variation<br />
Dic<strong>of</strong>ol 0.005 – 0.026 45.1<br />
β-Endosulfan 0.006 – 0.038 18.6<br />
β-HCH 0.008 – 0.052 95.4<br />
δ-HCH 0.005 – 0.026 61.3<br />
Tecnazene 0.005 – 0.026 80.6<br />
Note: Low recoveries for dic<strong>of</strong>ol and B-endosulfan indicates that if any residues were detected then the<br />
results would require careful interpretation. No such residues were detected during 2002.<br />
Organophosphorous <strong>Pesticide</strong>s<br />
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The results <strong>of</strong> the recovery studies carried out are presented in terms <strong>of</strong> percentage<br />
mean recovery, standard deviation <strong>of</strong> the mean recovery and co-efficient <strong>of</strong> variation:<br />
14 samples <strong>of</strong> milk were spiked with an organophosphorous pesticide mixture (Mix E)<br />
containing 9 pesticides.<br />
Mix E Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery Deviation <strong>of</strong> Variation<br />
Azinphos-Me 0.22 – 1.10 87.0 14.1 16.2<br />
Chlorpyrifos 0.10 – 0.47 81.5 8.9 10.9<br />
Chlorfenvinphos 0.10 – 0.54 84.1 10.5 12.5<br />
Diazinon 0.10 – 0.52 86.0 11.9 13.9<br />
Dimethoate 0.10 – 0.53 82.8 15.8 19.1<br />
Ethion 0.10 – 0.51 81.1 8.9 10.9<br />
Malathion 0.11 – 0.56 83.6 8.7 10.5<br />
Methidathion 0.08 – 0.34 86.4 10.5 12.1<br />
Triazophos 0.03 – 0.15 83.8 12.8 15.3<br />
4 samples <strong>of</strong> milk were spiked with an organophosphorous pesticide mixture (Mix F)<br />
containing 10 pesticides.<br />
Mix F Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery Deviation <strong>of</strong> Variation<br />
Azinphos-Et 0.20 – 0.94 76.8 10.1 13.2<br />
Dichlorvos 0.08 – 0.40 107.5 8.9 8.3<br />
Fenchlorophos 0.04 – 0.20 80.8 10.0 12.3<br />
Iod<strong>of</strong>enphos 0.06 – 0.31 79.3 10.8 13.7<br />
Mevinphos 0.08 – 0.38 84.1 22.7 27.0<br />
Parathion 0.10 – 0.48 79.4 8.4 10.5<br />
Parathion-Me 0.10 – 0.50 81.9 8.1 10.0<br />
Pirimphos-Et 0.10 – 0.45 78.9 9.7 12.3<br />
Propetamphos 0.10 – 0.47 84.9 12.8 15.0<br />
Phosalone 0.20 – 0.94 78.4 11.4 14.5<br />
3 samples <strong>of</strong> milk were spiked with an organophosphorous pesticide mixture (Mix G)<br />
containing 5 pesticides<br />
Mix G Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery Deviation <strong>of</strong> Variation<br />
Bromophos-Et 0.10 – 0.47 86.6 5.3 6.1<br />
Bromophos-Me 0.10 – 0.49 90.3 6.4 7.1<br />
Chlorpyrifos-Me 0.09 – 0.45 91.9 7.7 8.4<br />
Fon<strong>of</strong>os 0.10 – 0.50 96.5 6.3 6.6<br />
Pirimphos-Me 0.08 – 0.44 87.3 8.7 9.9<br />
5 samples <strong>of</strong> milk were spiked with a PCB mixture, PCB Mix 3, which contained 7<br />
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different PCB congeners.<br />
PCB Mix 3 Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery Deviation <strong>of</strong> Variation<br />
PCB 28 0.01 – 0.05 78.9 3.5 4.4<br />
PCB 52 0.01 – 0.05 78.8 4.7 6.0<br />
PCB 101 0.01 – 0.05 78.0 4.8 6.2<br />
PCB 118 0.01 – 0.05 80.0 4.4 5.4<br />
PCB 153 0.01 – 0.05 75.8 4.8 6.3<br />
PCB 138 0.01 – 0.05 76.7 4.5 5.9<br />
PCB 180 0.01 – 0.05 73.7 4.6 6.2<br />
iii<br />
Poultry Produce<br />
Eggs.<br />
2 samples <strong>of</strong> eggs were spiked with the organochlorine pesticide mixture, Mix A,<br />
containing 10 different pesticides and metabolites. All spiking was carried out at a<br />
single concentration.<br />
Mix A Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery (%) Deviation <strong>of</strong> Variation<br />
Aldrin 0.005 79.5 3.3 4.2<br />
pp-DDD 0.005 93.0 3.5 3.7<br />
pp-DDE 0.005 106.3 12.7 11.9<br />
pp- DDT 0.005 51.9 65.9 128.8<br />
α- Endosulfan 0.005 128 37.4 29.2<br />
Endrin 0.005 160.1 92.1 57.6<br />
HCB 0.005 79,9 0.7 0.9<br />
Lindane 0.005 95.9 8.9 9.3<br />
Methoxychlor 0.008 88.2 3.3 3.8<br />
Permethrin 0.05 79.9 2.5 3.1<br />
Note: Recovery data for pp-DDT and for endrin indicate that the method may have to be further refined to<br />
deal with these pesticides while recognising that this information is based on very limited recovery data.<br />
1 egg sample was spiked with the organochlorine pesticide mixture, Mix B, which<br />
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contained 8 different pesticides and metabolites.<br />
Mix B Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery (%) Deviation <strong>of</strong> Variation<br />
op-DDD 0.006 – 0.042 96.7<br />
op-DDE 0.006 – 0.040 83.7<br />
op-DDT 0.005 – 0.026 64.9<br />
α-HCH 0.005 – 0.026 93.2<br />
Dieldrin 0.005 – 0.028 124.9<br />
Heptachlor 0.005 – 0.028 64.6<br />
Heptachlor-epoxide 0.005 – 0.026 106.0<br />
Quintozene 0.005 – 0.028 120.8<br />
1 egg sample was spiked with the organochlorine pesticide mixture, Mix C, which<br />
contained 5 different pesticides and metabolites.<br />
Mix C Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery (%) Deviation <strong>of</strong> Variation<br />
Dic<strong>of</strong>ol 0.005 – 0.026 84.5<br />
β-Endosulfan 0.006 – 0.038 68.7<br />
β-HCH 0.008 – 0.052 93.5<br />
δ-HCH 0.005 – 0.026 102.7<br />
Tecnazene 0.005 – 0.026 85.7<br />
Organophosphorous <strong>Pesticide</strong>s. (OP)<br />
2 egg samples were spiked with the organophosphorous pesticide mixture, Mix E,<br />
containing 9 different pesticides.<br />
Mix E Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery Deviation <strong>of</strong> Variation<br />
Azinphos-Me 0.22 – 1.10 88.7 1.6 1.8<br />
Chlorpyrifos 0.10 – 0.47 83.8 2.4 2.8<br />
Chlorfenvinphos 0.10 – 0.54 83.8 1.0 1.2<br />
Diazinon 0.10 – 0.52 122.6 3.0 2.4<br />
Dimethoate 0.10 – 0.53 108.4 6.3 5.9<br />
Ethion 0.10 – 0.51 84.4 0.6 0.7<br />
Malathion 0.11 – 0.56 107.6 0.5 0.5<br />
Methidathion 0.08 – 0.34 100.5 11.8 11.7<br />
Triazophos 0.64 – 0.32 69.3 0.2 0.2<br />
2 samples <strong>of</strong> eggs were spiked with the organophosphorous pesticide mixture, Mix G,<br />
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which contained 5 different pesticides.<br />
Mix G Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery Deviation <strong>of</strong> Variation<br />
Bromophos-Et 0.10 – 0.47 70.7 10.2 14.4<br />
Bromophos-Me 0.10 – 0.49 74.2 3.4 4.6<br />
Chlorpyrifos-Me 0.09 – 0.45 84.2 11.5 13.7<br />
Fon<strong>of</strong>os 0.10 – 0.50 101.6 3.4 3.4<br />
Pirimphos-Me 0.08 – 0.44 83.8 5.0 6.0<br />
2 samples <strong>of</strong> eggs were spiked with the PCB mixture, PCB Mix 3, containing 7<br />
different PCB congeners.<br />
PCB Mix 3 Concentration Mean Standard Co-efficient<br />
(mg/kg) Recovery Deviation <strong>of</strong> Variation<br />
PCB 28 0.01 – 0.05 103.7 11.0 10.6<br />
PCB 52 0.01 – 0.05 85.8 5.7 6.7<br />
PCB 101 0.01 – 0.05 140.1 74.0 52.9<br />
PCB 118 0.01 – 0.05 152.7 9.6 6.3<br />
PCB 153 0.01 – 0.05 79.6 0.1 0.2<br />
PCB 138 0.01 – 0.05 67.4 26.2 38.8<br />
PCB 180 0.01 – 0.05 72.0 0.8 1.2<br />
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ANNEX IX<br />
PESTICIDES DETERMINED IN VEGETABLE SAMPLES ANALYZED BY<br />
ANALYTICAL CONSULTANTS, ON BEHALF OF BORD GLAS<br />
Organobromine Included in the PCS Recovery Limit <strong>of</strong><br />
Compounds Monitoring Programme (%) Determination<br />
(mg/kg)<br />
bromopropylate yes > 70 0.04<br />
Organobromine Included in the PCS Recovery Limit <strong>of</strong><br />
Compounds Monitoring Programme (%) Determination<br />
(mg/kg)<br />
aldrin<br />
cis-chlordane<br />
yes<br />
no<br />
> 70<br />
> 70<br />
0.03<br />
0.02<br />
trans-chlordane no > 70 0.03<br />
chlorothalonil yes > 70 0.02<br />
dieldrin yes > 70 0.02<br />
op’DDE yes > 70 0.03<br />
pp’DDE yes > 70 0.02<br />
op’DDT yes > 70 0.02<br />
pp’DDT yes > 70 0.02<br />
op’DDD yes > 70 0.03<br />
pp’DDD yes > 70 0.02<br />
dic<strong>of</strong>ol yes > 70 0.04<br />
endosulfan 1 yes > 70 0.02<br />
endosulfan 2 yes > 70 0.03<br />
endosulfate yes > 70 0.02<br />
endrin yes > 70 0.02<br />
heptachlor yes > 70 0.02<br />
heptachlor-epoxide yes > 70 0.02<br />
HCB yes > 70 0.02<br />
α-HCH yes > 70 0.02<br />
β-HCH yes > 70 0.04<br />
δ-HCH yes > 70 0.02<br />
lindane (γ-HCH) yes > 70 0.02<br />
methoxychlor yes > 70 0.04<br />
quintozene yes > 70 0.02<br />
tecnazene yes > 70 0.02<br />
Tolyfluanid Yes >70 0.02<br />
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Organophosphorous Included in the PCS Recovery Limit <strong>of</strong><br />
Compounds Monitoring Programme (%) Determination<br />
(mg/kg)<br />
acephate yes > 70 0.05<br />
azinphos-ethyl yes > 70 0.1<br />
azinphos-methyl yes > 70 0.1<br />
bromophos-ethyl yes > 70 0.05<br />
bromophos-methyl yes > 70 0.05<br />
chlorfenvinphos yes > 70 0.06<br />
chlorpyrifos yes > 70 0.06<br />
chlorpyrifos-methyl yes > 70 0.05<br />
demeton-S-methylsulfone yes > 70 0.07<br />
diazinon yes > 70 0.05<br />
dichlorvos yes > 70 0.04<br />
dimethoate yes > 70 0.05<br />
ethion yes > 70 0.05<br />
etrimfos yes > 70 0.03<br />
fenchlorphos yes > 70 0.02<br />
fenitrothion yes > 70 0.05<br />
fonophos yes > 70 0.05<br />
heptenophos yes > 70 0.04<br />
iod<strong>of</strong>enphos yes > 70 0.04<br />
is<strong>of</strong>enphos yes > 70 0.05<br />
malaoxon yes > 70 0.05<br />
malathion yes > 70 0.05<br />
methacrifos yes > 70 0.05<br />
methamidophos yes > 70 0.04<br />
methidathion yes > 70 0.04<br />
monocrotophos yes > 70 0.06<br />
mevinphos yes > 70 0.04<br />
omethoate yes > 70 0.05<br />
paraoxon yes > 70 0.05<br />
paraoxon-methyl yes > 70 0.04<br />
parathion yes > 70 0.05<br />
parathion-methyl yes > 70 0.04<br />
phosalone yes > 70 0.1<br />
phosmet yes > 70 0.1<br />
phosphamidon yes > 70 0.04<br />
pirimiphos-methyl yes > 70 0.05<br />
propetamphos yes > 70 0.05<br />
quinalphos yes > 70 0.04<br />
Tolcophos-methyl yes > 70 0.05<br />
triazophos yes > 70 0.03<br />
Pirimiphos-ethyl yes > 70 0.05<br />
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Dicarboximide Included in the PCS Recovery Limit <strong>of</strong><br />
Compounds Monitoring Programme (%) Determination<br />
(mg/kg)<br />
iprodione yes > 70 0.07<br />
procymidone yes > 70 0.1<br />
vinclozolin yes > 70 0.02<br />
Phthalimide Included in the PCS Recovery Limit <strong>of</strong><br />
Compounds Monitoring Programme (%) Determination<br />
(mg/kg)<br />
captafol yes > 70 0.02<br />
captan yes > 70 0.03<br />
folpet yes > 70 0.02<br />
Pyrethroid Included in the PCS Recovery Limit <strong>of</strong><br />
Compounds Monitoring Programme (%) Determination<br />
(mg/kg)<br />
bifenthrin yes > 70 0.07<br />
cyfluthrin yes > 70 0.04<br />
λ-cyhalothrin yes > 70 0.02<br />
cypermethrin yes > 70 0.07<br />
deltamethrin yes > 70 0.05<br />
fenvalerate yes > 70 0.06<br />
permethrin yes > 70 0.2<br />
Other Included in the PCS Recovery Limit <strong>of</strong><br />
Compounds Monitoring Programme (%) Determination<br />
(mg/kg)<br />
dichl<strong>of</strong>luanid yes > 70 0.03<br />
fenarimol yes > 70 0.05<br />
propyzamide yes > 70 0.1<br />
tetradifon yes > 70 0.03<br />
binapacryl yes > 70 0.04<br />
carbendazim yes >70 0.05<br />
thiabendazole yes >70 0.05<br />
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Annex X<br />
SUMMARY OF THE RESULTS OF THE ANALYSIS OF IRISH VEGETABLES<br />
SAMPLED AND ANALYSED BY AN BORD GLAS DURING 2002.<br />
Part 1. Vegetables sampled by An Bord Glas for pesticide residue analysis in 2002.<br />
Commodity No. <strong>of</strong> Residues detected<br />
samples > MRL < MRL ND<br />
analysed<br />
Apples<br />
Broccoli<br />
Brussel sprouts<br />
Cabbage<br />
Carrots<br />
Cauliflower<br />
Celery<br />
Cress<br />
Cucumbers<br />
Leeks<br />
Lettuce<br />
Mushrooms<br />
Onions<br />
Parsley<br />
Parsnips<br />
Potatoes<br />
Scallions<br />
Spinach<br />
Strawberry<br />
Swedes<br />
Tomatoes<br />
Turnips<br />
2<br />
64<br />
3<br />
6<br />
5<br />
6<br />
3<br />
1<br />
2<br />
2<br />
4<br />
49<br />
1<br />
1<br />
3<br />
33<br />
1<br />
1<br />
1<br />
3<br />
10<br />
1<br />
2<br />
0<br />
0<br />
0<br />
1<br />
0<br />
3<br />
0<br />
0<br />
0<br />
3<br />
6<br />
0<br />
1<br />
1<br />
1<br />
0<br />
0<br />
0<br />
0<br />
1<br />
0<br />
0<br />
6<br />
3<br />
6<br />
4<br />
6<br />
0<br />
1<br />
2<br />
2<br />
1<br />
43<br />
1<br />
0<br />
2<br />
32<br />
1<br />
1<br />
1<br />
3<br />
9<br />
1<br />
Total<br />
144<br />
19<br />
125<br />
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Part 2: <strong>Pesticide</strong> residues detected in vegetables sampled by An Bord Glas in 2002.<br />
Sample number. Residue detected. Residue (mg/kg) MRL (mg/kg)<br />
1. Fruit 1.3. Pome Fruit 1.3.1. Apples<br />
1094 Captan 0.08 3.0<br />
1097 Carbendazim 1.37 2.0<br />
2. Vegetables. 2.1. Root & Tuber Vegetables 2.1.1. Carrots.<br />
1072 Chlorfenvinphos 0.12 0.5<br />
2.1.3. Parsnip<br />
1076 Chlorfenvinphos 0.25 0.5<br />
2.3. Fruiting Veg. 2.3.1.1. Tomato<br />
1716 Iprodione 0.16 5.0<br />
2.5. Leafy Vegetables.2.5.1. Lettuce & Similar. 2.5.1.1. Lettuce.<br />
1632 Propyzamide 0.18 1.0<br />
1089 Iprodione 0.11 10<br />
1061 Iprodione 0.29 10<br />
Propyzamide 0.12 1.0<br />
2.5.5. Herbs. 2.5.5.1.Parsley<br />
1059 Cypermethrin 0.33 2.0<br />
2.7. Stem Vegetables 2.7.2. Celery<br />
1069 chlorothalonil 2.2 10<br />
1053 chlorothalonil 0.05 10<br />
1062 chlorothalonil 0.11 10<br />
2.8. Fungi 2.8.1. Mushrooms<br />
1733 Carbendazim 0.4 1.0<br />
1034 Carbendazim 0.1 1.0<br />
1738 Carbendazim 0.19 1.0<br />
1742 Carbendazim 0.1 1.0<br />
1706 Lindane 0.04 No Irish MRL.<br />
1100b Carbendazim 0.33 1.0<br />
5.0. Potatoes<br />
1030 Tecnazene 0.08 No MRL in 2002.<br />
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