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12 DETERMINATION OF Cd (II), Cu (II), Pb (II), AND Zn (II) IN BIOLOGICAL AND NOT BIOLOGICAL CITRUS ESSENTIAL OILS BY DERIVATIVE POTENTIOMETRIC STRIPPING ANALYSIS (dPSA) Dugo Giacomo, Giuffrida Daniele, Drogo Alessandra, La Pera Lara Dipartimento di Chmica Organica e Biologica Università di Messina Salita Sperone, 31, 90166 S. Agata -Messina Citrus essential oils are complex mixtures of many classes of volatile (85-98%) and not volatile (15-2%) compounds (1); they are used in food and cosmetic farm as aromatizer and in pharmaceutical industry as additives of some drugs (2). Their wide use implies a strict control of the presence of organic and inorganic contaminants as heavy metals. There is a lack of available data regarding to the presence of heavy metals: some reports concerning to the micro-elements composition of citrus peel extracts were found (3,4). Metals levels in citrus essential oils mostly depend on the type of soil, agrochemical treatments, but also on extraction procedures as scraping or pressing, since the fruits inevitably come in contact with metallic surfaces (5). In this work potentiometric stripping analysis is used to determine the content of Cd (II), Cu (II), Pb (II) and Zn (II) in lemon, mandarin, orange and bergamot non biological essential oils produced in Sicily and Calabria in the crop year 1999 (6). Moreover 13 samples of bergamot biological essential oils and 13 samples of non-biological essential oils produced in Calabria in the crop year 2000, were studied. MATERIALS AND METHODS Reagents All oils are sampled in dark glassy bottles, with blind nipples, and stored at 4°C until the analyses. Ultra pure hydrochloric acid (34-37%), Hg (II) (1000 µgmL -1 , 1M in hydrochloric acid) and Cd (II), Cu (II), Pd (II), Pb (II), Zn (II) (1000 µgmL -1 , 0.5 N in HNO3) standard solutions were purchased by Panreac (Barcelona, Spain); Ga (NO3)3⋅3H2O (5 g, 99.9%) was purchased by Aldrich Chem. Co. (Milwakee, WI, USA). The extracts were filtrated on a carbon column Supelclean ENVI-Carb SPE (0.5 g, 6 mL), purchased by Supelco (Bellefonte, PA, USA). Apparatus Metals analysis are carried out by a PSA ION 3 potentiometric stripping analyzer (Steroglass, S. Martino in Campo, Perugia, Italy), connected to an IBM-compatible personal computer. The analyzer operates under the control of the NEOTES 2.0.1 software package (Steroglass). The determination is carried out in a conventional three-electrode cell. The working electrode was a glassy carbon one coated with a thin mercury film; reference electrode was an Ag/AgCl electrode (KCl 3M), and a platinum wire auxiliary electrode was used. Procedures Hydrochloric acid extraction A 8.60 g (10.00 mL) sample aliquot and a 10 mL volume of 36% ultrapure-hydrochloric acid (Panreac, Barcellona), are introduced in a teflon beaker. The extraction was carried out for about 30 min under magnetic stirring at the temperature of 90 °C. The acid sample, was transferred in a separating funnel and let to cool for about 5 minutes. In order to favour the separation of the two phases, the mixture is spiked with 1.0 mL ultrapure methanol, then the acid layer was collected in a 20.00 mL flask. The organic layer is extracted again with 4.50 mL of concentrated hydrochloric acid for 5 min, under the same conditions described, and then washed with 4.50 mL of boiling water; washings were added to the acid extracts and made up to the mark with water. The obtained solution was passed through a carbon column. The filtered solution was used for the simultaneous determination of Cd (II), Cu (II), Pb (II), and Zn (II). Potentiometric determination All analysis were executed in a conventional three electrodes cell; working electrode was a glassy carbon electrode coated with a Hg film, the reference one was an Ag/AgCl electrode, the counter was a Pt electrode. The concentrations of Cd (II), Cu (II), Pb (II), and Zn (II) were simultaneously determined. 1.00 mL of acid extract, 17.50 mL of ultrapure water, 1.00 mL of 1000 µg mL -1 Hg (II) as oxidant agent and 0.50 mL of 10 µg mL -1 Ga (III) - in order to prevent Cu-Zn complexes formation on the mercury film (6)- were put into the electrochemical cell. The quantitative analysis was executed by the multiple points standard additions method. The potentiometric parameters are reported on table 1. Method performances PDF creato con FinePrint pdfFactory versione dimostrativa http://www.secom.re.it/fineprint 76
Recovery and repeatabilty tests were menaged by emploing the above described method to lemon, mandarin, orange and bergamot essential oils. Cd (II), Cu (II), Pb (II), and Zn (II) recoveries always spanned from 95.00-100.50% evidencing that metals quantification remained unaffected by the clean-up steps. The repeatability was > 95.00% for Cd (II), Cu (II), Pb (II), and Zn (II) in all types of oils. Detection limits obtained for the four analytes, ranged from 0.10 to 0.98 ng g -1 in lemon, mandarin, sweet orange and bergamot essential oils. Application Figure 1 show the concentration of Cd, Cu, Pb and Zn in lemon, sweet orange, mandarin in Sicilian and Calabrian bergamot essential oils. It’s evident that Cd is the metal present in the lowest amount and Zn in the highest, in all types of essential oils. Cd concentration spanned from 2 to 23.3 ng g -1 ; Cu from 17.8 to 380.0 ng g -1 ; Pb ranged from 75.9 to 180.3 ng g -1 and Zn from 804.5 to 1647.5 ng g -1 . Moreover, the concentration of Cd, Cu, Pb and Zn was determined in 13 samples of biological bergamot essential oils, and 13 non biological ones. Figure 2 evidences that there was any significant difference between biological and non biological oils metals level. LITERATURE 1. Di Giacomo A., Mincione B.Gli oli essenziali agrumari in Italia. 1994 Ed. Laruffa, p.196. 2. Gorinstein S., Martin-Belloso O., Park Y. S., Haruenkit R., Lojek A., Ciz, M., Caspi A., Libman, I., Trakhtenberg S.Comparison of some biochemical characteristics of different citrus fruit. Food Chem. 2001, 74, 309-315. 3. Simpkins W.A., Honway, L., Wu M., Harrison M., Goldberg D. Trace elements in Australian orange juice and other products. Food Chem, 2000, 71, 423-433. 4. Di Giacomo, A. Tecnologia dei prodotti agrumari. Parte II. 1988, duplicated lecture notes, Univrsità di Reggio Calabria, 95-120. 5. La Pera L., Saitta M., Di Bella G., Dugo G.mo. Simultaneous determination of Cd (II), Cu (II) Pb (II) and Zn (II) in citrus essential oils by derivative potentiometric stripping analysis. J. Agric. Food Chem. 2003 in press 6. La Pera L., Lo Curto S., Visco A., Dugo G.mo. Derivative Potentiometric Stripping Analysis (dPSA) used for determination of cadmium, copper, lead and zinc in in Sicilian olive oils. J. Agric. Food Chem. 2002, 50, 3090- 3094. PDF creato con FinePrint pdfFactory versione dimostrativa http://www.secom.re.it/fineprint 77
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International Congress BIOLOGICAL P
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15:40-16:20 G. Lozzia Università d
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MAIN SPEAKERS • V. Rotondo FIAO,
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Il settore oggi è regolamentato in
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target botanical synthetic sodium c
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RELIABILITY AND PROSPECTIVES FOR TH
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Vineyard Passive diffusion Spontane
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of the host, a relatively limited n
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LOZZIA G.C., RIGAMONTI I.E., 1994 -
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DIFESA DELLE COLTURE DAI PATOGENI F
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THE FUNGAL PHYTOTOXINS AND THEIR PO
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NEED FOR RESEARCH AND APPROPRIATE A
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Page 43 and 44: POSTER 1. Agosteo G.E., Ambrosio M.
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Page 49 and 50: 2 LUPINUS ALBUS, AN ANCIENT EUROPEA
Page 51 and 52: Table 1. Benzo(a)pyrene and benzo(e
Page 53 and 54: 5 INSETTICIDI D’ORIGINE VEGETALE
Page 55 and 56: Tabella 2. Piretrine: composizione
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Page 59 and 60: 7 NATURAL COMPOUNDS IN THE CONTROL
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Page 63 and 64: Figure 3. Effect of Pseudomonas sp.
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26 IL CONTROLLO DELLE OPERAZIONI DI
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Results and Discussion S. carpocaps
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entompathogenic nematodes. CSC-EC E
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After this preliminary screening an
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FIGURE 3. Insecticidal activity of
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Several colonies of Lepidopteran, C
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M. Scribano research work was suppo
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Nematode isolate % Mortality 3 100
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In our trial organic wheat showed a
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per "strippare" i vapori nitrosi re
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L’ultima parte della ricerca è s
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33 INVESTIGATIONS ON THE BACTERICID
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Vengono qui riportati i risultati d
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while for dinocap is 10 pg/µL. For
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[Pb](ng/ml) Figure 1: Pb content of
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