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18 INFLUENCE OF DIFFERENT TREATMENTS ON Cd (II), Cu (II), Pb (II) AND Zn (II) CONTENT IN SICILIAN OLIVE OILS La Pera Lara, Lo Turco Vincenzo, Lo Curto Simona, Mavrogeni Ekaterini, Dugo Giacomo Dipartimento di Chmica Organica e Biologica Università di Messina Salita Sperone, 31, 90166 S. Agata- Messina Metals can be found in fatty food as edible oils that are often subjected to refining, bleaching, and deodorization, during which they inevitably come in contact to metallic surfaces (1). Trace levels of some metal ions like Cu (II) could catalyse the oxidation reaction of fatty acid chains, with conseguent a deleterious effect on oil flavor and shelf-life of oils (2). Metals contamination of olive oil could be due to their presence in the soil, water and, particularly for lead, in the air (3). Many studies have been carried out in which the presence of trace metals in olive oils was correlated to agronomical techniques, harvesting methods, oil extraction and packaging procedures (4, 5). The purpose of this paper was to explore the correlation between the pesticide treatments occurred in olive growing and the content of metals found in oils. The analytical techniques frequently used for the subsequent determinations are emission and absorption spectrophotometric techniques as well as electroanalytical techniques (2,6). In this paper derivative potentiometric stripping analysis (dPSA) was used to determine copper (II), lead (II), cadmium (II) and zinc (II), in samples of virgin olive oils from Sicily (7-9). MATERIALS AND METHODS Samples Seven olive oils samples belonging to Nocellara del Belice variety, produced in the crop year 2000 -2001 from plants grown up on sandy soils in the zone of Valle del Belice (Trapani), were studied. Each of these samples was originated from olive grove subjected to different pesticides treatments as dimethoate/fenthion, dimethoate, copper oxy-chlorine/dimethoate, copper oxy-chlorine/fenthion; biological treatments as copper oxychlorine and biological fight and no treatment. Oil samples were stored in dark glassy bottles at 4°C for the time of analysis. Chemicals Ultra pure hydrochloric acid (34-37%), Hg (II) (1000 µgmL -1 , 1M in hydrochloric acid) and Cd (II), Cu (II), Pb (II), Zn (II), Ga (III) and Pd (II) (1000 µg mL -1 , 0.5 N in nitric acid) standard solutions were purchased by Panreac Quimica (Barcelona, Spain). The extracts are filtrated on a carbon column Supelclean ENVI-Carb SPE (0.5 g, 6 mL), purchased by Supelco (Bellefonte, PA, USA). Apparatus Determinations were carried out using a PSA ION 3 potentiometric stripping analyzer (Steroglass, S. Martino in Campo, Perugia, Italy), connected to an IBM-compatible personal computer. The analyzer operated under the control of the NEOTES software package (Steroglass). Electrode Preparation (plating) and potentiometric determination 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 plating of the working electrode was effected putting in the electrochemical cell a 20 mL volume of a 1000 µgmL -1 Hg standard solution and carrying out the electrolysis, at –950 mV against the reference electrode, for 1 min. The determination of Cd, Cu and Pb in oily extract was executed at pH 0.5, putting in the electrochemical cell a 3 mL volume of elute, a 17 mL volume of ultra pure H2O and a 1 mL volume of Hg (II) standard solution as oxidant agent. The determination of Zn was executed at pH 1.8, putting in the electrochemical cell a 1 mL volume of elute, 18.5 mL of ultra pure H2O and 0.5 mL of Hg (II) standard solution as oxidant agent. The quantitatve analysis was carried out by the multiple standard addition method. Metals determination was managed under analytical conditions described in table 1. RESULTS AND DISUSSION Method The repeatability of the method was attested at 86.4 % for cadmium, at 94.9% for copper, at 99.0% for lead and at 98.9% for zinc. Recoveries were carried out by spiking a sample of olive oil at different levels. PDF creato con FinePrint pdfFactory versione dimostrativa http://www.secom.re.it/fineprint 94
Obtained recoveries percent were: 84.5±9.9% for Cd, 97.3±2.7% for Cu, 1 00.7±0.7 % for Pb and 83.4±1.7 % for Zn. Instrumental detection limits were: 1.2 ngg -1 for Cd, 3.6 ngg -1 for Cu, 5.9 ngg -1 for Pb and 14.3 ngg -1 for Zn. Application Obtained results are reported on Table 1. Cd (II) was not found in any olive oil sample. The highest content of Cu (II) was found in the sample originated from biological strategy (96.1±5.3 ng g -1 ). A lower content of the metal was presented by the samples produced from plants treated with organic pesticides associated or not to copper oxy-chlorine, such as copper oxy-chlorine/dimethoate (91.4±5.1 ng g -1 ) and copper oxy-chlorine/fenthion (60.0±3.1 ng g -1 ). A smaller level of Cu was found in samples originated from dimethoate/fenthion (56.8±3.3 ng g -1 ), dimethoate (38.3±0.4 ng g -1 ) and no treated sample (44.8±1.5 ng g -1 ). The smallest Cu concentration was found in the oil originated from copper oxy-chlorine treatment (26.0±2.3 ng g -1 ). Oil samples produced from olive grove treated with organic pesticides - copper oxychlorine/fenthion (222.6±2.3 ng g -1 ), dimethoate (179.2 ±1.9 ng g -1 ), dimethoate/fenthion (165.0±1.5 ng g -1 ) - showed a higher lead amount respect to samples treated only with copper oxy-chlorine (47.5±0.5 ng g -1 ), no-treated sample (34.6±0.4ng g -1 ) and the sample from biological strategy (17.3±0.2 ng g -1 ), which presented the lowest Pb content (fig.1). An exception was represented by the sample treated with copper oxy-chlorine/dimethoate (32.8±0.3 ng g -1 ). Samples produced from olive groves treated with copper oxy-chlorine/fenthion (576.0±6.3 ng g -1 ) presented the highest content of Zn, followed by biological strategy (550.0±5.8 ng g -1 ) and copper oxychlorine/dimethoato (433.2±4.7 ng g -1 ) samples; the oils treated with dimethoate (176.0 ±1.9 ng g -1 ), copper oxy-chlorine (161.5±1.7 ng g -1 ), dimethoate/fenthion (140.8±1.5 ng g -1 ), showed a Zn level remarkably lower. The smallest concentration of the metal was found in no-treated sample (59.8±0.7 ng g -1 ). CONCLUSION Samples produced from no treated olive grove and by plants treated only with copper oxy-chlorine, always showed a lower content of Cu (II), Pb (II) and Zn (II) respect to samples originated from olive grove treated with the organophosphorated pesticides dimethoate and fenthion. These molecules, which contain S, P and O atoms, may influence the mechanism of metals uptake of the plants by complexing the cations (10). Samples originated from biological fight always present a high amount of the micronutrient Cu (II) and Zn (II) and a very low concentration of Pb (II). LITERATURE 1. Martín-Polvillo M., Albi T. and Guinda A. Determination of trace elements in edible vegetable oils by atomic absorption spectrophotometry. J. Am. Oil Chem. Soc. 1994, 71, 347-350. 2. Calapaj R., Chiricosta S., Saija G. and Bruno E. Method for the determination of heavy metals in vegetable oils by graphite furnace atomic absorption. At. Spectrosc. 1988, 9, 107-110. 3. Paoletti R., Nicosia S., Clementi F., Fumagalli G. 1 st ed. “Tossicologia degli alimenti”, 1999, Utet, Torino. 4. De Leonardis A., Macciola V. and De Felice M. 1997. La determinazione del ferro e del rame negli oli vergini d'oliva mediante spettrofotometria ad assorbimento atomico. Riv. Ital. Sostanze Grasse 74: 149. 5. Garrido M.D., Frías I., Díaz C. and Hardisson A. Concentrations of metals in vegetable edible oils. Food Chem. 1994, 50, 237-240. 6. Wahdat F., Hinkel S. and Neeb R. Direct inverse voltammetric determination of Pb, Cu and Cd in some edible oils after solubilization. Fresenius' Z. Anal. Chem. 1995, 352, 393-396. 7. La Pera L., Lo Curto S., Dugo G.mo, Lo Coco F. and Liberatori A. Determination of Copper (II), lead (II), cadmium (II) and zinc (II) in olive oils from Sicily by derivative potentiometric stripping analysis (dPSA). Presented at “European Conference of Advanced Technology for Safe and High Quality of Food”, Berlin, 5-7 December, 2001. 8. La Pera L., Lo Curto S., Visco A., La Torre L. and Dugo G.mo Derivative potentiometric stripping analysis (dPSA) used for the determination of cadmium, copper, lead and zinc in Sicilian olive oils. J. Agric. Food Chem. 2002, 95, 3090-3093. 9. La Pera, L.; Lo Coco, F.; Mavrogeni, E; Giuffrida, D.; Dugo, G.mo. Determination of Copper (II), Lead (II), Cadmium (II) and Zinc (II) in virgin olive oils produced in Sicily and Apulia by Derivative Potentiometric Stripping Analysis. Ital. J. Food Science 2002 in press. 10. Kaim W.; Schwedersky B. Bioinorganic Chemistry: inorganic elements in the chemistry of life. V th ed. Wiley & Sons Ltd, West Sussex, England, 1996. PDF creato con FinePrint pdfFactory versione dimostrativa http://www.secom.re.it/fineprint 95
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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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PRESENCE OF OCHRATOXIN IN EXPERIMEN
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5. Hohler, D. (1998). Ochratoxin A
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Table 3: Pesticide treatments on
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BIOPESTICIDES: EVALUATION PROCESS F
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Xenorhabdus spp. and Photorhabdus s
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It can be reproduced in vivo at 15
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Vinson, S. B., 1975, Biochemical co
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PROTECTION OF GRAPEVINE FROM POWDER
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I MEZZI TECNICI PER L'AGRICOLTURA B
Page 43 and 44: POSTER 1. Agosteo G.E., Ambrosio M.
Page 45 and 46: 31. Pietri A., Bertuzzi T., Barbier
Page 47 and 48: 1 PROVE DI LOTTA ALL’OIDIO DELLO
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
Page 57 and 58: californicus (fitoseide predatore)
Page 59 and 60: 7 NATURAL COMPOUNDS IN THE CONTROL
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Page 63 and 64: Figure 3. Effect of Pseudomonas sp.
Page 65 and 66: 9 IMPROVEMENT OF SOIL PROPERTIES AN
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Page 71 and 72: % cumulative hatch 40 35 30 25 20 1
Page 73 and 74: ROTENONE Il principio attivo è est
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Page 77 and 78: Recovery and repeatabilty tests wer
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Page 83 and 84: Tab. III - Residui di timolo(mg/Kg)
Page 85 and 86: phytotoxicity index (%) Results In
Page 87 and 88: 15 ORGANIC WHEAT QUALITY AND PRODUC
Page 89 and 90: 16 IL CONTROLLO DELLA “ MOSCA DEL
Page 91 and 92: Nel primo anno si può notare un an
Page 93: 17 Il contenimento della ticchiolat
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Page 103 and 104: Tab. 3 Flavonol content (µg/ml) in
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Page 111 and 112: 21 CONTAMINAZIONE DA MICOTOSSINE IN
Page 113 and 114: Ricerca: Aflatossine B1 B1+B2+G1+G2
Page 115 and 116: Campioni non Conformi 3,4 % B1 Camp
Page 117 and 118: 22 PEPTIDATI DI RAME: PRODOTTI INNO
Page 119 and 120: 23 CHARACTERIZATION OF ORGANIC VIRG
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Page 123 and 124: 25 EFFICACY EVALUATION OF BIOLOGICA
Page 125 and 126: Fig. 1 - Effects of Biological Cont
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Page 129 and 130: Results and Discussion S. carpocaps
Page 131 and 132: entompathogenic nematodes. CSC-EC E
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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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