The development of an analytical method for the determination of four selected pyrethroid insecticides at residue level in beef meat is presented. Acetone and petroleum ether at 40-60 degrees C were chosen as extraction solvents. A two-step clean-up was performed using an Extrelut NT3-C(18) system followed by a Florisil column, with disposable, ready-to-use cartridges. Instrumental analysis was carried out on a gas chromatograph equipped with an electron capture detector (GC-ECD), using matrix-matched and internal standard calibration techniques. Confirmatory analysis by GC-MS was performed. Recoveries at the EU Maximum Residue Limit (MRL), 0.5 x MRL and 1.5 x MRL levels and the repeatabilities were widely satisfactory. The main advantage of the method was the reduction of analysis time as compared with previously published works. The applicability of the method to different matrices and pesticide classes will be investigated.
Edible portions of 12 marine organisms from several areas of the Adriatic Sea, Italy, were collected during Spring 1997 and analysed for 32 organochlorine pesticides residues and 27 polychlorobiphenyl congeners. Only eight organochlorine pesticides - hexachlorobenzene (HCB), hexachlorocyclohexane (HCH) isomers, diphenyl-dichloro-trichloroethane (DDT) group, dieldrin - were determined at levels in the range <0.01-19.88 ng g(-1) wet weight, with 1,1'-dichloro-2,2'-bis(4-chlorophenyl)ethylene (DDE) being the more relevant single organochlorine. The contamination by organochlorine pesticides was comparable in organisms from the North, Centre and South Adriatic. Polychlorinated biphenyls (PCBs) were determined at levels in the range <0.05-14.46 ng g(-1), with CB 101, 118, 138, 153, 180 and 187 being more relevant (penta-, hexa- and hepta-chlorinated congeners). The sum of PCBs congeners determined were in the range 1.18-69.05 ng g(-1). The contamination by PCBs is more relevant in organisms from the North Adriatic Sea owing to the antropic discharge from major rivers such as Po and Adige that flow through highly industrialized and densely populated areas.
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