Development and Validation of an Analytical Method for Residues of Organochlorine, Fenopropathrin and Poly Chlorinated Biphnyl Compounds in Fatty Food

Abstract

A multi-residue method for the quantification of 9 organochlorine pesticides, one syntheticpyrithroid and 7 members of PCBs compounds residues in fish is described. The methodinvolves the application of a modified pesticide manual procedure followed by GC-ECD (GasChromatography coupled with Electron Capture Detector) analysis. The method is validatedaccording to the European Union SANCO/12495/2011 guidelines and Pesticide Manual ofAnalytical methods. The validation levels were 0.01; 0.04; and 0.2 mg /kg for organochlorinesexcept fenopropathrin (a synthetic pyrithroid insecticide) which has been validated at theconcentration of 0.02, 0.08 and 0.4 mg /kg and for PCBs at 0.005, 0.02 and 0.1 mg/kg.Acceptable values were obtained for the following parameters: limit of detection LOD (rangedbetween 0.003-0.009 mg/kg for organochlorine pesticides and 0.002 mg/kg for PCB’s) and limitof quantification (LOQ) (0.005 mg/kg for PCB’s and in the range of 0.01-0.02 mg/kg fororganochlorine compounds). The recovery percentages ranged between 70 and 120%, and themeasurement uncertainty tests was ±40.0%. The method showed to be linear from the LOQ up to the maximum level; 0.1 mg/kg for PCB’s and in the range of 0.2-0.4 mg/kg for organochlorinecompounds. These results demonstrate the applicability of this method in the routine practicefor detecting the residues of such compounds in fatty food.