Multi-residue method for the determination of organochlorine pesticides in fish feed based on a cleanup approach followed by gas chromatography-triple quadrupole tandem mass spectrometry

摘要

A multi-residue method for the determination of organochlorine pesticides in fish feed samples was developed and optimized. The method is based on a cleanup step of the extracted fat, carried out by liquid-liquid extraction on diatomaceous earth cartridge with n-hexane/acetonitrile (80/20, v/v) followed by solid phase extraction (SPE) with silica gel-SCX cartridge, before the identification and quantification of the residues by gas chromatography-triple quadrupole tandem spectrometry (GC-MS/MS). Performance characteristics, such as accuracy, precision, linear range, limits of detection (LOD) and quantification (LOQ), for each pesticide were determined. Instrumental LODs ranged from 0.01 to 0.11μgL~(-1), LOQs were in the range of 0.02-0.35μgL~(-1), and calibration curves were linear (r~2>0.999) in the whole range of explored concentrations (5-100μgL~(-1)). Repeatability values were in the range of 3-15%, evaluated from the relative standard deviation of six samples spiked at 100μgkg~(-1) of fat, and in compliance with that derived by the Horwitz's equation. No matrix effects or interfering substances were observed in fish feed analyses. The proposed method allowed high recoveries (92-116%) of spiked extracted fat samples at 100μgkg~(-1), and very low LODs (between 0.02 and 0.63μgkg~(-1)) and LOQs (between 0.05 and 2.09μgkg~(-1)) determined in fish feed samples.