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

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 0.11 μg L−1, LOQs were in the range of 0.02–0.35 μg L−1, and calibration curves were linear (r2 > 0.999) in the whole range of explored concentrations (5–100 μg L−1). Repeatability values were in the range of 3–15%, evaluated from the relative standard deviation of six samples spiked at 100 μg kg−1 of fat, and in compliance with that derived by the Horwitzʹs 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 100 μg kg−1, and very low LODs (between 0.02 and 0.63 μg kg−1) and LOQs (between 0.05 and 2.09 μg kg−1) determined in fish feed samples.