Determination of 41 pond cleaning commonly used pesticide residues in crucian carp and bottom sediment by gas chromatography-tandem mass spectrometry

An analytical method for the determination of 41 pesticide residues in crucian carp and bottom sediment was established using modified QuEChERS sample preparation and gas chromatography-tandem mass spectrometry (GC-MS/MS). The crucian carp samples were extracted by acetonitrile and ethyl acetate (V:V = 1:1) and cleaned-up with 600 mg Alumina-B. The bottom sediment samples were extracted by ethyl acetate and cleaned-up with 600 mg Florisil and 150 mg Graphitized carbon black. The pesticide residues were analyzed by GC-MS/MS. A HP-5MS column was used for the separation, and the electron ionization (EI) was employed using dynamic multiple reaction monitoring (dMRM) mode for the detection. The matrix-matched external standard calibration curves were used for quantitative analysis. The method validation results indicated that in crucian carp, the instrumental limits of detection (LOD) for 41 pesticides were 0.05-2.5 μg/L, and the limits of quantification (LOQ) were 0.1-5.0 μg/kg for the method. The linear correlation coefficients (r) of the calibration curves were 0.9960-0.9999. The average recoveries at three spiked levels (LOQ, 2LOQ and 10LOQ) were 73%-116% (n = 6) with relative standard deviations (RSDs) of 0.65%-13%. In aquaculture sediment, the instrumental LODs for 41 pesticides were 0.05-2.5 μg/L, and the LOQs were 0.1-5.0 μg/kg for the method. r of the calibration curves were 0.9964-1.000. The average recoveries at three spiked levels (LOQ, 2LOQ and 10LOQ) were 73%-104% (n = 6) with RSDs of 0.051%-10%. The method was rapid, sensitive and accurate, and has a good application prospect in the detection of amides, triazines, phenyl pyrazoles, organochlorine and organophosphorus pesticide residues in crucian carp and bottom sediment.