[Simultaneous determination of 64 pesticide residues in shellfish by accelerated solvent extraction coupled with gas chromatography-tandem mass spectrometry].

A method was established for the determination of 64 pesticide residues in shellfish using accelerated solvent simultaneous extraction and purification coupled with gas chromatography-tandem mass spectrometry (GC-MS/MS). The target compounds were extracted from shellfish using 90% (v/v) acetonitrile aqueous solution with 60% of the pool volume at 85℃ via a single cycle of accelerated solvent extraction. The extracts were synchronously purified with primary secondary amine (PSA) and graphitized carbon black (GCB) added to the extracting cell. After concentration, the target compounds were detected by GC-MS/MS in the multiple reaction monitoring (MRM) mode, and quantified by using the external standard method. Under the optimized conditions, good linearities were obtained for the 64 pesticides in the range of 10.0-1000 μg/L, with coefficients of determination greater than 0.989. The limits of quantification for the method were between 2.0 μg/kg and 10.0 μg/kg. At four spiked levels (5.0, 10.0, 100 μg/kg, and the LOQ level) in clam, the recoveries of all the pesticides were between 69.4% and 129.7%, with the relative standard deviations varying from 0.7% to 16.0% (