A method was developed for the rapid determination of 32 pesticide residues,including organ ochlorine,organophosphate and pyrethroid pesticides,in milk based on gas chromatography-ion trap tandem mass spectrometry.Electron impact ionization or chemical ionization were selected for the analytes with different sensitivities.Experimental parameters influencing the behaviours of compounds in the analysis of MS/MS were investigated and optimized.The mechanisms for the influencing factors were also discussed.Under the optimal conditions,the calibration curves for 32 pesticides were linear in the ranges of 25(10)-500(200) μg/L with correlation coefficients more than 0994.The method detection limits(MDL) for fention and chlorpyriphos were 1.7 μg/kg and 2.8 μg/kg,respectively,while those for the other pesticides were in the range of 0.026-1.2 μg/kg.The recoveries for 32 pesticides at two spiked levels of 50 and 200 μg/kg(organochlorine pesticides were spiked at 20 and 100 μg/kg) ranged from 71.5% to 116% with relative standard deviations(RSDs) of 1.9%-14%.The proposed method was applied in the detection for real samples,and could reduce the possibility of false positive results with strong anti interference.
关键词
气相色谱-离子阱串联质谱(GC-IT-MS/MS)电子轰击电离化学电离有机氯有机磷拟除虫菊酯
Keywords
gas chromatography-ion trap tandem mass spectrometry(GC-IT-MS/MS)electron impact ionizationchemical ionizationorganochlorineorganophosphatepyrethroid