GC-NCI-MS分析粮谷中多类农药残留

Multiresidue determination in grain by gas chromatography-negative chemical ionization-mass spectrometry

摘要: 建立了粮谷中14种农药残留(9种有机氯、3种拟除虫菊酯和2种含氯有机氮)气相色谱-负化学源-质谱(GC-NCI-MS)的分析方法,试样样品用V(正己烷):V(丙酮)=1:1超声波提取,硅镁吸附剂净化,采用GC-NCI-MS选择离子扫描方式检测.结果表明,该方法准确、快速、选择性好、抗干扰能力强,14种农药的方法最低检出限:0.01~0.18μg/kg,平均添加回收率在75.2%~109.7%之间,变异系数都小于10%,并成功应用于大米、面粉试样中痕量农药残留分析.

Abstract: A simultaneous determination of 14 pesticides(9 organochlorines,3 pyrethroid and 2 organonitrogen)in grain was developed.Pesticides were extracted from sample with 1:1 hexane-acetone in an ultrasonic bath and were purified on a Florisil column,then were determined by gas chromatography with negative chemical ionization mass spectrometer,using ion monitoring mode.The method was accurate,covenient,sensitive and selective.The detection limit of the method was 0.01—0.18 μg/kg,the average recoveries ranged from 75.2% to 109.7%,while the relative standard deviations were less then 10%.The analytical method was successfully applied to determine pesticides in several grain samples.