气相色谱-负化学离子源质谱法同时检测蔬菜中103种农药残留

Simultaneous Determination of 103 Pesticide Residues Using Gas Chromatography-Negative Chemical Ionization Mass Spectrometry

本文比较了负化学电离（NCI）和电子轰击电离（EI）两种电离方式下采用气相色谱-质谱（GC-MS）同时检测103种农药的灵敏度,发现在NCI方式下103个化合物信噪比分别提高1.2~447.0倍。将GC-NCI/MS方法应用于蔬菜中103种农药的检测,检出限在0.06~13.1μg/kg之间,添加水平为20μg/kg和100μg/kg时,回收率在63.5%~123.8%之间,相对标准偏差为3.6%~13.3%。研究结果表明,相对于常用的GC-EI/MS检测方法,上述103个农药更适合采用NCI方式进行GC-MS同时分析。

In the present paper,GC-NCI/MS and GC-EI/MS was compared for the analysis of 103 pesticides,and it was found that much lower detection limits（1.2~447.0 times lower） for the investigated pesticides could be obtained by GC-NCI/MS.Based on this observation,a method was proposed for the simultaneous determination of 103 pesticide residues in vegetable samples by GC-NCI/MS.The detection limits（S/N=3） of the developed method were found to be 0.06～13.1 μg/kg for 103 pesticide residues in vegetable samples.The average recoveries of 103 pesticides in spiked vegetable samples ranged from 63.5% to 123.8%,with RSDs less than 13.3%.