大米中13种有机磷农药的固相萃取结合大体积进样／气相色谱-质谱法快速分析

Rapid Analysis of 13 Pesticide Residues in Rice by Large Volume Injection/Gas Chromatography-Mass Spectrometry Coupled with Solid Phase Extraction

利用固相萃取柱对样品进行前处理，采用胃袋式大体积进样技术结合气相色谱-质谱（GC—MS），建立了大米中13种有机磷农药的快速分析方法。以保留时间和特征离子丰度比进行定性，以峰面积外标法进行定量。结果表明，除乐果外，其余12种有机磷农药的添加回收率为82％～96％，RSD为2．09％～9．09％，检出限（S／N=3）为0．03～5μg／kg。

A stomach large volume injection/gas chromatography -mass spectrometry（ LVI/GC -MS） coupled with solid phase extraction （SPE） method for the determination of 13 pesticide residues in rice sample was presented in this paper. Compounds were identified with their retention times, qualifier and target ions, and their qualifier/target abundance ratios. Quantifications were based on external standard addition. The limits of detection （LODs） were confirmed by the real value of the signal-to-noise ratio of 3 ： 1, the limits of quantification （LOQs） were confirmed by the real value of the signal-to-noise ratio of 10 ： 1. The recoveries obtained ranged from 82% to 96% with the relative standard deviations between 2. 09% and 9. 09% , except dimethoate. The detection limits of the method ranged from 0. 03 -5 μg/kg