谷粮中硫丹及其代谢物残留的GC-MS分析

Determination of Endosulfan and the Metabolite Residues in Grain by GC-MS

本文建立了固相萃取-气相色谱-质谱法(SPE-GC-MS)同时测定谷粮中硫丹及其代谢物的方法。样品经过正己烷提取、固相萃取柱净化,采用GC-MS检测,外标法定量。在此条件下,样品加标回收率在87.3%～110.2%之间,相对标准偏差在1.7%～3.9%之间(n=6),方法检出限(S/N=3)为0.002mg/kg～0.003mg/kg。该方法简便、快速,具有良好的灵敏度、重复性,可适用于谷粮中硫丹及其代谢物残留的检测。

An analytical method was developed for the simultaneous determination of endosuffans and its metabolite residues in grain based on solid phase extraction （SPE） coupled with gas chromatography-mass speetrometry（GC-MS）. The pesticide residues in grain were extracted with hexane, purified with solid phase extraction columns. Under this condition , the average recoveries in different addition levels of endosulfans and its metabolite were 87.3%-110.2%, the relative standard deviations werel.7%-3.9%（n=6）, and the detection limits were in the range of 0.002mg/kg-0.003mg/kg （S/ N=3）. The proposed method was sample, rapid, sensitive and applicable to the determination of endosu]fans and its metabolite residues in grain.