快速溶剂萃取-凝胶色谱净化-LC／MS／MS相结合测定血中的杀参毒素类农药

目的建立血中杀参毒素类农药残留的快速分析方法。方法取一定量的Al2O3放入萃取池中做吸附剂，通过快速溶剂萃取仪萃取血液中杀参毒素类农药，同时达到在线净化的效果，后运用凝胶色谱净化联用仪进一步净化浓缩到2ml，提取液经LC／MS／MS进行检验。结果杀虫双在1．2×10g／ml～1．2×10^-6g／ml范围内线性关系良好，检出限为0．04ppb，杀虫眯为1．2×10^-6g／ml～7．2×10g／ml，检出限为0．34ppm。2种杀参毒素农药的平均回收率为89％、90％，相对标准偏差为1．9％、3％。结论整个方法简便、快速、准确、重现性好、灵敏度高，杂质干扰少。

Determination of nereistoxin toxins in the blood using LC/MS/MS coupled with accelerated solvent extraction and gel permeation chromatographic purification

Objective To establish a method for determination of nereistoxin toxins in the blood using liquid chromatography-electrospray tandem mass spectrometry. Methods The nereistoxin toxins were extraeeted with ethyl acetate ： eyclohenane（1 ： 1）, cleaned by the aluminite powder online and then by auto gel permeation chromatography. The collected solution was analyzed by the high performance liquid chromatography-tandem spectrometry（HPLC-MS/MS）. Results The calibration of bisultap and chlordimeform had a good linear relationship in the range of 1.2×10^-9 g/ml - 1.2×10^-6 g/ml and 1.2×10^-6 g/ml - 7. 2×10^-6 g/ ml, the minimal detection limits （LOD） were 0.04ppb and 0. 34ppm respectively. The average recoveries were 89% and 90%, the relative standard deviations were 1.9 % and 3 %. Conclusion The entire method can be used for qualitative and quantitative analysis of components of mixed drugs rapidly and accurately.