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

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

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1.2×10-9g/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^7.2×10-6g/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。

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.