超高效液相色谱-串联质谱法快速测定血浆中乙草胺和异丙甲草胺  

Rapid determination of avermactin and metolachlor in plasmas by ultra performance liquid chromatography-tandem mass spectrometry

作　　者：李启[1] 纪律[1] 徐峻卿 杨秀丽 LI Qi;JI Lv;XU Jun-qing;YANG Xiu-li(Examination and Test Institute,Lishui Municipal Center for Disease Control and Prevention,Lishui,Zhejiang 323000,China)

机构地区：[1]丽水市疾病预防控制中心,浙江丽水323000

出　　处：《中国卫生检验杂志》2022年第7期798-801,共4页Chinese Journal of Health Laboratory Technology

基　　金：浙江省公共卫生应急检测关键技术重点实验室开放基金(202003);丽水市科技计划项目(2021ZDYF17)。

摘　　要：目的建立一种适用于公共卫生快速确证检测血浆中乙草胺和异丙甲草胺的超高效液相色谱-串联质谱方法。方法取血浆样本,以1.3的比例加入乙腈。旋涡1 min,10000 r/min、4℃离心3 min,吸取上清液于样品瓶中,以0.1%甲酸和乙腈进行超高效液相分离,在电喷雾正离子模式下进行多反应监测检测。结果乙草胺的检出限为0.3μg/L(S/N=3),在5μg/L、10μg/L、20μg/L 3个加标水平下的回收率为93.8%~108.8%,相对标准偏差为1.8%~7.9%(n=7)。异丙甲草胺的检出限为0.01μg/L(S/N=3),在3个加标水平下的回收率为92.9%~111.4%,相对标准偏差为2.5%~8.8%(n=7)。结论本方法操作简便,建立的超高效液相色谱质谱检测技术可实现大批量样本中乙草胺和异丙甲草胺的同时快速测定,为除草剂快速应急检测提供了技术研究平台。Objective To establish an ultra performance liquid chromatography-tandem mass spectrometry method for rapid and confirmatory determination of acetochlor and metolachlor in plasma.Methods Taking plasma samples and add acetonitrile in the ratio of 1.3,and after vortex oscillation for 1 min at 10000 r/min,and centrifugation at 4℃for 3 min,the supernatant was taken and placed in a sample bottle.The samples were separated by ultra high performance liquid chromatography with0.1%formic acid and acetonitrile,and detected by multiple reaction monitoring in positive electrospray ionization mode.Results The limit of detection for avermactin was 0.3μg/L(S/N=3).The recoveries at 5μg/L,10μg/L and 20μg/L spiked levels were 93.8%-108.8%with relative standard deviations of 1.8%-7.9%(n=7).The limit of detection for metolachlor was 0.01μg/L(S/N=3).The recovery ranged from 92.9%to 111.4%and the relative standard deviation were2.5%-8.8%(n=7).Conclusion The method is simple.The established ultra performance liquid chromatography-mass spectrometry detection technology can realize the rapid simultaneous determination of acetochlor and metolachlor in large quantities of samples,which provides a research platform for rapid emergency detection of herbicides.

关 键 词：乙草胺 异丙甲草胺 血浆 超高效液相色谱-串联质谱法 

分 类 号：O657.63[理学—分析化学]