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Simple-QuEChERS Nano结合GC-MS/MS同时检测全血中的97种农药
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作者单位
王丹,董林沛,任昕昕,姜红,王爱华,常靖,张云峰,张曦 1.中国人民公安大学侦查学院北京1000382.公安部物证鉴定中心北京1000383.岛津企业管理(中国)有限公司北京100020 
基金项目:国家重点研发计划课题(2018YFC0807301);中央级公益性科研院所基本科研业务费项目(2019JB002)
中文摘要:建立了Simple-QuEChERS Nano结合气相色谱-串联质谱(GC-MS/MS)同时检测血液中97种农药的方法,并对基质条件、提取溶剂以及净化材料进行了优化。05 mL血液样品经3倍水稀释混匀,使用20 mL乙酸乙酯提取后振荡、离心,过Simple-QuEChERS Nano净化柱及022 μm有机微孔滤膜后,采用多反应监测模式(MRM)进行分析。结果显示,97种农药在一定质量浓度范围内线性关系良好(r2≥0987 3),除丙烯菊酯(检出限和定量下限分别为1103、3676 ng/mL)外,其余农药的检出限为006~427 ng/mL,定量下限为018~1424 ng/mL。采用空白全血进行加标回收实验,97种农药在100、200、400 ng/mL 3个加标水平下的回收率为322%~120%,日内精密度为19%~11%,日间精密度为36%~13%。该方法由传统QuEChERS方法改进,绿色环保、操作简单、快速高效,可用于血液中多种农药的同时检测,用于实际案件血液样品中农药的筛查与定性定量检验,获得了良好的结果。
中文关键词:Simple-QuEChERS Nano  气相色谱-三重四极杆串联质谱(GC-MS/MS)  血液  农药
 
Simultaneous Determination of 97 Pesticides in Human Blood by Gas Chromatography-Triple Quadrupole Mass Spectrometry with Simple-QuEChERS Nano
Abstract:A method was established for simultaneous detection of 97 pesticides in human blood by gas chromatography-tandem mass spectrometry(GC-MS/MS) with Simple-QuEChERS Nano.05 mL of blood sample was added to a 15 mL conical bottom polypropylene centrifuge tube and mixed with 15 mL water,then extracted with 20 mL ethyl acetate.The tube was oscillated for 10 min at 20 r/min,and then centrifuged at 8 000 r/min for 10 min.After that,the supernatant of extracts was purified by filtration through a Simple-QuEChERS Nano column and 022 μm organic membrane filter,then detected in multiple reaction monitoring(MRM) mode.There were good linear relationships for all the analytes except fenitrothion,with their correlation coefficients(r2) no less than 0987 3.The limits of detection(LODs) and the limits of quantification(LOQs) for 96 pesticides except allethrin(LOD and LOQ was 1103,3676 ng/mL) ranged from 006 ng/mL to 427 ng/mL and 018 ng/mL to 1424 ng/mL,respectively.At three spiked levels of 100,200,400 ng/mL,the recoveries for 97 kinds of pesticides ranged from 322% to 120%.The intra day precision and inter day precision of the method evaluated at a concentration of 100 ng/mL ranged from 19% to 11% and 36% to 13%,respectively.The developed method,optimized by the traditional QuEChERS method,was not only environmentally friendly,but also improved the efficiency of sample pre treatment and exhibited an enhanced performance in purifying blood sample,which could be used for the qualitative and quantitative analysis of multi pesticides in blood samples of forensic cases.
Key Words:Simple-QuEChERS Nano  gas chromatography-triple quadrupole mass spectrometry  human blood  pesticides
引用本文:王丹,董林沛,任昕昕,姜红,王爱华,常靖,张云峰,张曦.Simple-QuEChERS Nano结合GC-MS/MS同时检测全血中的97种农药[J].分析测试学报,2021,40(3):347-355.
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