QuEChERS-高效液相色谱-四极杆-飞行时间质谱法正负离子切换同时检测血液中的6种除草剂  

Simultaneous Detection of Six Herbicides in Blood by QuEChERS-High Performance Liquid Chromatography-Quadrupole-Time of Flight Mass Spectrometry with Positive and Negative Ion Switching Mode

作　　者：史洪飞 徐伯芃 徐成鑫 SHI Hongfei;XU Bopeng;XU Chengxin(College of Criminal Science and Technology,Nanjing Police College,Nanjing 210023)

机构地区：[1]南京警察学院刑事科学技术学院,江苏南京210023

出　　处：《分析科学学报》2024年第2期219-224,共6页Journal of Analytical Science

基　　金：2022年国家级大学生创新重点项目(202212213022Z)。

摘　　要：建立了基于QuEChERS-高效液相色谱-四极杆-飞行时间质谱法检测血液中草除灵乙酯、二氯吡啶酸、三氯吡氧乙酸、三氟啶磺隆、丙炔氟草胺、硝黄草酮等6种除草剂的分析方法。样品用乙腈涡旋振荡提取,提取液经优化的QuEChERS方法净化,0.22μm滤膜过滤。采用ZORBAXEclipse PlusC18色谱柱(100mm×3.0mm,1.8μm),以0.1%甲酸水溶液和乙腈为流动相梯度洗脱实现色谱分离,四极杆-飞行时间质谱正负离子切换检测。结果显示,6种除草剂的线性相关系数均大于0.9981,检出限为0.02~1.95μg/L,定量限为0.07~6.49μg/L;在100μg/kg和500μg/kg两种加标水平下的样品回收率为88.19%~105.19%;仪器精密度为0.39%~1.65%,日内方法精密度为0.81%~2.93%,日间方法精密度为0.08%~2.85%。所建立方法灵敏度高、稳定性强、分析速度快,能够满足血液中除草剂成分的定性、定量分析需要,可为除草剂中毒案件中生物检材的检验提供参考。An analytical method based on QuEChERS-high performance liquid chromatography-quadrupole-time of flight mass spectrometry was developed for the determination of six herbicides,including Clopyralid,Mesotrione,Trifloxysulfuron,Triclopyr,Flumioxazin,Benazolinethyl in blood.The samples were extracted with acetonitrile by vortex oscillation,and the extracts were purified by the optimized QuEChERS method and filtered by 0.22μm filter membrane.The chromatographic separation was achieved on a ZORBAX Eclipse Plus C18 column(100 mm×3.0 mm,1.8μm)with a gradient elution of 0.1%formic acid aqueous solution and acetonitrile as the mobile phases,and the detection was switched between positive and negative ions by quadrupole-time of flight mass spectrometry.The linear correlation coefficient of the six herbicides were greater than 0.9981,the limit of detection(LODs)were in the range of 0.02-1.95μg/L and the limit of quantification(LOQs)were in the range of 0.07-6.49μg/L.The recoveries of six herbicides were in the ranges of 88.19%-105.19%at the two spiked levels of 100 and 500μg/kg.The intra-sample precisions were between 0.39%-1.65%.The intra-day precisions were between 0.81%-2.93%,and the inter-day precisions were between 0.08%-2.85%.This method has fast sample pretreatment speed,high sensitivity,good stability and high accuracy,which can meet the qualitative and quantitative analysis needs of herbicide components in blood.It can provide reference for the testing of biological samples in herbicide poisoning cases.

关 键 词：高效液相色谱 四极杆-飞行时间质谱法 正负离子切换模式 血液 除草剂 

分 类 号：O657.63[理学—分析化学]