UPLC-MS/MS法同时检测全血中16种除草剂

Simultaneous UPLC-MS/MS Determination of 16 Herbicides in Whole Blood

目的建立全血中16种除草剂的超高效液相色谱-串联质谱(UPLC-MS/MS)同时检测方法,为除草剂中毒案事件及其他刑事案件血液中该16种除草剂的检验鉴定提供依据。方法取200μL的血液,加入800μL乙腈-水(体积比80/20),进行蛋白沉淀后,采用Acquity BEH C18(2.1mm×100mm,1.7μm)色谱柱,以水(5mmol/L的甲酸铵,0.1%的甲酸)-乙腈为流动相进行梯度洗脱,采用电喷雾离子源(ESI)、多反应监测(MRM)正离子模式对16种化合物进行检测。结果在1~200ng/mL范围内线性关系良好,R2均大于0.996;基质效应(ME%)为85.2%~104.4%,相对标准偏差(RSD%)为0.72%~4.84%;仪器检出限(IDLs)为0.2~2 ng/mL(信噪比S/N≥3),方法检出限(MDLs)为0.5~3ng/mL(信噪比S/N≥3),最低定量限(LOQs)为1~7ng/mL(信噪比S/N≥10)。结论本实验建立的全血中16种除草剂同时检验方法,前处理简便快捷、回收率高、精密度好、方法检出限低,可作为该16种除草剂中(投)毒案件的检验方法。

Objective To establish a method for simultaneous determination of 16 herbicides in whole blood through UPLC-MS/MS so as to provide reference for identifi cation of the herbicidal poisoning and relevant cases.Methods 200μL sampling blood,spiked of 16 selected herbicides,was added with 800μL solution of acetonitrile-water(80/20,V/V)to have the protein precipitated.Through the Acquity UPLC BEH C18(100×2.1mm,1.8μm)column being fl owed with 0.1%formic acid water(5mmol/L ammonium formate)-acetonitrile as the mobile phase,the treated blood was undergone into the UPLCMS/MS detection that was carried out under the electrospray positive ionization(ESI+)and MRM mode,having the 16 selected herbicides analyzed.Results The 16 herbicides showed good linear relationship in the range of 1-200 ng/mL,with the coeffi cients of determination being R2>0.996,matrix effects(ME%)85.2%-104.4%,and the relative standard deviations(RSD%)0.72%-4.84%.The method revealed its instrument detection limits(IDLs)0.2-2ng/mL(S/N≥3),detection limits(MDLs)0.5-3ng/mL(S/N≥3),and limits of quantifi cation(LOQs)1-7ng/mL(S/N≥10).Conclusions Such one simultaneous method established here for determination of 16 herbicides in whole blood is simple and efficient,demonstrating high recovery,high precision and low detection limit,capable of determination of the 16 herbicides and similar poisoning cases.