超高效液相色谱-四极杆/静电场轨道阱高分辨质谱测定血液和肝脏中12种拟除虫菊酯类农药  

Determination of 12 Pyrethroid Pesticides in Blood and Liver by UPLC-QE-Orbitrap HRMS

作　　者：张鹤耀 国菲 贾振军[1] 李鹏 ZHANG He-yao;GUO Fei;JIA Zhen-jun;LI Peng(School of Investigation,People’s Public Security University of China,Beijing 100038,China;Judicial Appraisal Center of Zibo Public Security Bureau Organization-Company,Zibo 255022,China;School of Forensic Medicine,Shanxi Medical University,Taiyuan 030001,China)

机构地区：[1]中国人民公安大学侦查学院,北京100038 [2]山东省淄博市公安局刑侦支队,山东淄博255022 [3]山西医科大学法医学院,山西太原030001

出　　处：《分析测试学报》2023年第4期439-446,共8页Journal of Instrumental Analysis

基　　金：毒物基础数据库的建设项目(2022SJKJS07)。

摘　　要：建立了超高效液相色谱-四极杆/静电场轨道阱高分辨质谱(UPLC-QE-Orbitrap HRMS)测定血液和肝脏中12种拟除虫菊酯类农药的分析方法。血液和肝脏样品经乙腈沉淀蛋白后,采用Hypersil GOLD VAN⁃QUISH色谱柱(1.9μm,2.1 mm×100 mm),以5 mmol/L乙酸铵溶液(含0.1%甲酸)和甲醇作为流动相进行梯度洗脱分离,采用全扫描及自动触发二级质谱(Full MS/dd-MS2)进行检测。结果显示:12种拟除虫菊酯类农药在各自线性范围内线性良好(r2≥0.9904),血液和肝脏中的检出限分别为1~18 ng/mL和1~18 ng/g,定量下限分别为2~20 ng/mL和2~20 ng/g,基质效应为82.3%~117%,回收率为74.1%~120%,日内精密度(In⁃tra-RSD)≤11%,日间精密度(Inter-RSD)≤12%。该方法满足公安机关办理实际案件要求,适用于血液和肝脏样本中拟除虫菊酯类农药的检验鉴定。A method for the determination of 12 pyrethroid pesticides in blood and liver by ultra per⁃formance liquid chromatography-quadrupole/electrostatic field orbittrap high-resolution mass spec⁃trometry(UPLC-QE-Orbitrap HRMS)was developed.After acetonitrile precipitation,the blood and liver were separated by gradient elution on a Hypersil GOLD VANQUISH analytical column(1.9μm,2.1 mm×100 mm)with 5 mmol/L ammonium acetate(containing 0.1%formic acid)and methanol as mobile phase.Full scan and automatic trigger secondary mass spectrometry(Full MS/dd-MS2)were used for detection.The experimental results showed that the linearities of 12 pyre⁃throid pesticides were good in their linear range(r2≥0.9904).The limits of detection in blood and liver were in the range of 1-18 ng/mL and 1-18 ng/g,respectively.The limits of quantitation were 2-20 ng/mL and 2-20 ng/g,respectively.The matrix effects were 82.3%-117%,and the recoveries were 74.1%-120%.The intra-day RSD(intra-RSD)were not more than 11%,and interday RSD(inter-RSD)were not more than 12%.This method could meet the requirements of public se⁃curity organs in handling actual cases and was suitable for the detection and identification of pyre⁃throid pesticides in blood and liver samples.

关 键 词：超高效液相色谱-四极杆/静电场轨道阱高分辨质谱(UPLC-QE-Orbitrap HRMS) 拟除虫菊酯 血液 肝脏 检测 

分 类 号：O657.63[理学—分析化学] F767.2[理学—化学]