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

ZHANG He-yao; GUO Fei; JIA Zhen-jun; LI Peng

doi:10.19969/j.fxcsxb.22101203

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

Scientific Papers | 更新时间：2023-04-18

- Determination of 12 Pyrethroid Pesticides in Blood and Liver by UPLC－QE－Orbitrap HRMS
- Journal of Instrumental Analysis Vol. 42, Issue 4, Pages: 439-446(2023)
- 作者机构：
  
  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
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.22101203
  CLC：
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张鹤耀,国菲,贾振军等.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[J].分析测试学报,2023,42(04):439-446.

ZHANG He-yao,GUO Fei,JIA Zhen-jun,et al.Determination of 12 Pyrethroid Pesticides in Blood and Liver by UPLC－QE－Orbitrap HRMS[J].Journal of Instrumental Analysis,2023,42(04):439-446.
张鹤耀,国菲,贾振军等.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[J].分析测试学报,2023,42(04):439-446. DOI： 10.19969/j.fxcsxb.22101203.

ZHANG He-yao,GUO Fei,JIA Zhen-jun,et al.Determination of 12 Pyrethroid Pesticides in Blood and Liver by UPLC－QE－Orbitrap HRMS[J].Journal of Instrumental Analysis,2023,42(04):439-446. DOI： 10.19969/j.fxcsxb.22101203.

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 VANQUISH色谱柱（1.9 µm，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－MS,2,）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（,r,2, ≥ 0.990 4），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（Intra-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。

Abstract

A method for the determination of 12 pyrethroid pesticides in blood and liver by ultra performance liquid chromatography－quadrupole/electrostatic field orbittrap high-resolution mass spectrometry（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（1.9 µm，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－MS,2,） were used for detection．The experimental results showed that the linearities of 12 pyrethroid pesticides were good in their linear range（,r,2, ≥ 0.990 4）．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 inter-day RSD（inter-RSD） were not more than 12%．This method could meet the requirements of public security organs in handling actual cases and was suitable for the detection and identification of pyrethroid 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

Keywords

ultra performance liquid chromatography－quadrupole/electrostatic field orbittrap high-resolution mass spectrometry（UPLC－QE－Orbitrap HRMS）pyrethroidsbloodliverdetection

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Hubei Key Laboratory of Novel Reactor and Green Chemical Technology，Wuhan Institute of Technology

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