[Simultaneous determination of 12 rodenticides in whole blood and urine samples by high performance liquid chromatography-tandemmass spectrometry]

Zhonghua Lao Dong Wei Sheng Zhi Ye Bing Za Zhi. 2018 Jul 20;36(7):538-541. doi: 10.3760/cma.j.issn.1001-9391.2018.07.017.
[Article in Chinese]

Abstract

Objective: To develop a method for Simultaneous and rapid determination of 12 rodenticides including pindone, vacor, coumatetralyl, warfarin, diphacinone, coumachlor, chlorphacinon, difenacoum, brodifacoum, bromadiolone, difethialone and flocoumafen in whole blood and urine samples by high performance liquid chromatography-tandem mass (LC-MS-MS) . Methods: The whole blood samples were precipitated with acetonitrile, purified by OstroTM 96-well plate, The urine samples were extracted by acetonitrile, and then separated on a ODS column, analyzed with high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) . The external standard calibration were tested. Results: A good linearity was observed in their respective concentration ranges of 12 rodenticides. The related coefficients were 0.993 0~0.999 8. The limit of detections were 0.05 μg/L~1.4 μg/L. The rates of recovery were 92.5%~118.0%. The relative standard deviations were between 0.8%~17.3%. Conclusion: The method was simple, rapid, sensitive, accurate and suitable for simultaneous detection of the 12 rodenticides in whole blood and urine samples of intoxicated patients.

目的: 建立全血和尿液中杀鼠酮、灭鼠优、杀鼠迷、杀鼠灵、敌鼠、氯杀鼠灵、氯敌鼠、鼠得克、溴鼠灵、溴敌隆、噻鼠灵、氟鼠灵12种杀鼠剂同时快速测定的液相色谱-串联质谱测定方法。 方法: 全血样品用乙腈沉淀蛋白,经Ostro 96孔磷脂去除板净化,尿液样品用乙腈直接提取,采用ODS反相色谱柱分离,高效液相色谱-串联质谱多反应监测(MRM)模式检测,外标法定量。 结果: 12种杀鼠剂在各自质量范围内线性良好,相关系数为0.993 0~0.999 8,方法检出限在0.05~1.4 μg/L之间,样品加标回收率在92.5%~118.0%之间,相对标准偏差(RSD)在0.8%~17.3%之间。 结论: 该方法简便、快速、灵敏、准确,适用于中毒病人全血和尿液中12种杀鼠剂的同时测定。.

Keywords: LC-MS/MS; Rodenticides; Urine; Whole blood.

MeSH terms

  • Anticoagulants
  • Chromatography, High Pressure Liquid / methods*
  • Humans
  • Rodenticides / blood*
  • Rodenticides / urine*
  • Spectrum Analysis
  • Tandem Mass Spectrometry / methods*

Substances

  • Anticoagulants
  • Rodenticides