法医学杂志

法医学杂志 ›› 2019, Vol. 35 ›› Issue (4): 419-422.DOI: 10.12116/j.issn.1004-5619.2019.04.007

• 论著 • 上一篇    下一篇

HPLC-MS/MS法测定大鼠血浆样品中4-FMA含量#br#

郑茜1， 温美强1，2， 贾娟1， 王涛1， 尉志文1， 马红娟1， 王优美3， 徐鹏3， 贠克明1   

  1. 1. 山西医科大学，山西 太原 030001； 2. 沈阳药科大学，辽宁 沈阳 110000； 3. 公安部禁毒情报技术中心 国家毒品实验室，北京 100193
  • 发布日期:2019-08-25 出版日期:2019-08-28
  • 通讯作者: 徐鹏，女，博士，副研究员，主要从事毒品和新精神活性物质研究；E-mail：pengxu750@163.com 贠克明，男，博士，教授，主要从事法医毒物动力学研究；E-mail：yunkeming5142@163.com
  • 作者简介:郑茜（1988—），女，博士，在站博士后，讲师，主要从事天然药物化学及药物代谢动力学研究；E-mail：qianz88@163.com
  • 基金资助:
    国家科技基础性工作专项资助项目（2015FY111400）；国家重点研发计划资助项目（2017YFC0803504）；中国博士后科学基金资助项目（2018M641678）

Determination of the Content of 4-FMA in Rat Plasma Samples by HPLC-MS/MS Method

ZHENG Qian1, WEN Mei-qiang1,2, JIA Juan1, WANG Tao1, WEI Zhi-wen1, MA Hong-juan1, WANG You-mei3, XU Peng3, YUN Ke-ming1   

  1. 1. Shanxi Medical University, Taiyuan 030001, China; 2. Shenyang Pharmaceutical University, Shenyang 110000, China; 3. National Narcotics Laboratory, Drug Intelligence and Forensic Center of Ministry of Public Security, Beijing 100193, China
  • Online:2019-08-25 Published:2019-08-28

PDF (PC)

671

摘要： 目的 建立一种测定大鼠血浆中新精神活性物质4-氟甲基苯丙胺（4-fluoromethamphetamine，4-FMA）含量的高效液相色谱-串联质谱（high performance liquid chromatography-tandem mass spectrometry，HPLC-MS/MS）分析方法，为4-FMA在大鼠体内的毒物代谢动力学研究提供方法基础。 方法 大鼠血浆样品中加入内标物甲基苯丙胺（methamphetamine，MA），经甲醇沉淀蛋白后采用Poroshell 120 EC-C18色谱柱分离，0.1%甲酸水溶液和0.1%甲酸乙腈溶液为流动相，流速为0.4 mL/min，采用电喷雾离子源在多反应监测模式下进行检测。 结果 血浆样品中4-FMA在质量浓度5~1 000 ng/mL范围内线性关系良好（r>0.999），检出限为3 ng/mL，定量限为5 ng/mL。准确度以相对误差（relative error，RE）表示，在±5%范围内，日内精密度与日间精密度［以相对标准偏差（relative standard deviation，RSD）表示］<9%，提取回收率>90%。血浆样品的分析检测在2.5 min内完成。 结论 本研究建立了大鼠血浆样品中4-FMA的HPLC-MS/MS测定方法，该方法准确、快速、简单、灵敏，适用于4-FMA的代谢动力学研究。

关键词: 法医毒理学, 高效液相色谱-串联质谱, 4-氟甲基苯丙胺, 血浆, 大鼠

Abstract: Objective To develop a high performance liquid chromatography-tandem mass spectrometry （HPLC-MS/MS） method for the determination of the content of 4-fluoromethamphetamine （4-FMA） in rat plasma, and to provide a methodological basis for the study of the toxicokinetics of 4-FMA in rats. Methods Rat plasma samples were added into internal standard methamphetamine （MA）. Its proteins were precipitated with methanol and then separated with Poroshell 120 EC-C18 chromatographic column. A 0.1% formic acid aqueous solution and a 0.1% formic acid acetonitrile solution were used as the mobile phase at the flow rate of 0.4 mL/min. Electrospray ionization source was used for detection in the multiple reaction monitoring （MRM） mode. Results The linear relationship was good when the mass concentration of 4-FMA in plasma samples was in the range of 5-1 000 ng/mL （r>0.999）. The limit of detection （LOD） was 3 ng/mL and the limit of quantification （LOQ） was 5 ng/mL. The accuracy was expressed as relative error （RE）, and in the range of ±5%, the intra-day precision and inter-day precision （relative standard deviation, RSD） less than 9%, and the extraction recovery rate was more than 90%. The analysis and detection of plasma samples were completed within 2.5 min. Conclusion This study developed a HPLC-MS/MS method for the determination of 4-FMA in rat plasma samples. This method is accurate, rapid, simple and sensitive and can be applied to the study of toxicokinetics of 4-FMA.

Key words: forensic toxicology, high performance liquid chromatography-tandem mass spectrometry, 4-fluoromethamphetamine, plasma, rats