法医学杂志

法医学杂志 ›› 2019, Vol. 35 ›› Issue (4): 411-418.DOI: 10.12116/j.issn.1004-5619.2019.04.006

• 论著 • 上一篇    下一篇

血液中20种芬太尼类物质UPLC-MS/MS法的建立及应用

施妍， 强火生， 刘伟， 向平， 沈保华， 沈敏   

  1. 司法鉴定科学研究院 上海市法医学重点实验室 上海市司法鉴定专业技术服务平台，上海 200063
  • 发布日期:2019-08-25 出版日期:2019-08-28
  • 通讯作者: 沈敏，女，研究员，主要从事体内滥用物质的鉴定及体内代谢研究；E-mail：shenm@ssfjd.cn 沈保华，男，硕士，主任法医师，主要从事体内滥用物质的鉴定研究；E-mail：shenbh@ssfjd.cn
  • 作者简介:施妍（1984—），女，博士，副研究员，主要从事体内滥用物质的鉴定研究；E-mail：shiy@ssfjd.cn
  • 基金资助:
    “十三五”国家重点研发计划资助项目（2016YFC0800704）；中央科研院所青年推进项目（2019G-4）；国家自然科学基金资助项目（81501633，81971789）；上海市法医学重点实验室资助项目（17DZ2273200）；上海市司法鉴定专业技术服务平台资助项目（19DZ2292700）；上海市法医学重点实验室开放课题资助项目（KF1806）

Establishment and Its Application of UPLC-MS/MS Method for 20 Fentanyl-related Substances in Blood#br#

SHI Yan, QIANG Huo-sheng, LIU Wei, XIANG Ping, SHEN Bao-hua, SHEN Min   

  1. Shanghai Key Laboratory of Forensic Medicine, Shanghai Forensic Service Platform, Academy of Forensic Science, Shanghai 200063, China）
  • Online:2019-08-25 Published:2019-08-28

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摘要： 目的 建立同时分析血液中20种芬太尼类物质的超高效液相色谱-串联质谱（ultra-high performance liquid chromatography-tandem mass spectrometry，UPLC-MS/MS）快速测定方法。 方法 以芬太尼-D5为内标，血液经液液萃取后用ACQUITY UPLC HSS T3色谱柱分离，采用多反应监测模式同时测定20种芬太尼类物质。 结果 各化合物的检出限为0.02~0.03 ng/mL，定量限为0.05~0.2 ng/mL。在0.05~40 ng/mL质量浓度范围内，20种芬太尼物质均具有良好的线性关系，相关系数大于0.99。方法准确度为87.69%~114.68%，提取回收率为85.35%~101.80%，无明显基质效应。运用所建方法检测注射舒芬太尼后大鼠血液中的舒芬太尼，注射后10 h在大鼠血液中仍能检出舒芬太尼。 结论 该方法前处理简单、灵敏度高、选择性好，可用于法医毒物分析中芬太尼类物质的测定。

关键词: 法医毒理学, 芬太尼类, 超高效液相色谱-串联质谱, 血液

Abstract: Objective To establish an ultra-high performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS） rapid determination method for simultaneous analysis of 20 fentanyl-related substances in blood. Methods With fentanyl-D5 as an internal standard, the blood was extracted by liquid-liquid extraction （LLE）, then separated with an ACQUITY UPLC HSS T3 chromatographic column, and finally 20 fentanyl-related substances were simultaneously analyzed with multiple reaction monitoring （MRM） mode. Results The limits of detection （LOD） of all compounds were 0.02-0.03 ng/mL, and the limits of quantitation （LOQ） were 0.05-0.2 ng/mL. Within the mass concentration range of 0.05-40 ng/mL, 20 fentanyl-related substances had a good linear relationship, and correlation coefficients were larger than 0.99. The accuracy of the method was 87.69%-114.68% and the extraction recovery rate was 85.35%-101.80%, and no significant matrix effect was observed. The established method was successfully applied to the detection of sufentanil in rat blood after sufentanil was injected. Sufentanil could still be detected in blood of rats 10 h after sufentanil injection. Conclusion The established method has the advantages of simple pretreatment, high sensitivity and good selectivity, and can be used for the determination of fentanyl-related substances in forensic toxicology analysis.

Key words: forensic toxicology, fentanyl analogues, ultra-high performance liquid chromatography-tandem mass spectrometry, blood