法医学杂志

法医学杂志 ›› 2026, Vol. 42 ›› Issue (4): 318-327.DOI: 10.12116/j.issn.1004-5619.2026.360203

• 论著 • 上一篇    下一篇

UPLC-MS/MS法同时测定毛发中21种依托咪酯类成分及依托咪酯酸

韩兴1(), 李堪1, 刘昕1, 刘超1, 施月森1, 胡庆坤1, 杜明荦1, 钱振华2, 王小波1(), 郑珲2()   

  1. 1.广东省毒品实验技术中心 国家毒品实验室广东分中心 广东省精神活性物质监测与安全重点实验室，广东 广州 510230
    2.公安部禁毒情报技术中心 毒品监测管控与禁毒关键技术公安部重点实验室，北京 100193
  • 收稿日期:2026-02-24 发布日期:2026-10-28 出版日期:2026-08-25
  • 通讯作者: 王小波,郑珲
  • 作者简介:韩兴（1995—），男，硕士，主要从事理化检验研究；E-mail：cpuhanxing@163.com
  • 基金资助:
    国家重点研发计划资助项目(2024YFC3306601);国家重点研发计划资助项目(2024YFC3306603);公安部科技计划资助项目(2023JSM07)

Simultaneous Determination of 21 Etomidate Analogues and Etomidate Acid in Hair by UPLC-MS/MS

Xing Han1(), Kan Li1, Xin Liu1, Chao Liu1, Yuesen Shi1, Qingkun Hu1, Mingluo Du1, Zhenhua Qian2, Xiaobo Wang1(), Hui Zheng2()   

  1. 1.Anti-drug Technology Center of Guangdong Province, National Anti-drug Laboratory Guangdong Regional Center, Guangdong Provincial Key Laboratory of Psychoactive Substances Monitoring and Safety, Guangzhou 510230, China
    2.Key Laboratory of Drug Monitoring and Control, Drug Intelligence and Forensic Center, Ministry of Public Security, Beijing 100193, China
  • Received:2026-02-24 Online:2026-10-28 Published:2026-08-25
  • Contact: Xiaobo Wang, Hui Zheng

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摘要：

目的 建立毛发中21种依托咪酯类成分及依托咪酯酸的定性定量分析方法，探讨其在实际案件中的应用价值。 方法 毛发样本经冷冻湿法研磨提取，上清液经0.22 µm有机滤膜过滤，色谱柱选用Kinetex® Biphenyl（100 mm×2.1 mm，1.7 μm），流动相为5 mmol/L乙酸铵水溶液和甲醇，在15 min内进行梯度洗脱，UPLC-MS/MS法使用电喷雾离子源在正离子模式下采集数据，并进行方法学验证。 结果 毛发中21种依托咪酯类成分及依托咪酯酸的分离度较好，特别是3组同分异构体中的8个化合物［丙帕酯与异丙帕酯，丁托咪酯、仲丁咪酯、异丁咪酯与叔丁咪酯，1-甲氧羰基-2-甲基丙-2-基1-（1-苯乙基）-1H-咪唑-5-羧酸酯与1-甲氧羰基-2-甲基丙基1-（1-苯乙基）-1H-咪唑-5-羧酸酯］均得到有效分离，检出限为0.005~0.020 ng/mg，以0.05 ng/mg为定量下限，在定量线性范围内线性关系良好（r>0.999）。所建立方法的选择性、准确度与精密度均达到验证要求，基质效应、提取回收率在不同质量分数水平下重现性良好，处理后毛发样品在4 ℃下存放36 h定量结果稳定。实践应用结果表明，可在滥用者毛发中检出依托咪酯、美托咪酯、异丙帕酯、仲丁咪酯、异丁咪酯、三氟乙咪酯、甲氧羰基环丙咪酯及代谢物依托咪酯酸，但依托咪酯酸含量较低。 结论 本研究建立的方法操作简便、定量准确，可同时测定毛发中依托咪酯酸、已列管的13种依托咪酯类物质及尚未列管的8种潜在衍生物，涵盖酯侧链、苯环及咪唑环等位点的烷基、烷氧基、烷氧羰基、卤素及巯基取代类型，能够为打击依托咪酯类物质滥用提供技术支持。

关键词: 法医学, 毒物分析, 依托咪酯, 依托咪酯酸, 超高效液相色谱-串联质谱法, 毛发

Abstract:

Objective To establish a qualitative and quantitative analytical method for the determination of 21 etomidate analogues and etomidate acid in hair and to investigate its application value in actual forensic cases. Methods Hair samples were extracted following cryogenic wet grinding. The supernatant was filtered through a 0.22 μm organic membrane filter. The Kinetex® Biphenyl （100 mm×2.1 mm, 1.7 μm） column was used, and gradient elution was performed with methanol and 5 mmol/L ammonium acetate within 15 minutes. The data acquisition was acquired by UPLC-MS/MS with electrospray ionization in positive ion mode, followed by method verification. Results The 21 etomidate analogues and etomidate acid exhibited good chromatographic separation in hair samples. In particular, all eight compounds within three distinct groups of isomers, including propoxate and isopropoxate; butomidate, sec-butomidate, iso-butomidate and tert-butomidate; 1-（methoxycarbonyl）-2-methylpropan-2-yl 1-（1-phenylethyl）-1H-imidazole-5-carboxylate and 1-（methoxycarbonyl）-2-methylpropanyl 1-（1-phenylethyl）-1H-imidazole-5- carboxylate, were effectively separated. The method showed a good linear relationship in the quantitative linear range （r>0.999）， with the limits of detection （LOD） ranging from 0.005 to 0.020 ng/mg and the lower limit of quantification （LLOQ） of 0.05 ng/mg. The selectivity， accuracy and precision of the established method met the verification standards. The matrix effects and extraction recoveries showed good reproducibility at different concentration levels， and the quantitative results for processed hair samples remained stable after storage at 4 ℃ for 36 hours. Practical application results showed that etomidate, metomidate, isopropoxate, sec-butomidate, iso-butomidate, TF-etomidate, and ABP-700, and the metabolite etomidate acid could be detected in the hair of abusers, although the content of etomidate acid was relatively low. Conclusion The method established in this study is simple to perform and provides accurate quantification. It enables the simultaneous determination of etomidate acid, 13 scheduled etomidate analogues, and 8 unscheduled potential derivatives in hair. The analytical scope encompasses alkyl, alkoxy, alkoxycarbonyl, halogen, and sulfhydryl substitutions distributed across the ester side chain, benzene ring, and imidazole ring. It can provide technical support for combating the abuse of etomidate analogue substances.

Key words: forensic medicine, toxicological analysis, etomidate, etomidate acid, ultra-high performance liquid chromatography-tandem mass spectrometry （UPLC-MS/MS）, hair

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