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采用 LC-MS/MS 对同重化合物环丙基芬太尼、丁酰芬太尼、丙烯酰芬太尼和对甲基丙烯酰芬太尼进行色谱分离,以进行特异性确证。

Chromatographic separation of the isobaric compounds cyclopropylfentanyl, crotonylfentanyl, methacrylfentanyl, and para-methylacrylfentanyl for specific confirmation by LC-MS/MS.

机构信息

Center for Forensic Science Research and Education at the Fredric Rieders Family Foundation, Willow Grove, PA, USA; National Forensic Service, Wonju, Gangwon-do, South Korea.

Center for Forensic Science Research and Education at the Fredric Rieders Family Foundation, Willow Grove, PA, USA.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2019 Jun 15;1118-1119:164-170. doi: 10.1016/j.jchromb.2019.04.033. Epub 2019 Apr 25.

DOI:10.1016/j.jchromb.2019.04.033
PMID:31054450
Abstract

Cyclopropylfentanyl has been encountered by law enforcement and public health officials beginning in mid-2017 and has been associated with numerous overdoses and fatalities. The detection and identification of cyclopropylfentanyl has become more challenging with the subsequent emergence of multiple structural isomeric fentanyl species, some of which have been detected in seized drug casework. These include crotonylfentanyl, methacrylfentanyl, para-methylacrylfentanyl, and ortho-methylacrylfentanyl; all of which have the same exact mass and similar fragmentation patterns. Since these compounds may be scheduled differently and pharmacologically act differently, it is important to be able to differentiate them analytically. Our method was developed and validated for the analysis and differentiation of cyclopropylfentanyl from its isomers by liquid chromatography tandem mass spectrometry (LC-MS/MS), in order to confirm the identify of cyclopropylfentanyl in biological specimens from death investigation casework; 36 postmortem blood samples were submitted for analysis. Cyclopropylfentanyl, crotonylfentanyl, methacrylfentanyl, and para-methylacrylfentanyl were successfully resolved using a 13-minute run time and a simple gradient elution. Ortho-methacrylfentanyl was resolved only in a 20-minute chromatographic run. The assay met validation performance characteristics, with an analytical range of 1-100 ng/mL and limits of detection of 0.1 ng/mL for all analytes. Analysis of commonly encountered substances showed no interferences. All samples previously reported positive for cyclopropylfentanyl were confirmed positive for cyclopropylfentanyl in the absence of its isomers. To our knowledge to date, no positive toxicological specimens have been encountered for any cyclopropylfentanyl isomers.

摘要

环丙基芬太尼于 2017 年年中开始被执法部门和公共卫生官员发现,并与许多过量用药和死亡事件有关。随着随后出现的多种结构异构的芬太尼物质,包括丁酰芬太尼、甲基丙烯酰芬太尼、对甲基丙烯酰芬太尼和邻甲基丙烯酰芬太尼,检测和识别环丙基芬太尼变得更加具有挑战性,其中一些已在缉获的毒品案件中被检测到。这些化合物的分子量相同,碎片化模式也相似。由于这些化合物可能受到不同的管制,且在药理学上有不同的作用,因此能够对它们进行分析上的区分非常重要。我们的方法是通过液相色谱串联质谱法(LC-MS/MS)开发和验证的,用于分析和区分环丙基芬太尼与其异构体,以确认法医调查案件中生物样本中环丙基芬太尼的身份;共提交了 36 份死后血液样本进行分析。通过 13 分钟的运行时间和简单的梯度洗脱,成功地将环丙基芬太尼、丁酰芬太尼、甲基丙烯酰芬太尼和对甲基丙烯酰芬太尼分离开来。邻甲基丙烯酰芬太尼仅在 20 分钟的色谱运行中被分离开来。该测定符合验证性能特征,分析范围为 1-100ng/mL,所有分析物的检测限为 0.1ng/mL。对常见物质的分析表明没有干扰。所有以前报告为环丙基芬太尼阳性的样本在没有其异构体的情况下均被确认为环丙基芬太尼阳性。据我们所知,迄今为止,尚未遇到任何环丙基芬太尼异构体的阳性毒理学样本。

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