超高效合相色谱-质谱技术对芬太尼类物质异构体的快速分离和检测  

Fast Separation and Detection of Fentanyls Isomers by Ultra Performance Convergence Chromatography-Mass Spectrometry

作　　者：胡爽[1,2] 花镇东 黄钰 程芳彬 刘耀 HU Shuang;HUA Zhen-Dong;HUANG Yu;CHENG Fang-Bin;LIU Yao(School of Criminal Investigation,People’s Public Security University of China,Beijing 100038,China;Department of Criminal Science and Technology,Beijing Police College,Beijing 102202,China;Key Laboratory of Drug Monitoring and Control,Anti-Drug Information Technology Center of the Ministry of Public Security,Beijing 100193,China;School of Pharmacy,China Pharmaceutical University,Nanjing 210009,China;Zhongshan Public Security Bureau Criminal Detachment,Zhongshan 528403,China)

机构地区：[1]中国人民公安大学侦查学院,北京100038 [2]北京警察学院刑事科学技术系,北京102202 [3]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 [4]中国药科大学药学院,南京210009 [5]中山市公安局刑事警察支队,中山528403

出　　处：《分析化学》2022年第6期964-972,共9页Chinese Journal of Analytical Chemistry

基　　金：北京市教育委员会科研计划项目(No.KM202114019001);公安部科技强警基础工作专项项目(No.2020GABJC21)资助。

摘　　要：芬太尼类物质作为一类新型精神活性物质,具有种类繁多、更新换代迅速、结构极其相似等特点,对其同分异构体进行准确定性分析是当前毒品分析工作面临的难题。超高效合相色谱法是实现同分异构体高效分离的有力手段,基于此,本研究建立了超高效合相色谱-质谱技术快速分离和检测芬太尼类物质的分析方法,对分离过程中色谱柱、改性剂、柱温等条件进行了优化。在最优条件下,采用Waters ACQUITY UPC2BEH色谱柱,以超临界流体CO;为主要流动相、含20 mmol/L甲酸铵的甲醇为改性剂,在柱温50℃下进行梯度洗脱,使用Xevo TQD三重四极杆质谱进行检测,6.5 min内即可实现13种芬太尼类物质的有效分离,所有同分异构体的分离度均大于1.5,并且色谱峰对称性良好。方法的检出限为0.01~0.05 ng/mL,保留时间的相对标准偏差均小于0.6%,9种常见毒品对13种目标物的测定没有干扰。与常规的超高效液相色谱-质谱检测方法相比,本方法在异构体分离方面具有显著优势,可满足当前公安禁毒部门对于芬太尼类物质准确定性分析的需要。As a new class of psychoactive substances, fentanyls have the characteristics of wide variety,rapid replacement and extremely similar structures. The accurate identification of their isomers is a major problem faced by drug analysts. Ultra performance convergence chromatography is a powerful tool to achieve efficient separation of isomers. Therefore, a new method was established for fast separation and detection of fentanyls by ultra performance convergence chromatography-mass spectrometry in this work. The separation conditions of the chromatographic column, modifiers and column temperature were optimized. The separation and detection was conducted on Waters ACQUITY UPC2 BEH column with supercritical fluid CO;as primary mobile phase, methanol containing 20 mmol/L ammonium formate as the modifier, column temperature at 50 ℃ and a Xevo TQD triple quadrupole as mass spectrometer. A total of 13 kinds of fentanyls were completely separated within 6.5 min with an above 1.5-resolution to all the isomers. The chromatographic peaks were perfectly symmetric. Methodological statistics showed that, 9 kinds of common drugs did not interfere with the determination of 13 kinds of target substances;the detection limits were 0.01–0.05 ng/mL and the relative standard deviations of the retention time were less than 0.6%. Compared with the conventional ultra-high performance liquid chromatography-mass spectrometry detection method, this method had significant advantages in the separation of isomers,which fully met the anti-drug public security departments’ needs for the accurate identification of fentanyls.

关 键 词：超高效合相色谱 质谱 芬太尼类 异构体 新精神活性物质 

分 类 号：O657.63[理学—分析化学] D918.9[理学—化学]