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

引用本文: 胡爽, 花镇东, 黄钰, 程芳彬, 刘耀. 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[J]. 分析化学, 2022, 50(6): 964-972. doi: 10.19756/j.issn.0253-3820.210839 shu

Citation: HU Shuang, HUA Zhen-Dong, HUANG Yu, CHENG Fang-Bin, LIU Yao. Fast Separation and Detection of Fentanyls Isomers by Ultra Performance Convergence Chromatography-Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, 2022, 50(6): 964-972. doi: 10.19756/j.issn.0253-3820.210839 shu

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

胡爽 ^1,2, ,
花镇东 ^{3,
,} ,
黄钰 ^4, ,
程芳彬 ^5, ,
刘耀 ^{1,
,}

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

通讯作者: 花镇东,E-mail:28008085@qq.com; 刘耀,E-mail:Liuyao1123@aliyun.com

基金项目:
北京市教育委员会科研计划项目（No.KM202114019001）和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 UPC² BEH色谱柱，以超临界流体CO₂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。

关键词:

English

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

HU Shuang ^1,2, ,
HUA Zhen-Dong ^{3,
,} ,
HUANG Yu ^4, ,
CHENG Fang-Bin ^5, ,
LIU Yao ^{1,
,}

1.
School of Criminal Investigation, People's Public Security University of China, Beijing 100038, China;
2.
Department of Criminal Science and Technology, Beijing Police College, Beijing 102202, China;
3.
Key Laboratory of Drug Monitoring and Control, Anti-Drug Information Technology Center of the Ministry of Public Security, Beijing 100193, China;
4.
School of Pharmacy, China Pharmaceutical University, Nanjing 210009, China;
5.
Zhongshan Public Security Bureau Criminal Detachment, Zhongshan 528403, China

Corresponding author: HUA Zhen-Dong, ; LIU Yao,

Received Date: 16 November 2021
Revised Date: 05 March 2022
Fund Project:
Supported by the Scientific Research Project of Beijing Municipal Education Commission(No. KM202114019001) and the Science and Technology to Strengthen Basic Work Project of Ministry of Public Security(No. 2020GABJC21).

Abstract: 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 CO₂ 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.

Key words:

Ultra performance convergence chromatography
/ Mass spectrometry
/ Fentanyls
/ Isomers
/ New psychoactive substances

1. [1]
  VARDANYAN R S, HRUBY V J. Future Med. Chem., 2014, 6(4):385-412.VARDANYAN R S, HRUBY V J. Future Med. Chem., 2014, 6(4):385-412.
2. [2]
  MOUNTENEY J, GIRAUDON I, DENISSOV G, GRIFFITHS P. Int. J. Drug Policy, 2015, 26(7):626-631.MOUNTENEY J, GIRAUDON I, DENISSOV G, GRIFFITHS P. Int. J. Drug Policy, 2015, 26(7):626-631.
3. [3]
  SUZUKI S. Forensic Sci. Int., 1989, 43(1):15-19.SUZUKI S. Forensic Sci. Int., 1989, 43(1):15-19.
4. [4]
  RITTGEN J, PUTZ M, ZIMMERMANN R. Electrophoresis, 2012, 33(11):1595-1605.RITTGEN J, PUTZ M, ZIMMERMANN R. Electrophoresis, 2012, 33(11):1595-1605.
5. [5]
  GILBERT N, ANTONIDES L H, SCHOFIELD C J, COSTELLO A, KILKELLY B, CAIN A R, DALZIEL P R V, HORNER K, MEWIS R E, SUTCLIFFE O B. Drug Test. Anal., 2020, 12(6):798-811.GILBERT N, ANTONIDES L H, SCHOFIELD C J, COSTELLO A, KILKELLY B, CAIN A R, DALZIEL P R V, HORNER K, MEWIS R E, SUTCLIFFE O B. Drug Test. Anal., 2020, 12(6):798-811.
6. [6]
  ROJKIEWICZ M, MAJCHRZAK M, CELINSKI R, KUS P, SAJEWICZ M. Drug Test. Anal., 2017, 9(3):405-414.ROJKIEWICZ M, MAJCHRZAK M, CELINSKI R, KUS P, SAJEWICZ M. Drug Test. Anal., 2017, 9(3):405-414.
7. [7]
  KANAMORI T, IWATA Y T, SEGAWA H, YAMAMURO T, KUWAYAMA K, TSUJIKAWA K, INOUE H. J.Forensic Sci., 2017, 62(6):1472-1478.KANAMORI T, IWATA Y T, SEGAWA H, YAMAMURO T, KUWAYAMA K, TSUJIKAWA K, INOUE H. J.Forensic Sci., 2017, 62(6):1472-1478.
8. [8]
  BUCHALTER S, MARGINEAN I, YOHANNAN J. J. Chromatogr. A, 2019, 1596:183-193.BUCHALTER S, MARGINEAN I, YOHANNAN J. J. Chromatogr. A, 2019, 1596:183-193.
9. [9]
  LURIE I S, IIO R. J. Chromatogr. A, 2009, 1216(9):1515-1519.LURIE I S, IIO R. J. Chromatogr. A, 2009, 1216(9):1515-1519.
10. [10]
  BUSARDO F P, CARLIER J, GIORGETTI R, TAGLIABRACCI A, PACIFICI R, GOTTARDI M, PICHINI S.Front. Chem., 2019, 7(2):184-197.BUSARDO F P, CARLIER J, GIORGETTI R, TAGLIABRACCI A, PACIFICI R, GOTTARDI M, PICHINI S.Front. Chem., 2019, 7(2):184-197.
11. [11]
  SALEMMILANI R, MOSKIVITS M, MEINHART C D. Analyst, 2019, 144(2):3080-3087.SALEMMILANI R, MOSKIVITS M, MEINHART C D. Analyst, 2019, 144(2):3080-3087.
12. [12]
  BERNAL J L, MARTIN M T, TORIBIO L. J. Chromatogr. A, 2013, 1313(SI):24-36.BERNAL J L, MARTIN M T, TORIBIO L. J. Chromatogr. A, 2013, 1313(SI):24-36.
13. [13]
  ZHANG Wen-Hua, XIE Wen, HOU Jian-Bo, CHEN Qin-Ke, LI Shu-Min, ZHU Ze-Long, ZOU Xue-Quan, XU Dun-Ming. Chin. J. Chromatogr., 2019, 37(12):1356-1362.张文华, 谢文, 侯建波, 陈钦可, 李淑敏, 祝泽龙, 邹学权, 徐敦明.色谱. 2019, 37(12):1356-1362.
14. [14]
  ZHOU Wei, WANG Bo, LIU Qian-Qian, YANG Sheng-Xin, WANG Li-Ting. Chin. J. Anal. Chem., 2015, 43(1):115-120.周围, 王波, 刘倩倩, 杨盛鑫, 王丽婷.分析化学, 2015, 43(1):115-120.
15. [15]
  QIU Yue, LI Gen-Rong, LONG Mei, RUAN Yan, TAN Chao-Lan, ZHANG Lu, XIA Zhi-Ning. Chin. J. Anal.Chem., 2020, 48(2):255-261.邱月, 李根容, 龙梅, 阮燕, 谭超兰, 张璐, 夏之宁.分析化学, 2020, 48(2):255-261.
16. [16]
  PAUK V, ZIHLOVA V, BOROVCOVA L, HAVLICEK V, SCHUG K, LEMR K. J. Chromatogr. A, 2015, 1423:169-176.PAUK V, ZIHLOVA V, BOROVCOVA L, HAVLICEK V, SCHUG K, LEMR K. J. Chromatogr. A, 2015, 1423:169-176.
17. [17]
  BREITENBACH S, ROWE W F, MCCORD B. J. Chromatogr. A, 2016, 1440:201-211.BREITENBACH S, ROWE W F, MCCORD B. J. Chromatogr. A, 2016, 1440:201-211.
18. [18]
  CARNES S, BRIEN S, SZEWCZAK A, TREMEAU C L, ROWE W F, MCCORD B, LURIE I S. J. Sep. Sci., 2017, 40(17):3545-3556.CARNES S, BRIEN S, SZEWCZAK A, TREMEAU C L, ROWE W F, MCCORD B, LURIE I S. J. Sep. Sci., 2017, 40(17):3545-3556.
19. [19]
  SEGAWA H, KUSAKABE K, ISHII A, KATO N, IWATA Y T, YAMAMURO T, KANAMORI T. Anal. Sci. Adv., 2020, 1(1):22-33.SEGAWA H, KUSAKABE K, ISHII A, KATO N, IWATA Y T, YAMAMURO T, KANAMORI T. Anal. Sci. Adv., 2020, 1(1):22-33.
20. [20]
  HUA Zhen-Dong, JIA Wei, LIU Cui-Mei, QIAN Zhen-Hua. Handbook of New Psychoactive Substance Analysis-Mass Spectrometry(Second Edition). Beijing:People's Public Security University of China Press, 2019:529-561.花镇东, 贾薇, 刘翠梅, 钱振华.新精神活性物质分析手册-质谱分册(第二版).北京:中国人民公安大学出版社, 2019:529-561.

扫一扫看文章

计量

PDF下载量: 3
文章访问数: 201
HTML全文浏览量: 32

通讯作者: 陈斌, bchen63@163.com

1.
沈阳化工大学材料科学与工程学院沈阳 110142

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

通讯作者: 花镇东,E-mail:28008085@qq.com; 刘耀,E-mail:Liuyao1123@aliyun.com

English

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

Corresponding author: HUA Zhen-Dong, ; LIU Yao,

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南：你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

计量

通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

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

通讯作者: 花镇东,E-mail:28008085@qq.com; 刘耀,E-mail:Liuyao1123@aliyun.com

English

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

Corresponding author: HUA Zhen-Dong, ; LIU Yao,

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

计量

文章相关

通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

CCS Chemistry：颜徐州、鲍哲南：你的皮肤可能是一片SPMs