色谱

色谱 ›› 2018, Vol. 36 ›› Issue (3): 268-277.DOI: 10.3724/SP.J.1123.2017.11034

• 研究论文 • 上一篇    下一篇

高效液相色谱-离子阱/飞行时间质谱鉴定违禁药品邻氯苯基环戊酮中杂质及其标准物质的制备

马晓萌1, 靳兰1, 李雅宁1, 郑珲2, 魏芸1   

  1. 1. 北京化工大学理学院, 化工资源有效利用国家重点实验室, 北京 100029;
    2. 公安部物证鉴定中心毒品检验技术处, 北京 100038
  • 收稿日期:2017-11-21 出版日期:2018-03-08 发布日期:2018-04-04
  • 通讯作者: 魏芸,Tel&Fax:+86-10-64442928,E-mail:weiyun@mail.buct.edu.cn
  • 基金资助:

    National Key Research and Development Program of China (No. 2017YFF0207800); National Natural Science Foundation of China (No. 21075007); Program for New Century Excellent Talents in University (No. NCET-11-0563); Beijing Nova Program Interdisciplinary Cooperation Project (No. Z161100004916045).

Identification of the impurities in o-chlorophenyl cyclopentyl ketone samples by high performance liquid chromatography-hybrid ion trap/time-of-flight mass spectrometry and preparation of o-chlorophenyl cyclopentyl ketone standard

MA Xiaomeng1, JIN Lan1, LI Yaning1, ZHENG Hui2, WEI Yun1   

  1. 1. State Key Laboratory of Chemical Resource Engineering, Faculty of Sciences, Beijing University of Chemical Technology, Beijing 100029, China;
    2. Drug Detection Division, Institute of Forensic Science, Ministry of Public Security, Beijing 100038, China
  • Received:2017-11-21 Online:2018-03-08 Published:2018-04-04
  • Supported by:

    National Key Research and Development Program of China (No. 2017YFF0207800); National Natural Science Foundation of China (No. 21075007); Program for New Century Excellent Talents in University (No. NCET-11-0563); Beijing Nova Program Interdisciplinary Cooperation Project (No. Z161100004916045).

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摘要：

建立了高效液相色谱-离子阱/飞行时间质谱（HPLC-IT/TOF MS）分析违禁药品邻氯苯基环戊酮样品中杂质成分的方法。对邻氯苯基环戊酮标准品进行多级质谱分析，根据各碎片离子的精确质量数推测邻氯苯基环戊酮的裂解路径，并利用该方法检测出邻氯苯基环戊酮样品中的2种杂质成分：2-氯苯甲酸酸酐和1，2-二邻氯苯甲酰基环戊烯，推断出该违禁药品的合成方法，为追溯其来源提供了重要依据。同时建立了制备邻氯苯基环戊酮标准品的方法，制备高效液相色谱条件是流动相甲醇-水（85∶15，v/v），流速8 mL/min，进样量1 mL。制备得到的邻氯苯基环戊酮标准物质纯度为99.53%。该方法简单、高效，可拓展应用于其他违禁药物标准物质的制备。

关键词: 标准物质, 高效液相色谱-离子阱/飞行时间质谱, 邻氯苯基环戊酮, 杂质鉴定, 制备高效液相色谱

Abstract:

A method for the identification of relevant impurities in illegal o-chlorophenyl cyclopentyl ketone drug was developed. Identification of impurities could help regulation of this illegal drug and allow the sources of samples of the drug to be identified. An efficient and effective method for qualitatively analyzing samples using high performance liquid chromatography-hybrid ion trap/time-of-flight mass spectrometry (HPLC-IT/TOF MS) was developed. The o-chlorophenyl cyclopentyl ketone fragmentation pathway during HPLC-MSn was determined by analyzing a standard by HPLC-IT/TOF MS. The optimized HPLC-IT/TOF MS method allowed two impurities in o-chlorophenyl cyclopentyl ketone samples to be identified. According to the exact mass data of MSn and the element composition analysis, two impurities were identified as o-chlorobenzoic acid anhydride and 1,2-di-o-chlorobenzoylcyclopentene. The synthetic route of the o-chlorophenyl cyclopentyl ketone samples was proposed by analysis of these impurities. The established method made it easy to identify impurities and find the source of this illegal drug. A method for the preparation an o-chlorophenyl cyclopentyl ketone reference standard from actual samples using preparative HPLC was also developed. The mobile phase was methanol-water (85:15, v/v) and flow rate was 8 mL/min. The purity of the obtained standards, determined by analytical HPLC, was 99.53%. This method is simple, efficient, and can be used for the preparation of other illegal drugs.

Key words: o-chlorophenyl cyclopentyl ketone, high performance liquid chromatography-hybrid ion trap/time-of-flight mass spectrometry (HPLC-IT/TOF MS), impurity identification, preparative high performance liquid chromatography, standards

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