法医学杂志

法医学杂志 ›› 2019, Vol. 35 ›› Issue (6): 682-686.DOI: 10.12116/j.issn.1004-5619.2019.06.007

• 论著 • 上一篇    下一篇

新精神活性物质Dibutylone的鉴定

王跨陡1， 曹芳琦2， 江雪2， 陈红2， 袁晓亮2， 陈永生1， 胡钧健2   

  1. 1. 上海市公安局物证鉴定中心 上海市现场物证重点实验室，上海 200083； 2. 上海市刑事科学技术研究院 上海市现场物证重点实验室，上海 200083
  • 发布日期:2019-12-25 出版日期:2019-12-28
  • 通讯作者: 曹芳琦，女，硕士，副研究员，主要从事毒品、毒物分析与快速检测研究；E-mail：frankie-cao@163.com
  • 作者简介:王跨陡（1970—），男，副主任法医师，主要从事毒品、毒物分析检测研究；E-mail：wangkd001@163.com
  • 基金资助:
    上海市公安局科学技术发展基金资助项目（2016009，2016002，2018003）

Identification of the New Psychoactive Substance Dibutylone#br#

WANG Kua-dou1, CAO Fang-qi2, JIANG Xue2, CHEN Hong2, YUAN Xiao-liang2, CHEN Yong-sheng1, HU Jun-jian2   

  1. 1. Shanghai Key Laboratory of Crime Scene Evidence, Institute of Forensic Science, Shanghai Public Security Bureau, Shanghai 200083, China; 2. Shanghai Key Laboratory of Crime Scene Evidence, Shanghai Research Institute of Criminal Science and Technology, Shanghai 200083, China
  • Online:2019-12-25 Published:2019-12-28

PDF (PC)

668

摘要： 目的 建立基于气相色谱-质谱（gas chromatography-mass spectrometry，GC-MS）、高分辨质谱和核磁共振波谱技术联合鉴定未知样品的方法。 方法 样品用含内标盐酸双苯戊二氨酯（SKF525A）的甲醇溶液溶解后，采用GC-MS和高分辨质谱检测。混合样品经硅胶柱层析分离纯化后，用氘代甲醇溶液溶解进行核磁共振氢谱（1H nuclear magnetic resonance spectroscopy，1H NMR）的结构解析。 结果 GC-MS检测获得样品中主要组分的质谱特征碎片离子m/z为86.1（基峰）、71.2、121.1、149.0，高分辨质谱实测分子离子峰的精确质量数为236.128 89，经数据分析再结合数据库比对在未知样品中检索出卡西酮类新精神活性物质1-[3，4-（亚甲二氧基）苯基]-2-二甲氨基-1-丁酮（Dibutylone），另外未知样品中还含有少量咖啡因。样品纯化后经1H NMR鉴定，进一步确证为Dibutylone。此外，样品中主要组分的GC-MS保留时间和特征碎片离子与Dibutylone对照品一致。 结论 本研究建立的方法可用于混合样品中Dibutylone的鉴定。

关键词: 法医毒理学, 气相色谱-质谱法, 高分辨质谱, 核磁共振波谱法, 1-[3, 4-（亚甲二氧基）苯基]-2-二甲氨基-1-丁酮

Abstract: Objective To establish a method to identify unknown samples based on combined use of gas chromatography-mass spectrometry （GC-MS）, high resolution mass spectrometry （HRMS） and nuclear magnetic resonance spectrum （NMR） technique. Methods The unknown samples were dissolved in methanol solution containing internal standard SKF525A and detected by GC-MS and HRMS. The mixed samples were separated and purified by silica gel column chromatography, and then dissolved in methanol-d4 solution for structural analysis of 1H nuclear magnetic resonance spectroscopy （1H NMR）. Results The characteristic fragment ions （m/z） were 86.1 （base peak）, 71.2, 121.1, and 149.0, and the accurate mass number of molecular ion peak was measured by HRMS to be 236.128 89. By combined use of data analysis and database comparison, a new psychoactive substance of the cathinone class, Dibutylone, was detected in the sample, and the sample also contained a small amount of caffeine. The sample was purified, then identified using 1H NMR, and was further confirmed to be Dibutylone. In addition, the GC-MS retention time and characteristic fragment ions of the main components of the sample were consistent with those of Dibutylone reference material. Conclusion The method established in this study can be used for the identification of Dibutylone in mixed samples.

Key words: forensic toxicology, gas chromatography-mass spectrometry, high resolution mass spectrometry, nuclear magnetic resonance spectroscopy, 1-（3,4-methylenedioxyphenyl）-2-（dimethylamino）butan-1-one （Dibutylone）