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236.12889,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。
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 SKF525 Aand 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.
作者
王跨陡
曹芳琦
江雪
陈红
袁晓亮
陈永生
胡钧健
WANG Kua-dou;CAO Fang-qi;JIANG Xue;CHEN Hong;YUAN Xiao-liang;CHEN Yong-sheng;HU Jun-jian(Shanghai Key Laboratory of Crime Scene Evidence,Institute of Forensic Science,Shanghai Public Security Bureau,Shanghai 200083,China;Shanghai Key Laboratory of Crime Scene Evidence,Shanghai Research Institute of Criminal Science and Technology,Shanghai 200083,China)
出处
《法医学杂志》
CAS
CSCD
2019年第6期682-686,共5页
Journal of Forensic Medicine
基金
上海市公安局科学技术发展基金资助项目(2016009,2016002,2018003)