Morello David R, Cooper Sam D, Panicker Sini, Casale John F
U.S. Drug Enforcement Administration, Special Testing and Research Laboratory, Dulles, VA 20166-9509, USA.
J Forensic Sci. 2010 Jan;55(1):42-9. doi: 10.1111/j.1556-4029.2009.01220.x. Epub 2009 Nov 30.
The illicit manufacture of heroin results in the formation of trace level acidic and neutral impurities. These impurities are detectable in illicit heroin and provide valuable information about the manufacturing process used. The isolation, derivatization, and semiquantitative analysis of neutral and acidic heroin manufacturing impurities by programmed temperature vaporizing injector-gas chromatography-mass spectrometry (PTV-GC-MS) is described. Trace acidic and neutral heroin impurities were isolated from basic fractions using liquid-liquid extraction. Extracted impurities were treated with N-Methyl-N-trimethylsilyltrifluoroacetamide followed by PTV-GC-MS analyses. Semiquantitative data were obtained using full scan mass spectrometry utilizing unique ions or ion combinations for 36 trace impurities found in crude and/or highly refined heroin samples. Minimum detection limits for acidic and neutral impurities were estimated to be at the 10(-7) level relative to total morphine. Over 500 authentic heroin samples from South America, Mexico, Southwest Asia, and Southeast Asia were analyzed. Classification of illicit heroin based on the presence or absence and relative amounts of acidic and neutral impurities is presented.
海洛因的非法制造会产生痕量水平的酸性和中性杂质。这些杂质在非法海洛因中可被检测到，并能提供有关所使用制造过程的宝贵信息。本文描述了通过程序升温汽化进样器-气相色谱-质谱联用仪（PTV-GC-MS）对海洛因制造过程中的中性和酸性杂质进行分离、衍生化及半定量分析的方法。痕量酸性和中性海洛因杂质通过液-液萃取从碱性馏分中分离出来。萃取后的杂质用N-甲基-N-三甲基硅烷基三氟乙酰胺处理，然后进行PTV-GC-MS分析。利用全扫描质谱法，针对粗制和/或高度精制海洛因样品中发现的36种痕量杂质，使用独特的离子或离子组合获取半定量数据。酸性和中性杂质的最低检测限估计相对于总吗啡为10^(-7)水平。对来自南美洲、墨西哥、西南亚和东南亚的500多个纯正海洛因样品进行了分析。文中给出了基于酸性和中性杂质的存在与否及相对含量对非法海洛因进行分类的结果。
