Marginean Ioan, Rowe Walter F, Lurie Ira S
Department of Forensic Sciences, The George Washington University, 2100 Foxhall Road, NW, Somers Hall, Washington, DC 20007, United States.
Department of Forensic Sciences, The George Washington University, 2100 Foxhall Road, NW, Somers Hall, Washington, DC 20007, United States.
Forensic Sci Int. 2015 Apr;249:83-91. doi: 10.1016/j.forsciint.2015.01.013. Epub 2015 Jan 28.
Separation and mass spectrometric techniques are integral parts of forensic drug analysis for both screening and confirmation. The Scientific Working Group for the Analysis of Seized Drugs (SWGDRUG), which is responsible for setting standards for drug analysis, requires for drug identification a Category A test such as mass spectrometry with an additional test from either Category B or C. If a Category A method is not used at least two uncorrelated tests from Category B must be included, for which separation techniques such as gas chromatography and liquid chromatography would qualify. The utility and validity of using ultra high performance liquid chromatography (UHPLC) and time-of-flight (TOF) mass spectrometry (MS) for the analysis of synthetic cannabinoids is presented. The separation of 32 solutes, including 23 controlled substances and nine non-controlled positional isomers of JWH-018, are compared using UHPLC with TOF detection and capillary GC with electron ionization (EI). For these solutes, the reversed phase UHPLC separation on three different 2.1 mm × 150 mm × 2.7 μm superficially porous (SPP) columns (C18, Phenyl-Hexyl and Dimethylpentafluorophenylpropyl (PFP)) compared favorably with the capillary gas chromatography (GC) separation using an Elite-5MS column 0.25 mm × 30 m × 0.25 μm. Principal component analysis revealed that all three UHPLC separations for the separation of the controlled substances are orthogonal to the capillary GC separation. It was also revealed by principal component analysis that the separation of JWH-018 and the nine non-controlled positional isomers for the various techniques were significantly more correlated than the separation of the controlled substances. Although most of the controlled synthetic cannabinoids gave unique TOF in-source collision-induced dissociation MS spectra and EI spectra, it was not possible to discriminate among the geometric isomers (CP47, 497, Epi CP47, 497; Cp47, 497 C8 homologue, Epi CP47, 497 C8 homologue). JWH-018 could be distinguished from the non-controlled isomers based on its EI spectra. In contrast, several of the non-controlled JWH-018 isomers give identical TOF in-source collision-induced dissociation MS spectra to JWH-018.
分离和质谱技术是法医毒品分析筛查和确证环节不可或缺的部分。负责制定毒品分析标准的缉获毒品分析科学工作组（SWGDRUG）要求，毒品鉴定需采用A类检测方法，如质谱法，并辅以B类或C类中的一项附加检测。若未使用A类方法，则必须包含至少两项不相关的B类检测，气相色谱和液相色谱等分离技术符合此类要求。本文介绍了使用超高效液相色谱（UHPLC）和飞行时间（TOF）质谱（MS）分析合成大麻素的实用性和有效性。采用UHPLC与TOF检测联用以及毛细管气相色谱（GC）与电子电离（EI）联用的方法，对32种溶质进行分离，其中包括23种管制物质和JWH - 018的9种非管制位置异构体。对于这些溶质，在三根不同的2.1 mm×150 mm×2.7μm表面多孔（SPP）柱（C18、苯基己基和二甲基五氟苯基丙基（PFP））上进行的反相UHPLC分离，与使用0.25 mm×30 m×0.25μm的Elite - 5MS柱进行的毛细管气相色谱（GC）分离相比，效果良好。主成分分析表明，所有三种用于分离管制物质的UHPLC分离方法与毛细管GC分离方法相互正交。主成分分析还表明，各种技术对JWH - 018及其9种非管制位置异构体的分离相关性，明显高于对管制物质的分离相关性。尽管大多数管制合成大麻素在TOF源内碰撞诱导解离质谱图和EI质谱图中呈现独特特征，但无法区分几何异构体（CP47,497、表型CP47,497；Cp47,497 C8同系物、表型CP47,497 C8同系物）。基于EI质谱图，JWH - 018可与非管制异构体区分开来。相比之下，几种非管制的JWH - 018异构体在TOF源内碰撞诱导解离质谱图中与JWH - 018相同。
