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目的建立准确可靠的甲基苯丙胺(即冰毒,MA)初筛阳性样本的确证分析方法,排除由于服用药物而产生的假阳性结果。方法在样品前处理中选用环己烷萃取临床样本中的MA,采用七氟丁酸酐对萃取出的MA进行衍生化,结合串联四级杆气相色谱质谱联用法(GC-MS/MS)开发的多反应检测(MRM)方法对样本进行确证分析。结果在MA确证分析中前处理采用衍生化处理后的检测结果不论在峰型、峰高、检测限、灵敏度、定量线性范围方面均优于未进行衍生化处理的结果,不同的衍生化试剂中选用七氟丁酸酐衍生的结果最好。结论本研究建立的GC-MS/MS分析方法对于毒品确证十分准确、有效,可推广应用于其他毒品初筛为阳性的样本进行进一步的确证。
Objective To establish an accurate and reliable method for confirmatory analysis of positive samples of methamphetamine (MA, MA), and to exclude false positive results from taking the drug. Methods In the sample preparation, cyclohexane was used to extract MA from clinical samples, and the extracted MA was derivatized with heptafluorobutyric anhydride. The GC was developed by GC-MS / MS Multiple reaction detection (MRM) method for confirmatory analysis of the sample. Results In the MA confirmatory analysis, the results of the pretreatment with derivatization were better than those without derivatization in terms of peak shape, peak height, limit of detection, sensitivity and quantitative linearity. Among the different derivatization reagents Sephacryl anhydride derived the best choice. Conclusion The GC-MS / MS analysis method established in this study is very accurate and effective for drug confirmation. It can be extended to other positive samples for further confirmation.