Hornbeck C L, Czarny R J
Navy Drug Screening Laboratory, San Diego, California 92134.
J Anal Toxicol. 1989 May-Jun;13(3):144-9. doi: 10.1093/jat/13.3.144.
A urine assay for methamphetamine and amphetamine that is compatible with our existing high-volume GC/MS assays for other drugs of abuse has been developed. Trichloroacetic anhydride is used for derivatization and its derivative is substantially less volatile than other commonly used derivatives. The internal standard is the primary amine 2-methylphenethylamine. The procedure utilizes an initial liquid-liquid extraction, a liquid-liquid back extraction for specimen cleanup, and derivatization for removal of excess trichloroacetic anhydride and acid by-product. A GC temperature of about 180 degrees C results in retention times of approximately 2.8, 3.2, and 4.3 min for amphetamine, the internal standard, and methamphetamine, respectively. Five ions are monitored: 91+, 118+, 188+ for amphetamine; 105+, 118+ for 2-methylphenethylamine; and 91+, 118+, 202+ for methamphetamine. Full scan GC/MS data from a variety of other derivatives are examined and used to illustrate the advantages of derivatizing molecules with strongly electronegative atoms near the reaction site. This situation forces fragmentation patterns in which positive charges are located on larger and structurally acceptable identifying mass fragments of the original methamphetamine or amphetamine molecule.
已开发出一种用于检测甲基苯丙胺和苯丙胺的尿液检测方法，该方法与我们现有的用于检测其他滥用药物的高容量气相色谱/质谱检测方法兼容。三氯乙酸酐用于衍生化，其衍生物的挥发性远低于其他常用衍生物。内标是伯胺2-甲基苯乙胺。该程序首先进行液-液萃取，然后进行液-液反萃取以净化样品，并进行衍生化以去除过量的三氯乙酸酐和酸性副产物。气相色谱温度约为180℃时，苯丙胺、内标和甲基苯丙胺的保留时间分别约为2.8、3.2和4.3分钟。监测五个离子：苯丙胺的91+、118+、188+；2-甲基苯乙胺的105+、118+；甲基苯丙胺的91+、118+、202+。对来自各种其他衍生物的全扫描气相色谱/质谱数据进行了检查，并用于说明在反应位点附近用强电负性原子衍生化分子的优势。这种情况会导致碎片模式，其中正电荷位于原始甲基苯丙胺或苯丙胺分子的更大且结构上可接受的识别质量碎片上。
