Kim Jin Young, Jung Kyu Sung, Kim Min Kyoung, Lee Jae Il, In Moon Kyo
Drug Analysis Laboratory, Forensic Science Division, Supreme Prosecutors' Office, Seocho-ggu, Seoul, Korea.
Rapid Commun Mass Spectrom. 2007;21(11):1705-20. doi: 10.1002/rcm.3010.
A gas chromatography/mass spectrometric (GC/MS) method was developed and validated for the determination of thirteen psychotropic phenylalkylamine derivatives (amphetamine; AP, phentermine; PT, methamphamine; MA, cathinone; Khat, methcathinone; MCAT, fenfluramine; FFA, desmethylselegiline; DSEL, 3,4-methylenedioxyamphetamine; MDA, 3,4-methylenedioxymethamphetamine; MDMA, 3,4-methylenedioxyethylamphetamine; MDEA, norketamine; NKT, mescaline; MES, 4-bromo-2,5-dimethoxyphenethylamine; 2CB) in human hair. Hair samples (20 mg) were washed with distilled water and acetone, cut into small fragments (<1 mm), and incubated in 0.25 M methanolic HCl under ultrasonication at 50 degrees C for 1 h. The resulting solutions were evaporated to dryness, derivatized using trifluoroacetic anhydride (TFAA) at 70 degrees C for 30 min, and analyzed by GC/MS. The linear ranges were 0.02-25.0 ng/mg for AP, PT, Khat, FFA, DSEL, MDMA, and 2CB; 0.05-25.0 ng/mg for MA, MCAT, and MES; 0.05-12.5 ng/mg for MDA; and 0.1-25.0 ng/mg for MDEA and NKT, with good correlation coefficients (r(2) > 0.9985). The intra-day, inter-day, and inter-person precisions were within 12.7%, 14.8%, and 16.8%, respectively. The intra-day, inter-day, and inter-person accuracies were between -10.7 and 13.4%, -12.7 and 11.6%, and -15.3 and 11.9%, respectively. The limits of quantifications (LOQs) for each compound were lower than 0.08 ng/mg. The recoveries were in the range of 76.7-95.6%. The method proved to be suitable for the simultaneous qualification and quantification of phenylalkylamine derivatives in hair specimens.
建立并验证了一种气相色谱/质谱（GC/MS）方法，用于测定人发中13种精神活性苯烷基胺衍生物（苯丙胺；AP，芬特明；PT，甲基苯丙胺；MA，卡西酮；卡塔叶，甲卡西酮；MCAT，芬氟拉明；FFA，去甲基司来吉兰；DSEL，3,4-亚甲基二氧基苯丙胺；MDA，3,4-亚甲基二氧基甲基苯丙胺；MDMA，3,4-亚甲基二氧基乙基苯丙胺；MDEA，去甲氯胺酮；NKT，三甲氧苯乙胺；MES，4-溴-2,5-二甲氧基苯乙胺；2CB）。头发样本（20毫克）先用蒸馏水和丙酮洗涤，切成小碎片（<1毫米），然后在50℃超声条件下于0.25M甲醇盐酸中孵育1小时。所得溶液蒸发至干，在70℃下用三氟乙酸酐（TFAA）衍生化30分钟，然后用GC/MS分析。AP、PT、卡塔叶、FFA、DSEL、MDMA和2CB的线性范围为0.02 - 25.0 ng/mg；MA、MCAT和MES的线性范围为0.05 - 25.0 ng/mg；MDA的线性范围为0.05 - 12.5 ng/mg；MDEA和NKT的线性范围为0.1 - 25.0 ng/mg，相关系数良好（r(2)>0.9985）。日内、日间和人与人之间的精密度分别在12.7%、14.8%和16.8%以内。日内、日间和人与人之间的准确度分别在-10.7%至13.4%、-12.7%至11.6%和-15.3%至11.9%之间。每种化合物的定量限（LOQ）低于0.08 ng/mg。回收率在76.7% - 95.6%范围内。该方法被证明适用于同时对头发样本中的苯烷基胺衍生物进行定性和定量。
