Drug Analysis Laboratory, Forensic Science Division, Supreme Prosecutors' Office, Seoul, Republic of Korea.
Forensic Sci Int. 2010 Mar 20;196(1-3):43-50. doi: 10.1016/j.forsciint.2009.12.045. Epub 2010 Jan 13.
A gas chromatography-mass spectrometric (GC-MS) method was developed and validated for the determination of five psychotropic phenylalkylamine derivatives (amphetamine, AP; methamphetamine, MA; 3,4-methylenedioxyamphetamine, MDA; 3,4-methylenedioxymethamphetamine, MDMA; norketamine, NKT) in human hair. Hair samples (10mg) were washed with distilled water and acetone, mechanically pulverized for 1.5 min with a bead mill, and then incubated in 1 mL of methanol under ultrasonication at 50 degrees C for 1h. The resulting solutions were evaporated to dryness, derivatized using heptafluorobutyric anhydride (HFBA) at 50 degrees C for 30 min, and analyzed by GC-MS. The linear ranges were 0.1-20.0 ng/mg for AP and MA and 0.05-20.0 ng/mg for MDA, MDMA, and NKT, with the coefficients of determination (r(2)>0.9982). The intra-day and inter-day precisions were within 11.5% and 12.8%, respectively. The intra-day and inter-day accuracies were -4.1% to 5.8% and -6.6% to 4.2%, respectively. The limits of detections (LODs) for each compound were lower than 0.028 ng/mg. The recoveries were in the range of 78.9-101.2%. Based on these results, the method proved to be effective for the rapid and simple determination of phenylalkylamine derivatives in hair specimens.
建立并验证了一种气相色谱-质谱联用（GC-MS）方法，用于测定人发中五种精神药物苯丙胺类衍生物（苯丙胺、AP；甲基苯丙胺、MA；3,4-亚甲二氧基苯丙胺、MDA；3,4-亚甲二氧基甲基苯丙胺、MDMA；去甲海洛因、NKT）。取 10mg 毛发样品，先用蒸馏水和丙酮洗涤，然后用珠磨机以 1.5min 的速度机械粉碎，接着在 50°C 下于 1mL 甲醇中超声孵育 1h。所得溶液蒸发至干，用七氟丁酰酐（HFBA）在 50°C 下衍生 30min，然后进行 GC-MS 分析。AP 和 MA 的线性范围为 0.1-20.0ng/mg，MDA、MDMA 和 NKT 的线性范围为 0.05-20.0ng/mg，相关系数（r²>0.9982）。日内和日间精密度分别在 11.5%和 12.8%以内。日内和日间准确度分别为-4.1%至 5.8%和-6.6%至 4.2%。各化合物的检出限（LOD）均低于 0.028ng/mg。回收率在 78.9%-101.2%之间。基于这些结果，该方法被证明可有效用于快速、简单地测定发样中的苯丙胺类衍生物。
