Nakamura Shinichi, Tomita Mamoru, Wada Mitsuhiro, Chung Heesun, Kuroda Naotaka, Nakashima Kenichiro
Department of Clinical Pharmacy, Course of Pharmaceutical Sciences, Graduate School of Biomedical Sciences, Nagasaki University, Japan.
Biomed Chromatogr. 2006 Jun-Jul;20(6-7):622-7. doi: 10.1002/bmc.670.
A sensitive semi-micro column high-performance liquid chromatography with fluorescence detection method was developed for the determination of 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylenedioxyamphetamine (MDA), methamphetamine (MP) and amphetamine (AP) in human hair. 4-(4,5-Diphenyl-1H-imidazol-2-yl)benzoyl chloride (DIB-Cl) and 1-methyl-3-phenylpropylamine were used as labeling reagent and internal standard, respectively. These drugs were extracted from hair into 5% trifluoroacetic acid in methanol, and fluorescent labeled with DIB-Cl. The separation of DIB-derivatives was achieved on a reversed-phase semi-micro ODS column with an acetonitrile-methanol-water (30:40:30, v/v/v%) mixture as a mobile phase. The limits of detection at a signal-to-noise ratio of 3 for MDMA, MDA, MP and AP were 0.25, 0.15, 0.25 and 0.19 ng/mg, respectively. Precision of intra- and inter-day assay as the relative standard deviation were in the range 1.5-6.8% (n = 5) and 2.7-4.7% (n = 5), respectively. The proposed method was highly sensitive and able to detect MDMA and its related compounds in small amounts of hair sample, and could be applied to quantification of six abusers' hair samples.
建立了一种灵敏的半微柱高效液相色谱-荧光检测法，用于测定人发中的3,4-亚甲基二氧甲基苯丙胺（摇头丸）、3,4-亚甲基二氧苯丙胺（MDA）、甲基苯丙胺（MP）和苯丙胺（AP）。分别以4-(4,5-二苯基-1H-咪唑-2-基)苯甲酰氯（DIB-Cl）和1-甲基-3-苯基丙胺作为标记试剂和内标。这些药物从毛发中提取到含5%三氟乙酸的甲醇中，并用DIB-Cl进行荧光标记。DIB衍生物在反相半微ODS柱上分离，以乙腈-甲醇-水（30:40:30，v/v/v%）混合物作为流动相。摇头丸、MDA、MP和AP在信噪比为3时的检测限分别为0.25、0.15、0.25和0.19 ng/mg。日内和日间测定的精密度以相对标准偏差计，分别在1.5-6.8%（n = 5）和2.7-4.7%（n = 5）范围内。所提出的方法灵敏度高，能够检测少量毛发样品中的摇头丸及其相关化合物，可用于6名滥用者毛发样品的定量分析。
