title: Quantification of MDMA and MDA in abusers' hair samples by semi-micro column HPLC with fluorescence detection.
abstract: 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.
authors.affiliation: Department of Clinical Pharmacy, Course of Pharmaceutical Sciences, Graduate School of Biomedical Sciences, Nagasaki University, Japan.
authors.forename: Shinichi
authors.initials: S
authors.lastname: Nakamura
authors.forename: Mamoru
authors.initials: M
authors.lastname: Tomita
authors.forename: Mitsuhiro
authors.initials: M
authors.lastname: Wada
authors.forename: Heesun
authors.initials: H
authors.lastname: Chung
authors.forename: Naotaka
authors.initials: N
authors.lastname: Kuroda
authors.forename: Kenichiro
authors.initials: K
authors.lastname: Nakashima
mesh_terms: D015104:3,4-Methylenedioxyamphetamine / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D006197:Hair / Q000737:chemistry*; D006801:Humans; D018817:N-Methyl-3,4-methylenedioxyamphetamine / Q000032:analysis*; D012015:Reference Standards; D013050:Spectrometry, Fluorescence / Q000379:methods*
chemical_list: D015104:3,4-Methylenedioxyamphetamine; D018817:N-Methyl-3,4-methylenedioxyamphetamine