title: A simple and sensitive HPLC-fluorescence method for quantification of MDMA and MDA in blood with 4-(4,5-diphenyl-1H-imidazol-2-yl)benzoyl chloride (DIB-Cl) as a label.
abstract: A sensitive high-performance liquid chromatographic method with fluorescence detection to determine 3,4-methylenedioxymethamphethamine (MDMA) and 3,4-methylenedioxyamphethamine (MDA) in human and rat whole blood or plasma samples was developed by using 4-(4,5-diphenyl-1H-imidazol-2-yl)benzoyl chloride (DIB-Cl) as a label. MDMA and MDA in a small amount of blood sample (ca 100 microL) were extracted by liquid-liquid extraction with ethyl acetate, and were derivatized with DIB-Cl under mild conditions (10 min at room temperature). A good separation of DIB-derivatives could be achieved within 45 min using a commercially available ODS column with an isocratic eluent of 10 mM citric acid-20 mM Na(2)HPO(4) aqueous buffer (pH 4.0)-CH(3)CN-CH(3)OH (50:45:5, v/v/v %). The calibration curves prepared with 1-methyl-3-phenylpropylamine (MPPA) as an internal standard showed good linearity (r = 0.999) with 0.36-0.83 ng/mL detection limit at a signal-to-noise ratio of 3. MDMA and MDA in rat whole blood could be monitored for 6 h after a single administration of MDMA (2.2 mg/kg, i.p.). The pharmacokinetic parameters for MDMA and MDA obtained by triplicate measurements were 426 +/- 23 and 39 +/- 6 ng/mL (C(max)), 20 +/- 5 and 100 +/- 10 min (T(max)), respectively.
authors.affiliation: Department of Clinical Pharmacy, Course of Pharmaceutical Sciences, Graduate School of Biomedical Sciences, Nagasaki University, 1-14 Bunkyo-machi, Nagasaki 852-8521, Japan.
authors.forename: Mamoru
authors.initials: M
authors.lastname: Tomita
authors.forename: Mihoko N
authors.initials: MN
authors.lastname: Nakashima
authors.forename: Mitsuhiro
authors.initials: M
authors.lastname: Wada
authors.forename: Kenichiro
authors.initials: K
authors.lastname: Nakashima
mesh_terms: D015104:3,4-Methylenedioxyamphetamine / Q000097:blood*; D000818:Animals; D001565:Benzoates / Q000737:chemistry; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D005453:Fluorescence; D005456:Fluorescent Dyes / Q000737:chemistry; D006801:Humans; D007093:Imidazoles / Q000737:chemistry; D018817:N-Methyl-3,4-methylenedioxyamphetamine / Q000097:blood*; D051381:Rats
chemical_list: C114684:4-(4,5-diphenyl-1H-imidazol-2-yl)benzoyl chloride; D001565:Benzoates; D005456:Fluorescent Dyes; D007093:Imidazoles; D015104:3,4-Methylenedioxyamphetamine; D018817:N-Methyl-3,4-methylenedioxyamphetamine