PMID- 17080504 OWN - NLM STAT- MEDLINE DCOM- 20070226 LR - 20191210 IS - 0269-3879 (Print) IS - 0269-3879 (Linking) VI - 20 IP - 12 DP - 2006 Dec TI - 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. PG - 1380-5 AB - 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. CI - Copyright (c) 2006 John Wiley & Sons, Ltd. FAU - Tomita, Mamoru AU - Tomita M AD - Department of Clinical Pharmacy, Course of Pharmaceutical Sciences, Graduate School of Biomedical Sciences, Nagasaki University, 1-14 Bunkyo-machi, Nagasaki 852-8521, Japan. FAU - Nakashima, Mihoko N AU - Nakashima MN FAU - Wada, Mitsuhiro AU - Wada M FAU - Nakashima, Kenichiro AU - Nakashima K LA - eng PT - Journal Article PT - Validation Study PL - England TA - Biomed Chromatogr JT - Biomedical chromatography : BMC JID - 8610241 RN - 0 (4-(4,5-diphenyl-1H-imidazol-2-yl)benzoyl chloride) RN - 0 (Benzoates) RN - 0 (Fluorescent Dyes) RN - 0 (Imidazoles) RN - 4764-17-4 (3,4-Methylenedioxyamphetamine) RN - KE1SEN21RM (N-Methyl-3,4-methylenedioxyamphetamine) SB - IM MH - 3,4-Methylenedioxyamphetamine/*blood MH - Animals MH - Benzoates/chemistry MH - Chromatography, High Pressure Liquid/*methods MH - Fluorescence MH - Fluorescent Dyes/chemistry MH - Humans MH - Imidazoles/chemistry MH - N-Methyl-3,4-methylenedioxyamphetamine/*blood MH - Rats EDAT- 2006/11/03 09:00 MHDA- 2007/02/27 09:00 CRDT- 2006/11/03 09:00 PHST- 2006/11/03 09:00 [pubmed] PHST- 2007/02/27 09:00 [medline] PHST- 2006/11/03 09:00 [entrez] AID - 10.1002/bmc.716 [doi] PST - ppublish SO - Biomed Chromatogr. 2006 Dec;20(12):1380-5. doi: 10.1002/bmc.716.