PMID- 15924321 OWN - NLM STAT- MEDLINE DCOM- 20051201 LR - 20131121 IS - 1522-7235 (Print) IS - 1522-7235 (Linking) VI - 20 IP - 3 DP - 2005 May-Jun TI - Determination of MDMA and MDA in rat urine by semi-micro column HPLC-fluorescence detection with DBD-F and their monitoring after MDMA administration to rat. PG - 210-5 AB - A simultaneous semi-micro column HPLC method with fluorescence detection of abused drugs, such as 3,4-methylenedioxymethamphetamine (MDMA), 3,4-methylenedioxyamphetamine (MDA), amphetamine (AP) and methamphetamine (MP) in rat urine was examined by using 4-(N,N-dimethylaminosulphonyl)-7-fluoro-1,2,3-benzoxadiazole (DBD-F) as a labelling reagent and alpha-phenylethylamine as an internal standard (IS). A sample (50 microL) of rat urine was added to 5 microL IS and 100 microL 100 mmol/L borate buffer (pH 12) and extracted with 1.5 mL n-hexane. After evaporation, 50 microL 75 mmol/L borate buffer (pH 8.5) and 50 microL 20 mmol/L DBD-F in CH3CN were added to the residue and mixed well. The resultant solution was heated for 20 min at 80 degrees C and then cooled in an ice bath. A good separation of DBD-derivatives could be achieved within 45 min using a semi-micro ODS column with an eluent of CH3CN/CH3OH/10 mmol/L imidazole-HNO3 buffer (pH 7.0) (= 45:5:50, v/v/v %). The DBD derivatives were monitored at 565 nm with an excitation at 470 nm. The calibration curves showed good linearity (r = 0.997) with 0.5-15 ng/mL detection limits at a S/N ratio of 3. MDMA and MDA in rat urine could be monitored for 15 h after a single administration of MDMA to rat (2.0 mg/kg, i.p.). The concentrations for MDMA and MDA (n = 3) were 0.13-160.1 and 0.17-10.9 microg/mL, respectively. FAU - Wada, Mitsuhiro AU - Wada 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 - Nakamura, Shinichi AU - Nakamura S FAU - Tomita, Mamoru AU - Tomita M FAU - Nakashima, Mihoko N AU - Nakashima MN FAU - Nakashima, Kenichiro AU - Nakashima K LA - eng PT - Journal Article PL - England TA - Luminescence JT - Luminescence : the journal of biological and chemical luminescence JID - 100889025 RN - 0 (Borates) RN - 0 (Diazonium Compounds) RN - 0 (p-(N-N-dimethylamino)-benzendiazonium fluoroborate) RN - 4764-17-4 (3,4-Methylenedioxyamphetamine) RN - KE1SEN21RM (N-Methyl-3,4-methylenedioxyamphetamine) SB - IM MH - 3,4-Methylenedioxyamphetamine/*urine MH - Animals MH - Borates MH - Calibration MH - Chromatography, High Pressure Liquid MH - Diazonium Compounds MH - Drug Monitoring/methods MH - Fluorometry MH - Male MH - N-Methyl-3,4-methylenedioxyamphetamine/administration & dosage/*urine MH - Rats MH - Rats, Wistar MH - Substance Abuse Detection/*methods/standards EDAT- 2005/06/01 09:00 MHDA- 2005/12/13 09:00 CRDT- 2005/06/01 09:00 PHST- 2005/06/01 09:00 [pubmed] PHST- 2005/12/13 09:00 [medline] PHST- 2005/06/01 09:00 [entrez] AID - 10.1002/bio.821 [doi] PST - ppublish SO - Luminescence. 2005 May-Jun;20(3):210-5. doi: 10.1002/bio.821.