PMID- 11106329 OWN - NLM STAT- MEDLINE DCOM- 20010104 LR - 20190722 IS - 0009-9147 (Print) IS - 0009-9147 (Linking) VI - 46 IP - 12 DP - 2000 Dec TI - Determination of the designer drugs 3, 4-methylenedioxymethamphetamine, 3,4-methylenedioxyethylamphetamine, and 3,4-methylenedioxyamphetamine with HPLC and fluorescence detection in whole blood, serum, vitreous humor, and urine. PG - 1968-77 AB - BACKGROUND: The popular designer drugs 3, 4-methylenedioxymethamphetamine (MDMA) and 3, 4-methylenedioxyethylamphetamine (MDEA) can be determined in serum, whole blood, and urine, but also in vitreous humor. The latter matrix is interesting when dealing with decomposed bodies in a toxicological setting. METHODS: After extraction, chromatographic separation was achieved on a narrow-bore C(18) column by gradient elution with fluorometric detection; results were confirmed by liquid chromatography-tandem mass spectrometry (LC-MS/MS). RESULTS: The method was linear over the range of 2-1000 microg/L for whole blood, serum, and vitreous humor, and 0.1-5 mg/L for urine. Extraction recoveries were >70%, imprecision (CV) was 2.5-19%, and analytical recoveries were 95.5-104.4%. The limit of detection (LOD) and the limit of quantification (LOQ) were 0.8 and 2 microg/L, respectively, for whole blood, serum, and vitreous humor, and 2.5 microg/L and 0.1 mg/L, respectively, for urine. Excellent correlations between the quantitative LC-fluorescence and LC-MS/MS results were obtained. We found the following concentrations in a thanatochemical distribution study in rabbits: in serum, 5.3-685 microg/L for MDMA and from the LOQ to 14.5 microg/L for 3, 4-methylenedioxyamphetamine (MDA); in whole blood, 19.7-710 microg/L for MDMA and from the LOQ to 17.8 microg/L for MDA; in vitreous humor, 12.1-97.8 microg/L for MDMA and from the LOQ to 3.86 microg/L for MDA. In routine toxicological urine samples, concentrations ranged from LOQ to 14.62 mg/L for MDA, from LOQ to 157 mg/L for MDMA, and from LOQ to 32.54 mg/L for MDEA. CONCLUSIONS: The HPLC method described is sensitive, specific, and suitable for the determination of MDMA, MDEA, and MDA in whole blood, serum, vitreous humor, and urine. FAU - Clauwaert, K M AU - Clauwaert KM AD - Laboratory of Toxicology and Laboratory of Medicinal Chemistry, Ghent University, Harelbekestraat 72, B-9000 Gent, Belgium. FAU - Van Bocxlaer, J F AU - Van Bocxlaer JF FAU - De Letter, E A AU - De Letter EA FAU - Van Calenbergh, S AU - Van Calenbergh S FAU - Lambert, W E AU - Lambert WE FAU - De Leenheer, A P AU - De Leenheer AP LA - eng PT - Journal Article PL - England TA - Clin Chem JT - Clinical chemistry JID - 9421549 RN - 0 (Designer Drugs) RN - 4764-17-4 (3,4-Methylenedioxyamphetamine) RN - KE1SEN21RM (N-Methyl-3,4-methylenedioxyamphetamine) RN - ML1I4KK67B (3,4-methylenedioxyethamphetamine) SB - IM MH - 3,4-Methylenedioxyamphetamine/*analogs & derivatives/*analysis/blood/urine MH - Animals MH - Chromatography, High Pressure Liquid MH - Designer Drugs/*analysis MH - Humans MH - Mass Spectrometry MH - N-Methyl-3,4-methylenedioxyamphetamine/*analysis/blood/urine MH - Rabbits MH - Reproducibility of Results MH - Sensitivity and Specificity MH - Spectrometry, Fluorescence MH - Substance Abuse Detection/*methods MH - Vitreous Body/*chemistry EDAT- 2000/12/06 11:00 MHDA- 2001/02/28 10:01 CRDT- 2000/12/06 11:00 PHST- 2000/12/06 11:00 [pubmed] PHST- 2001/02/28 10:01 [medline] PHST- 2000/12/06 11:00 [entrez] PST - ppublish SO - Clin Chem. 2000 Dec;46(12):1968-77.