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Clauwaert KM, Van Bocxlaer JF, De Letter EA, Van Callenbergh S, Lambert WE, De Leenheer AP. 
“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”. 
Clin Chem. 2000;46(12):19681977.
Abstract

BACKGROUND: The popular designer drugs 3,4-methyl-enedioxymethamphetamine (MDMA) and 3,4-methyl-enedioxyethylamphetamine (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 C18 column by gradient elution with fluorometric detection; results were con-firmed by liquid chromatography-tandem mass spec-trometry (LC-MS/MS).


RESULTS: The method was linear over the range of 21000 mg/L for whole blood, serum, and vitreous humor, and 0.15 mg/L for urine. Extraction recoveries were >70%, imprecision (CV) was 2.519%, and analytical recoveries were 95.5104.4%. The limit of detection (LOD) and the limit of quantification (LOQ) were 0.8 and 2 mg/L, respectively, for whole blood, serum, and vitreous hu-mor, and 2.5 mg/L and 0.1 mg/L, respectively, for urine. Excellent correlations between the quantitative LC-flu-orescence and LC-MS/MS results were obtained. We found the following concentrations in a thanatochemi-cal distribution study in rabbits: in serum, 5.3 685 mg/L for MDMA and from the LOQ to 14.5 mg/L for 3,4-methylenedioxyamphetamine (MDA); in whole blood, 19.7710 mg/L for MDMAand from the LOQ to 17.8 mg/L for MDA; in vitreous humor, 12.197.8 mg/L for MDMA and from the LOQ to 3.86 mg/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.
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