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):1968–1977.
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 2–1000 mg/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 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, 19.7–710 mg/L for MDMAand from the LOQ to 17.8 mg/L for MDA; in vitreous humor, 12.1–97.8 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.