Determination of 3,4-methylenedioxymethamphetamine and its five main metabolites in rat urine by solid-phase extraction and high performance liquid chromatography with on line mass spectrometry

作者:Menet Marie Claude*; Fonsart Julien; Herve Francoise; Fompeydie Dominique; Galliot Guilley Martine; Noble Florence; Scherrmann Jean Michel
来源:Journal of Chromatography B-Analytical Technologies in the Biomedical and Life Sciences, 2010, 878(28): 2905-2910.
DOI:10.1016/j.jchromb.2010.08.018

摘要

The consumption of psychostimulant amphetamine-like drugs has increased significantly in recent years. Some MDMA metabolites are probably involved in the neurotoxicity and neurodegeneration caused by prolonged use rather than MDMA itself. We recently developed a method to analyze MDMA and its five main metabolites in rat plasma [7]. We have now fully validated this method to the quantification of these drugs in rat urine. We extracted MDMA and its metabolites with Oasis WCX cartridges, separated them on a Nucleodur C18 analytical column and quantified them by ion-trap mass spectrometry. Linearity was excellent: 12.5-1250 ng/mL urine for HMA, HMMA, MDA and MDMA, 25-2500 ng/mL for HHMA, and 150-7500 ng/mL for HHA (r(2) > 0.993 for all analytes). The lower limits of quantification were 12.5 ng/mL urine for MDMA, MDA, HMA and HMMA, 25 ng/mL for HHMA and 150 ng/mL for HHA. Reproducibility was good (intra-assay precision = 1.7-6.1%; inter-assay precision = 0.6-5.7%), as was accuracy (intra-assay deviation = 0.1-4.8%; inter-assay deviation = 0.7-7.9%). Average recoveries were around 85.0%, except for HHMA (66.2%) and HHA (53.0%) (CV < 8.3%). We also checked the stability of stock solutions and the internal standards after freeze-thawing and in the autosampler. Lastly, we measured the MDMA, MDA. HHMA, H HA, HMMA and HMA in urine samples taken over 24 h from rats given subcutaneous MDMA.

  • 出版日期2010-10-15