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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.
J Chromatogr B Analyt Technol Biomed Life Sci. 2010 Oct 15; 878(28):2905-10.JC

Abstract

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: 12.5-1250ng/mL urine for HMA, HMMA, MDA and MDMA, 25-2500ng/mL for HHMA, and 150-7500ng/mL for HHA (r(2)>0.993 for all analytes). The lower limits of quantification were 12.5ng/mL urine for MDMA, MDA, HMA and HMMA, 25ng/mL for HHMA and 150ng/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, HHA, HMMA and HMA in urine samples taken over 24h from rats given subcutaneous MDMA.

Authors+Show Affiliations

EA 4463 Université Paris Descartes, Laboratoire de Chimie-Toxicologie Analytique et Cellulaire, Faculté de Pharmacie, Avenue de l'Observatoire, F-75006 Paris, France. marie-claude.menet@parisdescartes.frNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article

Language

eng

PubMed ID

20843750

Citation

Menet, Marie-Claude, et al. "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." Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, vol. 878, no. 28, 2010, pp. 2905-10.
Menet MC, Fonsart J, Hervé F, et al. 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. J Chromatogr B Analyt Technol Biomed Life Sci. 2010;878(28):2905-10.
Menet, M. C., Fonsart, J., Hervé, F., Fompeydie, D., Galliot-Guilley, M., Noble, F., & Scherrmann, J. M. (2010). 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. Journal of Chromatography. B, Analytical Technologies in the Biomedical and Life Sciences, 878(28), 2905-10. https://doi.org/10.1016/j.jchromb.2010.08.018
Menet MC, et al. 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. J Chromatogr B Analyt Technol Biomed Life Sci. 2010 Oct 15;878(28):2905-10. PubMed PMID: 20843750.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - 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. AU - Menet,Marie-Claude, AU - Fonsart,Julien, AU - Hervé,Françoise, AU - Fompeydie,Dominique, AU - Galliot-Guilley,Martine, AU - Noble,Florence, AU - Scherrmann,Jean-Michel, Y1 - 2010/08/21/ PY - 2010/04/14/received PY - 2010/07/24/revised PY - 2010/08/14/accepted PY - 2010/9/17/entrez PY - 2010/9/17/pubmed PY - 2011/1/25/medline SP - 2905 EP - 10 JF - Journal of chromatography. B, Analytical technologies in the biomedical and life sciences JO - J Chromatogr B Analyt Technol Biomed Life Sci VL - 878 IS - 28 N2 - 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: 12.5-1250ng/mL urine for HMA, HMMA, MDA and MDMA, 25-2500ng/mL for HHMA, and 150-7500ng/mL for HHA (r(2)>0.993 for all analytes). The lower limits of quantification were 12.5ng/mL urine for MDMA, MDA, HMA and HMMA, 25ng/mL for HHMA and 150ng/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, HHA, HMMA and HMA in urine samples taken over 24h from rats given subcutaneous MDMA. SN - 1873-376X UR - https://www.unboundmedicine.com/medline/citation/20843750/Determination_of_34_methylenedioxymethamphetamine_and_its_five_main_metabolites_in_rat_urine_by_solid_phase_extraction_and_high_performance_liquid_chromatography_with_on_line_mass_spectrometry_ L2 - https://linkinghub.elsevier.com/retrieve/pii/S1570-0232(10)00509-X DB - PRIME DP - Unbound Medicine ER -