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Two-dimensional gas chromatography/electron-impact mass spectrometry with cryofocusing for simultaneous quantification of MDMA, MDA, HMMA, HMA, and MDEA in human plasma.
Clin Chem. 2008 Feb; 54(2):379-87.CC

Abstract

BACKGROUND

3,4-Methylenedioxymethamphetamine (MDMA, or Ecstasy) is a popular recreational drug. Analysis of MDMA and metabolites in human plasma, particularly in pharmacokinetic studies, requires low limits of quantification. Two-dimensional GC/MS with cryofocusing is a chromatographic technique recognized for its increased selectivity and resolution.

METHODS

This method simultaneously quantifies 3,4-methylenedioxyethylamphetamine (MDEA), MDMA, and its metabolites, 3,4-methylenedioxyamphetamine (MDA), 4-hydroxy-3-methoxymethamphetamine (HMMA), and 4-hydroxy-3-methoxyamphetamine (HMA) in human plasma. With hydrochloric acid, we hydrolyzed 1 mL plasma, fortified with internal standard. Analytes were subjected to solid-phase extraction, derivatized with heptafluorobutyric acid anhydride, and quantified using cryofocused 2-dimensional GC/MS operated in electron-impact selected ion-monitoring mode.

RESULTS

Limits of quantification were 1.0 microg/L for MDA and 2.5 microg/L for MDEA, MDMA, HMMA, and HMA. Calibration curves were linear to 100 microg/L for MDA and HMA and to 400 microg/L for MDEA, MDMA, and HMMA, with r(2) > 0.997. At 3 concentrations spanning the linear dynamic range of the assay, mean overall extraction efficiencies from plasma were > or =85% for all compounds of interest. Recoveries were 85.6% to 107.2% of target, and intra- and interassay imprecision (CV) was <8.5% for all drugs at 3 concentrations within the range of the assay. None of the 66 exogenous compounds tested interfered with analyte quantification.

CONCLUSIONS

This GC/MS assay provides low limits of quantification for simultaneous determination of MDEA, MDMA, and metabolites MDA, HMMA, and HMA in human plasma. The 2D chromatographic system should be suitable for application to other analytes and to other complex matrices.

Authors+Show Affiliations

Chemistry and Drug Metabolism, Intramural Research Program, National Institute on Drug Abuse, National Institutes of Health, Baltimore, MD, USA.No affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article
Research Support, N.I.H., Intramural

Language

eng

PubMed ID

18089653

Citation

Kolbrich, Erin A., et al. "Two-dimensional Gas Chromatography/electron-impact Mass Spectrometry With Cryofocusing for Simultaneous Quantification of MDMA, MDA, HMMA, HMA, and MDEA in Human Plasma." Clinical Chemistry, vol. 54, no. 2, 2008, pp. 379-87.
Kolbrich EA, Lowe RH, Huestis MA. Two-dimensional gas chromatography/electron-impact mass spectrometry with cryofocusing for simultaneous quantification of MDMA, MDA, HMMA, HMA, and MDEA in human plasma. Clin Chem. 2008;54(2):379-87.
Kolbrich, E. A., Lowe, R. H., & Huestis, M. A. (2008). Two-dimensional gas chromatography/electron-impact mass spectrometry with cryofocusing for simultaneous quantification of MDMA, MDA, HMMA, HMA, and MDEA in human plasma. Clinical Chemistry, 54(2), 379-87.
Kolbrich EA, Lowe RH, Huestis MA. Two-dimensional Gas Chromatography/electron-impact Mass Spectrometry With Cryofocusing for Simultaneous Quantification of MDMA, MDA, HMMA, HMA, and MDEA in Human Plasma. Clin Chem. 2008;54(2):379-87. PubMed PMID: 18089653.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Two-dimensional gas chromatography/electron-impact mass spectrometry with cryofocusing for simultaneous quantification of MDMA, MDA, HMMA, HMA, and MDEA in human plasma. AU - Kolbrich,Erin A, AU - Lowe,Ross H, AU - Huestis,Marilyn A, Y1 - 2007/12/18/ PY - 2007/12/20/pubmed PY - 2008/4/4/medline PY - 2007/12/20/entrez SP - 379 EP - 87 JF - Clinical chemistry JO - Clin Chem VL - 54 IS - 2 N2 - BACKGROUND: 3,4-Methylenedioxymethamphetamine (MDMA, or Ecstasy) is a popular recreational drug. Analysis of MDMA and metabolites in human plasma, particularly in pharmacokinetic studies, requires low limits of quantification. Two-dimensional GC/MS with cryofocusing is a chromatographic technique recognized for its increased selectivity and resolution. METHODS: This method simultaneously quantifies 3,4-methylenedioxyethylamphetamine (MDEA), MDMA, and its metabolites, 3,4-methylenedioxyamphetamine (MDA), 4-hydroxy-3-methoxymethamphetamine (HMMA), and 4-hydroxy-3-methoxyamphetamine (HMA) in human plasma. With hydrochloric acid, we hydrolyzed 1 mL plasma, fortified with internal standard. Analytes were subjected to solid-phase extraction, derivatized with heptafluorobutyric acid anhydride, and quantified using cryofocused 2-dimensional GC/MS operated in electron-impact selected ion-monitoring mode. RESULTS: Limits of quantification were 1.0 microg/L for MDA and 2.5 microg/L for MDEA, MDMA, HMMA, and HMA. Calibration curves were linear to 100 microg/L for MDA and HMA and to 400 microg/L for MDEA, MDMA, and HMMA, with r(2) > 0.997. At 3 concentrations spanning the linear dynamic range of the assay, mean overall extraction efficiencies from plasma were > or =85% for all compounds of interest. Recoveries were 85.6% to 107.2% of target, and intra- and interassay imprecision (CV) was <8.5% for all drugs at 3 concentrations within the range of the assay. None of the 66 exogenous compounds tested interfered with analyte quantification. CONCLUSIONS: This GC/MS assay provides low limits of quantification for simultaneous determination of MDEA, MDMA, and metabolites MDA, HMMA, and HMA in human plasma. The 2D chromatographic system should be suitable for application to other analytes and to other complex matrices. SN - 0009-9147 UR - https://www.unboundmedicine.com/medline/citation/18089653/Two_dimensional_gas_chromatography/electron_impact_mass_spectrometry_with_cryofocusing_for_simultaneous_quantification_of_MDMA_MDA_HMMA_HMA_and_MDEA_in_human_plasma_ L2 - https://academic.oup.com/clinchem/article-lookup/doi/10.1373/clinchem.2007.096800 DB - PRIME DP - Unbound Medicine ER -