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Drug testing in blood: validated negative-ion chemical ionization gas chromatographic-mass spectrometric assay for enantioselective measurement of the designer drugs MDEA, MDMA, and MDA and its application to samples from a controlled study with MDMA.
Clin Chem. 2005 Oct; 51(10):1811-22.CC

Abstract

BACKGROUND

The enantiomers of the designer drugs 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA), and 3,4-methylenedioxyethylamphetamine (MDEA) differ in their pharmacologic and toxicologic potency. The aim of this study was to develop an assay for measuring these enantiomers in small plasma volumes and to analyze samples from a controlled study with MDMA.

METHODS

The analytes were extracted from < or = 0.2 mL of plasma by mixed-mode solid-phase extraction. After derivatization with S-(-)-heptafluorobutyrylprolyl chloride, the resulting diastereomers were separated by gas chromatography (HP-5MS) within 17 min and detected by mass spectrometry in the negative-ion chemical ionization mode. The method was fully validated and applied to samples from a controlled study in which a single dose of racemic MDMA (75 mg) was administered.

RESULTS

The derivatized enantiomers were well separated and detected with good sensitivity. The assay was linear (per enantiomer) at 1-50 microg/L for MDA and 5-250 microg/L for MDMA and MDEA. Analytical recovery, accuracy, repeatability, and intermediate precision data were within required limits. Extraction yields were 82.1%-95.3%. In the study samples, concentrations of R-(-)-MDMA significantly exceeded those of S-(+)-MDMA. Their ratios (R vs S) were always >1.0 and increased over time. Concentrations of S-(+)-MDA exceeded those of R-(-)-MDA, their ratios (R vs S) also increasing over time but remaining <1.0.

CONCLUSIONS

This assay enables sensitive, reliable, and fast enantioselective measurement of MDA, MDMA, and MDEA in small volumes of plasma. The controlled study data confirm previous findings of MDMA and MDA enantiomer ratios (R vs S) increasing over time after ingestion of racemic MDMA.

Authors+Show Affiliations

Department of Experimental and Clinical Toxicology, Institute of Experimental and Clinical Pharmacology and Toxicology, University of Saarland, Homburg, Germany.No affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

Journal Article
Research Support, Non-U.S. Gov't
Validation Study

Language

eng

PubMed ID

16099938

Citation

Peters, Frank T., et al. "Drug Testing in Blood: Validated Negative-ion Chemical Ionization Gas Chromatographic-mass Spectrometric Assay for Enantioselective Measurement of the Designer Drugs MDEA, MDMA, and MDA and Its Application to Samples From a Controlled Study With MDMA." Clinical Chemistry, vol. 51, no. 10, 2005, pp. 1811-22.
Peters FT, Samyn N, Lamers CT, et al. Drug testing in blood: validated negative-ion chemical ionization gas chromatographic-mass spectrometric assay for enantioselective measurement of the designer drugs MDEA, MDMA, and MDA and its application to samples from a controlled study with MDMA. Clin Chem. 2005;51(10):1811-22.
Peters, F. T., Samyn, N., Lamers, C. T., Riedel, W. J., Kraemer, T., de Boeck, G., & Maurer, H. H. (2005). Drug testing in blood: validated negative-ion chemical ionization gas chromatographic-mass spectrometric assay for enantioselective measurement of the designer drugs MDEA, MDMA, and MDA and its application to samples from a controlled study with MDMA. Clinical Chemistry, 51(10), 1811-22.
Peters FT, et al. Drug Testing in Blood: Validated Negative-ion Chemical Ionization Gas Chromatographic-mass Spectrometric Assay for Enantioselective Measurement of the Designer Drugs MDEA, MDMA, and MDA and Its Application to Samples From a Controlled Study With MDMA. Clin Chem. 2005;51(10):1811-22. PubMed PMID: 16099938.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Drug testing in blood: validated negative-ion chemical ionization gas chromatographic-mass spectrometric assay for enantioselective measurement of the designer drugs MDEA, MDMA, and MDA and its application to samples from a controlled study with MDMA. AU - Peters,Frank T, AU - Samyn,Nele, AU - Lamers,Caroline T J, AU - Riedel,Wim J, AU - Kraemer,Thomas, AU - de Boeck,Gert, AU - Maurer,Hans H, Y1 - 2005/08/11/ PY - 2005/8/16/pubmed PY - 2006/1/13/medline PY - 2005/8/16/entrez SP - 1811 EP - 22 JF - Clinical chemistry JO - Clin. Chem. VL - 51 IS - 10 N2 - BACKGROUND: The enantiomers of the designer drugs 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA), and 3,4-methylenedioxyethylamphetamine (MDEA) differ in their pharmacologic and toxicologic potency. The aim of this study was to develop an assay for measuring these enantiomers in small plasma volumes and to analyze samples from a controlled study with MDMA. METHODS: The analytes were extracted from < or = 0.2 mL of plasma by mixed-mode solid-phase extraction. After derivatization with S-(-)-heptafluorobutyrylprolyl chloride, the resulting diastereomers were separated by gas chromatography (HP-5MS) within 17 min and detected by mass spectrometry in the negative-ion chemical ionization mode. The method was fully validated and applied to samples from a controlled study in which a single dose of racemic MDMA (75 mg) was administered. RESULTS: The derivatized enantiomers were well separated and detected with good sensitivity. The assay was linear (per enantiomer) at 1-50 microg/L for MDA and 5-250 microg/L for MDMA and MDEA. Analytical recovery, accuracy, repeatability, and intermediate precision data were within required limits. Extraction yields were 82.1%-95.3%. In the study samples, concentrations of R-(-)-MDMA significantly exceeded those of S-(+)-MDMA. Their ratios (R vs S) were always >1.0 and increased over time. Concentrations of S-(+)-MDA exceeded those of R-(-)-MDA, their ratios (R vs S) also increasing over time but remaining <1.0. CONCLUSIONS: This assay enables sensitive, reliable, and fast enantioselective measurement of MDA, MDMA, and MDEA in small volumes of plasma. The controlled study data confirm previous findings of MDMA and MDA enantiomer ratios (R vs S) increasing over time after ingestion of racemic MDMA. SN - 0009-9147 UR - https://www.unboundmedicine.com/medline/citation/16099938/Drug_testing_in_blood:_validated_negative_ion_chemical_ionization_gas_chromatographic_mass_spectrometric_assay_for_enantioselective_measurement_of_the_designer_drugs_MDEA_MDMA_and_MDA_and_its_application_to_samples_from_a_controlled_study_with_MDMA_ L2 - http://www.clinchem.org/cgi/pmidlookup?view=long&amp;pmid=16099938 DB - PRIME DP - Unbound Medicine ER -