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Negative-ion chemical ionization gas chromatography-mass spectrometry assay for enantioselective measurement of amphetamines in oral fluid: application to a controlled study with MDMA and driving under the influence cases.
Clin Chem. 2007 Apr; 53(4):702-10.CC

Abstract

BACKGROUND

Enantioselective analysis of amphetamine (AM), methamphetamine (MA), 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA), and 3,4-methylenedioxyethylamphetamine (MDEA) helps interpret toxicological results. Methods have been described for various matrices, but so far not for oral fluid, a matrix of increasing importance in testing for drugs of abuse, especially in the context of driving under the influence of drugs (DUID).

METHODS

After dilution with 200 microL carbonate buffer (pH 9), oral fluid samples (10-50 microL) were derivatized with S-heptafluorobutyrylprolyl chloride. The resulting diastereomers were extracted into 100 microL of cyclohexane, separated by gas chromatography (HP-5MS column), and detected by mass spectrometry in the negative-ion chemical ionization mode (GC-NICI-MS). The method was validated and applied to samples from a controlled study with MDMA and from authentic DUID cases.

RESULTS

The derivatized AM, MA, MDA, MDMA, and MDEA enantiomers were well separated from each other. The method was linear from 5-250 microg/L per enantiomer of MDA and from 25-1250 microg/L per enantiomer of AM, MA, MDMA, and MDEA. With the exception of MDEA, analytical recoveries, repeatability, and intermediate precision were within required limits. The analyte concentrations and enantiomer ratios in the application samples correlated only weakly with corresponding published plasma data.

CONCLUSIONS

This sensitive, reliable, and fast GC-NICI-MS assay enantioselectively measures AM, MA, MDA, and MDMA in oral fluid samples. Prediction of plasma concentrations and enantiomer ratios from respective oral fluid data is not possible.

Authors+Show Affiliations

Department of Experimental and Clinical Toxicology, Saarland University, Homburg (Saar), Germany.No affiliation info availableNo affiliation info availableNo affiliation info availableNo affiliation info available

Pub Type(s)

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

Language

eng

PubMed ID

17332148

Citation

Peters, Frank T., et al. "Negative-ion Chemical Ionization Gas Chromatography-mass Spectrometry Assay for Enantioselective Measurement of Amphetamines in Oral Fluid: Application to a Controlled Study With MDMA and Driving Under the Influence Cases." Clinical Chemistry, vol. 53, no. 4, 2007, pp. 702-10.
Peters FT, Samyn N, Kraemer T, et al. Negative-ion chemical ionization gas chromatography-mass spectrometry assay for enantioselective measurement of amphetamines in oral fluid: application to a controlled study with MDMA and driving under the influence cases. Clin Chem. 2007;53(4):702-10.
Peters, F. T., Samyn, N., Kraemer, T., Riedel, W. J., & Maurer, H. H. (2007). Negative-ion chemical ionization gas chromatography-mass spectrometry assay for enantioselective measurement of amphetamines in oral fluid: application to a controlled study with MDMA and driving under the influence cases. Clinical Chemistry, 53(4), 702-10.
Peters FT, et al. Negative-ion Chemical Ionization Gas Chromatography-mass Spectrometry Assay for Enantioselective Measurement of Amphetamines in Oral Fluid: Application to a Controlled Study With MDMA and Driving Under the Influence Cases. Clin Chem. 2007;53(4):702-10. PubMed PMID: 17332148.
* Article titles in AMA citation format should be in sentence-case
TY - JOUR T1 - Negative-ion chemical ionization gas chromatography-mass spectrometry assay for enantioselective measurement of amphetamines in oral fluid: application to a controlled study with MDMA and driving under the influence cases. AU - Peters,Frank T, AU - Samyn,Nele, AU - Kraemer,Thomas, AU - Riedel,Wim J, AU - Maurer,Hans H, Y1 - 2007/03/01/ PY - 2007/3/3/pubmed PY - 2007/5/22/medline PY - 2007/3/3/entrez SP - 702 EP - 10 JF - Clinical chemistry JO - Clin. Chem. VL - 53 IS - 4 N2 - BACKGROUND: Enantioselective analysis of amphetamine (AM), methamphetamine (MA), 3,4-methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA), and 3,4-methylenedioxyethylamphetamine (MDEA) helps interpret toxicological results. Methods have been described for various matrices, but so far not for oral fluid, a matrix of increasing importance in testing for drugs of abuse, especially in the context of driving under the influence of drugs (DUID). METHODS: After dilution with 200 microL carbonate buffer (pH 9), oral fluid samples (10-50 microL) were derivatized with S-heptafluorobutyrylprolyl chloride. The resulting diastereomers were extracted into 100 microL of cyclohexane, separated by gas chromatography (HP-5MS column), and detected by mass spectrometry in the negative-ion chemical ionization mode (GC-NICI-MS). The method was validated and applied to samples from a controlled study with MDMA and from authentic DUID cases. RESULTS: The derivatized AM, MA, MDA, MDMA, and MDEA enantiomers were well separated from each other. The method was linear from 5-250 microg/L per enantiomer of MDA and from 25-1250 microg/L per enantiomer of AM, MA, MDMA, and MDEA. With the exception of MDEA, analytical recoveries, repeatability, and intermediate precision were within required limits. The analyte concentrations and enantiomer ratios in the application samples correlated only weakly with corresponding published plasma data. CONCLUSIONS: This sensitive, reliable, and fast GC-NICI-MS assay enantioselectively measures AM, MA, MDA, and MDMA in oral fluid samples. Prediction of plasma concentrations and enantiomer ratios from respective oral fluid data is not possible. SN - 0009-9147 UR - https://www.unboundmedicine.com/medline/citation/17332148/Negative_ion_chemical_ionization_gas_chromatography_mass_spectrometry_assay_for_enantioselective_measurement_of_amphetamines_in_oral_fluid:_application_to_a_controlled_study_with_MDMA_and_driving_under_the_influence_cases_ L2 - http://www.clinchem.org/cgi/pmidlookup?view=long&pmid=17332148 DB - PRIME DP - Unbound Medicine ER -