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Clinical Chemistry 48: 1472-1485, 2002;
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(Clinical Chemistry. 2002;48:1472-1485.)
© 2002 American Association for Clinical Chemistry, Inc.

Drug Testing in Blood: Validated Negative-Ion Chemical Ionization Gas Chromatographic–Mass Spectrometric Assay for Determination of Amphetamine and Methamphetamine Enantiomers and Its Application to Toxicology Cases

Frank T. Peters1, Thomas Kraemer1 and Hans H. Maurera1

1 Department of Experimental and Clinical Toxicology, Institute of Experimental and Clinical Pharmacology and Toxicology, University of Saarland, D-66421 Homburg (Saar), Germany.

aAuthor for correspondence. Fax 49-6841-16-26051; e-mail hans.maurer{at}uniklinik-saarland.de.

Background: Enantioselective analysis of amphetamine (AM) or methamphetamine (MA) in urine is already a well-established tool for differentiation of illicit from therapeutic ingestion of AM or MA derivatives. However, because of the increasing importance of plasma or serum in analytical toxicology, a method for enantioselective analysis of AM and MA in these matrices is needed.

Methods: AM and/or MA were extracted from 0.2 mL of blood plasma or serum by mixed-mode solid-phase extraction. After derivatization with S-(-)-heptafluorobutyrylprolyl chloride, the resulting diastereomers were separated by gas chromatography on a HP-5MS column during a 15-min program and detected by mass spectrometry in the negative-ion chemical ionization mode (NICI-GC-MS). The method was fully validated and applied to >50 samples from authentic toxicology cases.

Results: The derivatized AM and MA enantiomers were well separated and sensitively detected. The method was linear from 5 to 250 µg/L per enantiomer with analytical recoveries, accuracy, and within- and between-run precision well within required limits. Extraction yields were 88.9–98.6%. Implications of concentrations and enantiomeric composition of AM and MA in the authentic samples were considered.

Conclusions: This sensitive, reliable, rapid NICI-GC-MS assay is suitable for enantioselective determination of AM and MA in blood plasma or serum samples.




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