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Enantioselective trace analysis of amphetamine in human plasma by gas chromatography/negative ion chemical ionization mass spectrometry
Author(s) -
Leis HansJörg,
Rechberger Gerald N.,
Fauler Günter,
Windischhofer Werner
Publication year - 2003
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.949
Subject(s) - chemistry , derivatization , chromatography , mass spectrometry , chemical ionization , calibration curve , enantiomer , gas chromatography , gas chromatography–mass spectrometry , sample preparation , analytical chemistry (journal) , ionization , detection limit , ion , organic chemistry
A method for the quantitative enantioselective analysis of amphetamine in human plasma by gas chromatography/negative ion chemical ionization mass spectrometry (GC/NICI‐MS) is presented. Five‐fold deuterated analogues of both enantiomers were used as internal standard. Plasma sample preparation was performed by a rapid liquid–liquid extraction using n‐hexane. Derivatization with ( S )‐( − )‐ N ‐(heptafluorobutyryl)prolyl chloride was accomplished directly in the n‐hexane extract to avoid loss of amphetamine during sample concentration. The method was validated in the expected concentration range of 0.006 for a pharmacokinetic study. Calibration curves were linear within a range 0.006–50 ng/mL plasma. Precision and accuracy were acceptable over the entire calibration range. Baseline separation of the enantiomers was easily achieved on a 15‐m nonchiral apolar column. The method is simple and robust, and has been applied to the batch analysis of amphetamine enantiomers. Copyright © 2003 John Wiley & Sons, Ltd.