Enantioselective trace analysis of amphetamine in human plasma by gas chromatography/negative ion chemical ionization mass spectrometry |
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Authors: | Leis Hans-Jörg Rechberger Gerald N Fauler Günter Windischhofer Werner |
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Institution: | University Children's Hospital, Division of Analytical Biochemistry and Mass Spectrometry, Auenbruggerplatz 30, 8036 Graz, Austria. hans.leis@uni-graz.at |
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Abstract: | 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. |
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