title: Enantioselective trace analysis of amphetamine in human plasma by gas chromatography/negative ion chemical ionization mass spectrometry.
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.
authors.affiliation: University Children's Hospital, Division of Analytical Biochemistry and Mass Spectrometry, Auenbruggerplatz 30, 8036 Graz, Austria. hans.leis@uni-graz.at
authors.forename: Hans-Jörg
authors.initials: HJ
authors.lastname: Leis
authors.forename: Gerald N
authors.initials: GN
authors.lastname: Rechberger
authors.forename: Günter
authors.initials: G
authors.lastname: Fauler
authors.forename: Werner
authors.initials: W
authors.lastname: Windischhofer
mesh_terms: D000661:Amphetamine / Q000097:blood* / Q000737:chemistry / Q000493:pharmacokinetics; D002138:Calibration; D002849:Chromatography, Gas / Q000379:methods*; D004355:Drug Stability; D006586:Hexanes; D006801:Humans; D013058:Mass Spectrometry / Q000379:methods*; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D013237:Stereoisomerism
chemical_list: D006586:Hexanes; C026385:n-hexane; D000661:Amphetamine