Simultaneous Identification of the Enantiomers and Diastereomers of N,O-Di-trifluoroacetylated Ephedrine and Norephedrine in Blood Plasma using Chiral Capillary Gas Chromatography-Mass Spectrometry with Selected Ion Monitoring
| Autor: | Shinobu Yamauchi, Akira Kurosu, Atsushi Tohei, Junko Maeda, Shogo Tokudome, Kazumi Matsushima, Masahito Hitosugi, Toshiaki Nagai |
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| Rok vydání: | 2012 |
| Předmět: |
Male
Health Toxicology and Mutagenesis Guinea Pigs Phenylpropanolamine Toxicology Mass spectrometry Gas Chromatography-Mass Spectrometry Analytical Chemistry Plasma chemistry.chemical_compound medicine Animals Humans Environmental Chemistry Selected ion monitoring Ephedrine Derivatization Detection limit Chemical Health and Safety Chromatography Amphetamines beta-Cyclodextrins Diastereomer Stereoisomerism Pseudoephedrine chemistry Calibration Enantiomer medicine.drug |
| Zdroj: | Journal of Analytical Toxicology. 36:96-105 |
| ISSN: | 1945-2403 0146-4760 |
| Popis: | A method for identifying the enantiomers of N,O-di-trifluoroacetylated ephedrine (EP) and norephedrine (NE) and the enantiomers of pseudoephedrine (PEP) and pseudonorephedrine (PNE) in plasma was developed using chiral capillary gas chromatography-mass spectrometry (GC-MS) with selected ion monitoring (SIM). N,O-Di-trifluoroacethyl (TFA) derivatization was accomplished in a dried hydrochloride extract of plasma (minimum quantity of 0.2 mL). An SIM GC-MS method with a β-cyclodextrin chiral capillary column allowed the successful and simultaneous detection of each TFA-derivatized stereoisomer of EP, NE, PEP, PNE, and an internal standard (IS; S-(+)-ethylamphetamine). Each TFA-drivatized stereoisomer was identified using four mass fragment ions (m/z 140, 154, 168, and 230). The TFA-derivatized stereoisomers of EP, NE, PEP, PNE, and IS were separated completely and were detected with sufficient sensitivity. The assay allowed the stereoisomers to be determined in a linear range of 12.5-1250 ng/mL for the EP stereoisomers and a linear range of 5-1250 ng/mL for the PEP, NE, and PNE stereoisomers. The detection limits were 7.5 ng/mL for the EP stereoisomers and 2.5 ng/mL for the PEP, NE, and PNE stereoisomers. The intra- and interday precisions were less than 5.9% and 8.2%, respectively. This chiral capillary SIM GC-MS method was sufficiently effective in the analysis of plasma from users of over-the-counter cold medicines and was also fully applicable to the plasma analysis of guinea pigs following their treatment with racemic EP. |
| Databáze: | OpenAIRE |
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