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Determination of amphetamine and methamphetamine enantiomers by chiral derivatization and gas chromatography–mass spectrometry as a test case for an automated sample preparation system
Author(s) -
Sievert HansJürgen P.
Publication year - 1994
Publication title -
chirality
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.43
H-Index - 77
eISSN - 1520-636X
pISSN - 0899-0042
DOI - 10.1002/chir.530060413
Subject(s) - derivatization , chemistry , chromatography , analyte , reproducibility , sample preparation , mass spectrometry , enantiomer , gas chromatography , diastereomer , organic chemistry
An automated sample preparation system has been applied to the chiral analysis of amphetamine and methamphetamine using derivatization with trifluoracetyl‐ L ‐prolyl chloride ( L ‐TPC) and subsequent separation on a gas chromatography–mass spectrometry (GC‐MS) system. Tasks automated were the dilution of standards and the off‐line preparation of the diastereoisomer derivatives. Chromatographic performance, sensitivity, and reproducibility of the automated procedure were compared to the equivalent values obtained with two existing assays methods which employ manual derivatiation, either on‐column or off‐line. Chromatographic performance was unaffected by the derivatization procedure and sensitivity was better for both automated and manual off‐line derivatization. Qualitative reproducibility as based on enantiomeric composition was equivalent for all three approaches, while quantitative reproducibility as based on peak areas was best for the automated procedure. Considering the fact that the diastereoisomer derivatives are unstable over time, automated sample preparation with “just‐in‐time” derivatization can increase the overall precision of the analytical method. The procedures described here are general enough in nature that they could be applied to other chiral or even achiral analytes. © 1994 Wiley‐Liss, Inc.