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Quantitative method for determination of amphetamine in plasma using negative ion chemical ionisation GC ‐ MS of o ‐(pentafluorobenzyloxycarbonyl)‐benzoyl derivatives
Author(s) -
Leis Hans J.,
Windischhofer Werner
Publication year - 2012
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201200082
Subject(s) - chemistry , chromatography , reagent , mass spectrometry , chemical ionization , benzoyl chloride , derivatization , extraction (chemistry) , gas chromatography , sample preparation , analytical chemistry (journal) , gas chromatography–mass spectrometry , ionization , ion , organic chemistry
The use of a novel electrophoric derivatisation reagent, o ‐(pentafluorobenzyloxycarbonyl)‐benzoyl chloride is described for the quantitative determination of amphetamine in plasma. Amphetamine can be quantitatively measured down to 49 pg/mL plasma using only 250 μL of sample due to the extraordinary sensitivity of the derivatives under negative ion chemical ionisation mass spectrometry. Plasma samples were made alkaline with carbonate buffer and treated with n ‐hexane and reagent solution for 20 min, which, after concentration was measured by negative ion chemical ionisation gas chromatography‐mass spectrometry. The method is rapid as extraction and derivatisation occur in one single step. [ 2 H 5 ]‐Amphetamine was used as an internal standard. Validation data are given to demonstrate the usefulness of the assay, including specificity, linearity, accuracy and precision, benchtop stability, freeze–thaw stability, autosampler stability, aliquot analysis and prospective analytical batch size accuracy.