Quantitative method for determination of amphetamine in plasma using negative ion chemical ionisation GC-MS of o-(pentafluorobenzyloxycarbonyl)-benzoyl derivatives.
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.
University Hospital of Youth and Adolescence Medicine, Research Unit of Osteology and Analytical Mass Spectrometry, Medical University of Graz, Graz, Austria. hans.leis@medunigraz.at
Hans J
HJ
Leis
Werner
W
Windischhofer
D000661:Amphetamine / Q000097:blood*; D001565:Benzoates / Q000737:chemistry*; D002138:Calibration; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D015203:Reproducibility of Results; D005464:Fluorobenzenes; D005466:Fluorocarbons
D000661:Amphetamine; D001565:Benzoates; C555522:2-(pentafluorobenzyloxycarbonyl)benzoyl chloride; D005464:Fluorobenzenes; D005466:Fluorocarbons