Journal
ANALYTICA CHIMICA ACTA
Volume 508, Issue 2, Pages 147-158Publisher
ELSEVIER
DOI: 10.1016/j.aca.2003.11.067
Keywords
quinoxaline-2-carboxylic acid; gas chromatography-electron capture negative ionization mass spectrometry; carbadox; porcine liver; taguchi orthogonal array
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A sensitive and robust method using isotope dilution gas chromatography-electron capture negative chemical ionization mass spectrometry (GC-ECNI-MS) was developed and validated for the analysis of quinoxaline-2-carboxylic acid (QCA) in porcine liver. [H-2(4)]QCA was added to liver samples which were then deproteinated with 2% metaphosphoric acid in 20% methanol. Followed by sequential extraction with water-saturated ethyl acetate and phosphate buffer, the buffer extracts were subject to solid-phase extraction clean-up by mixed mode anion-exchange columns. QCA was derivatized with N-methyl-N-tert-butyldimethylsilyltrifluoroacetamide (MTBSTFA) prior to GC-ECNI-MS determination. For unambiguous identification, a second GC-ECNI-MS experiment was performed on suspected positive samples which were derivatized independently with another derivatization agent, trimethylsilyldiazomethane. Excellent recovery and precision were obtained and the limit of quantitation. was 0.7 mug/kg (S/N > 60). Method ruggedness by Taguchi orthogonal array technique is also presented. (C) 2003 Elsevier B.V. All rights reserved.
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