Journal
JOURNAL OF CHROMATOGRAPHY A
Volume 1034, Issue 1-2, Pages 13-23Publisher
ELSEVIER
DOI: 10.1016/j.chroma.2004.02.032
Keywords
derivatization, GC; ethoxycarbonylation; methoximation; tert-butyldimethylsilylation; retention index matching; amino acids; carboxylic acids; keto acids
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Amino acids (AAs) in alkaline solution were first ethoxycarbonylated with subsequent methoximation of keto acids (KAs). After acidification and solid-phase extraction, tert-butyldimethylsilylation was performed for direct analysis by gas chromatography (GC) on dual-columns with different polarities, which provided simultaneous separation of multiple amino acids, carboxylic acids (CAs) and keto acids, facilitating accurate peak confirmation based on matching with retention index sets characteristic of each analyte. The present method was linear (r(2) greater than or equal to 0.9955) with good precision (0.1-9.4%) and accuracy (-8.6 to 9.9%), allowing simultaneous screening for diagnostic amino acids along with carboxylic acids and keto acids in urine from a phenylketonuria patient. (C) 2004 Elsevier B.V. All rights reserved.
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