TITLE

Reagent peak-free liquid chromatography–fluorescence analysis of carboxylic acids using a fluorous scavenging–derivatization method

AUTHOR(S)
Todoroki, Kenichiro; Hashimoto, Hiroki; Mikawa, Tomohiko; Itoyama, Miki; Hayama, Tadashi; Kojima, Eijiro; Yoshida, Hideyuki; Nohta, Hitoshi; Yamaguchi, Masatoshi
PUB. DATE
July 2010
SOURCE
Analytical & Bioanalytical Chemistry;Jul2010, Vol. 397 Issue 6, p2409
SOURCE TYPE
Academic Journal
DOC. TYPE
Article
ABSTRACT
We developed a fluorous scavenging–derivatization method for reagent peak-free liquid chromatography (LC)–fluorescence analysis of carboxylic acids. In this method, carboxylic acids were fluorescently derivatized with 1-pyrenemethylamine in the presence of 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide and 1-hydroxy-1 H-benzotriazole. Residual excess unreacted reagent was tagged with 2-(perfluorooctyl)ethyl isocyanate and could be selectively removed by microfluorous solid-phase extraction before LC analysis. With use of this method, eight fluorescent derivatives of linear aliphatic carboxylic acids (C1–C8) can be separated within 30 min by reversed-phase LC with gradient elution. In the chromatogram obtained, the fluorous-tagged unreacted reagent peak is greatly decreased after microfluorous solid-phase extraction and does not interfere with the quantification of each acid. With use of microfluorous solid-phase extraction with 80% (v/v) aqueous methanol elution, over 99.9% of the unreacted fluorescent reagent was removed. The detection limits (signal-to-noise ratio of 3) for the carboxylic acids examined are 2.3–8.0 fmol per 10-μL injection. We also applied this method successfully to the analysis of highly polar carboxylic acids such as α-keto acids and tricarboxylic acid cycle metabolites.
ACCESSION #
51880435

 

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