Precolumn derivatization for improved detection in liquid chromatography-photolysis-electrochemistry. 1987

M Y Chang, and L R Chen, and X D Ding, and C M Selavka, and I S Krull, and K Bratin
Barnett Institute of Chemical Analysis, Northeastern University, Boston, Massachusetts 02115.

Precolumn, homogeneous chemical derivatization with Sanger's reagent (2,4-dinitrofluorobenzene) is utilized to improve the chromatographic and detection properties of amino alcohols and amino acids. The 2,4-dinitrophenyl derivatives are separated using reversed-phase liquid chromatography and are detected using the hybrid photolysis-electrochemical (hv-EC) detector in tandem with UV absorbance detection. Following optimization of reaction, chromatographic, and detection variables, the derivatization-detection approach provides limits of detection in the low parts-per-billion range, with a linearity of roughly three orders of magnitude. Selectivity is based on retention times as well as dual electrode response ratios and a "lamp on/off" responsiveness criterion unique to the hv-EC detector. The method is applied to the determination of serine in beer.

UI MeSH Term Description Entries
D002853 Chromatography, Liquid Chromatographic techniques in which the mobile phase is a liquid. Liquid Chromatography
D004139 Dinitrofluorobenzene Irritants and reagents for labeling terminal amino acid groups. DNFB,Fluorodinitrobenzene,1-Fluoro-2,4-dinitrobenzene,1 Fluoro 2,4 dinitrobenzene
D004563 Electrochemistry The study of chemical changes resulting from electrical action and electrical activity resulting from chemical changes. Electrochemistries
D000596 Amino Acids Organic compounds that generally contain an amino (-NH2) and a carboxyl (-COOH) group. Twenty alpha-amino acids are the subunits which are polymerized to form proteins. Amino Acid,Acid, Amino,Acids, Amino
D000605 Amino Alcohols Compounds possessing both a hydroxyl (-OH) and an amino group (-NH2). Alcohols, Amino

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