RT info:eu-repo/semantics/article T1 Enantiomeric separation of non-protein amino acids by Electrokinetic Chromatography A1 Pérez Miguez, Raquel A1 Marina Alegre, María Luisa A1 Castro Puyana, María K1 Non-protein amino acids K1 Enantiomeric separation K1 Chiral CE K1 Electrokinetic chromatography K1 Citrulline K1 Food supplements K1 Química K1 Chemistry AB New analytical methodologies enabling the enantiomeric separation of a group of non-protein amino acids of interest in the pharmaceutical and food analysis fields were developed in this work using Electrokinetic Chromatography. The use of FMOC as derivatization reagent and the subsequent separation using acidic conditions (formate buffer at pH 2.0) and anionic cyclodextrins as chiral selectors allowed the chiral separation of eight from the ten non-protein amino acids studied. Pyroglutamic acid, norvaline, norleucine, 3,4-dihydroxyphenilalanine, 2-aminoadipic acid, and selenomethionine were enantiomericaly separated using sulfated-alpha-CD while sulfated-gamma-CD enabled the enantiomeric separation of norvaline, 3,4-dihydroxyphenilalanine, 2-aminoadipic acid, selenomethionie, citrulline, and pipecolic acid. Moreover, the potential of the developed methodologies was demonstrated in the analysis of citrulline and its enantiomeric impurity in food supplements. For that purpose, experimental and instrumental variables were optimized and the analytical characteristics of the proposed method were evaluated. LODs of 2.1 x 10(-7) and 1.8 x 10(-7) M for D-and L-citrulline, respectively, were obtained. D-Cit was not detectable in any of the six food supplement samples analyzed showing that the effect of storage time on the racemization of citrulline was negligible. (C) 2016 Elsevier B.V. All rights reserved. SN 0021-9673 YR 2016 FD 2016-06-18 LK http://hdl.handle.net/10017/48159 UL http://hdl.handle.net/10017/48159 LA eng DS MINDS@UW RD 23-abr-2024