Enantiomeric separation of non-protein amino acids by Electrokinetic Chromatography

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...

Descripción completa

Detalles Bibliográficos
Autores: Pérez Miguez, Raquel, Marina Alegre, María Luisa|||0000-0002-5583-1624, Castro Puyana, María|||0000-0003-1412-4103
Tipo de recurso: artículo
Fecha de publicación:2016
País:España
Institución:Universidad de Alcalá (UAH)
Repositorio:e_Buah Biblioteca Digital Universidad de Alcalá
Idioma:inglés
OAI Identifier:oai:ebuah.uah.es:10017/48159
Acceso en línea:http://hdl.handle.net/10017/48159
https://dx.doi.org/10.1016/j.chroma.2016.06.058
Access Level:acceso abierto
Palabra clave:Non-protein amino acids
Enantiomeric separation
Chiral CE
Electrokinetic chromatography
Citrulline
Food supplements
Química
Chemistry
Descripción
Sumario: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.