Article (Scientific journals)
Chemo- and enantio-selective method for the analysis of amino acids by capillary electrophoresis with in-capillary derivatization.
Fradi, Ines; Servais, Anne-Catherine; Lamalle, Caroline et al.
2012In Journal of Chromatography. A, 1267, p. 121-6
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Keywords :
Amino acids; Chiral capillary electrophoresis; In-capillary derivatization
Abstract :
[en] A novel dual chiral CE method was developed for the separation of l- and d-amino acids (AAs), using in-capillary derivatization with 9-fluoroenylmethyl chloroformate (FMOC). Firstly, using pre-column derivatization, the enantioseparation of FMOC-AAs was optimized according to the nature of cyclodextrins (CD). A background electrolyte (BGE) composed of 30mM beta-CD, 30mM octakis(2,3-dihydroxy-6-O-sulfo)-gamma-CD (OS-gamma-CD), 40mM tetraborate and 15% isopropanol (IPA) was selected and led to 17 baseline resolved pairs (R(s)=1.7-5.8) and two partially resolved pairs (Lys, R(s)=0.5 and Arg, R(s)=1.2). Experimental conditions for in-capillary derivatization were then optimized. Several parameters, such as mixing voltage and time, concentration of labeling solution and the length of the spacer plug were studied. The optimal conditions for in-capillary derivatization procedure were obtained using successive hydrodynamic injections (30mbar) of AAs for 2s, borate buffer for 4s and 10mM FMOC solution for 6s, followed by a mixing at 3kV for 72s and wait time of 1min. Moreover, a particular attention was paid to improve separation chemoselectivity. The effect on stereoselectivity and chemoselectivity of different factors, such as decrease of pH and tetraborate concentration and the addition of sodium dodecyl sulfate (SDS), was investigated using the in-capillary derivatization procedure. The best separation of a standard mixture of ten AA racemates was observed using a BGE containing 30mM beta-CD, 30mM OS-gamma-CD, 25mM SDS, 40mM sodium tetraborate and 17% IPA.
Disciplines :
Pharmacy, pharmacology & toxicology
Author, co-author :
Fradi, Ines ;  Université de Liège - ULiège > Doct. sc. bioméd. & pharma. (Bologne)
Servais, Anne-Catherine  ;  Université de Liège - ULiège > Département de pharmacie > Analyse des médicaments
Lamalle, Caroline ;  Université de Liège - ULiège > Département de pharmacie > Analyse des médicaments
Kallel, M.
Abidi, M.
Crommen, Jacques ;  Université de Liège - ULiège > Département de pharmacie > Département de pharmacie
Fillet, Marianne ;  Université de Liège - ULiège > Département de pharmacie > Analyse des médicaments
Language :
English
Title :
Chemo- and enantio-selective method for the analysis of amino acids by capillary electrophoresis with in-capillary derivatization.
Publication date :
2012
Journal title :
Journal of Chromatography. A
ISSN :
0021-9673
eISSN :
1873-3778
Publisher :
Elsevier, Amsterdam, Netherlands
Volume :
1267
Pages :
121-6
Peer reviewed :
Peer Reviewed verified by ORBi
Funders :
WBI - Wallonie-Bruxelles International [BE]
F.R.S.-FNRS - Fonds de la Recherche Scientifique [BE]
Fonds Léon Fredericq [BE]
Commentary :
Copyright (c) 2012 Elsevier B.V. All rights reserved.
Available on ORBi :
since 02 July 2012

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