Reference : Chemo- and enantio-selective method for the analysis of amino acids by capillary electro...
Scientific journals : Article
Human health sciences : Pharmacy, pharmacology & toxicology
http://hdl.handle.net/2268/126615
Chemo- and enantio-selective method for the analysis of amino acids by capillary electrophoresis with in-capillary derivatization.
English
Fradi, Ines mailto [Université de Liège - ULg > > > Doct. sc. bioméd. & pharma. (Bologne)]
Servais, Anne-Catherine mailto [Université de Liège - ULg > Département de pharmacie > Analyse des médicaments >]
Lamalle, Caroline mailto [Université de Liège - ULg > Département de pharmacie > Analyse des médicaments >]
Kallel, M. [> >]
Abidi, M. [> >]
Crommen, Jacques mailto [Université de Liège - ULg > Département de pharmacie > Département de pharmacie >]
Fillet, Marianne mailto [Université de Liège - ULg > Département de pharmacie > Analyse des médicaments >]
2012
Journal of Chromatography. A
Yes (verified by ORBi)
International
0021-9673
1873-3778
[en] Amino acids ; Chiral capillary electrophoresis ; In-capillary derivatization
[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.
Wallonia Brussels International (WBI) ; Fonds de la Recherche Scientifique (Communauté française de Belgique) - F.R.S.-FNRS ; Fonds Léon Fredericq
http://hdl.handle.net/2268/126615
Copyright (c) 2012 Elsevier B.V. All rights reserved.

File(s) associated to this reference

Fulltext file(s):

FileCommentaryVersionSizeAccess
Restricted access
JCA 2012.pdfPublisher postprint597.6 kBRequest copy

Bookmark and Share SFX Query

All documents in ORBi are protected by a user license.