Separation strategy for acidic chiral pharmaceuticals with capillary electrochromatography on polysaccharide stationary phases.
The effect of five factors on the capillary electrochromatographic enantioseparation of acidic compounds was studied using an experimental design. The studied factors were pH, acetonitrile content in the mobile phase, temperature, buffer concentration, and applied voltage. These experiments allowed defining a generic separation strategy applicable on acidic compounds with chemical and structural diversity. The starting screening conditions consist of a 45 mM ammonium formate electrolyte at pH 2.9 mixed with 65% acetonitrile, an applied voltage of 15 kV, and a temperature of 25 degrees C. The screening phase occasionally can be followed by an optimization procedure. Evaluation of the proposed strategy pointed out that it allows achieving baseline resolution within a relatively short time when a beginning of separation is obtained at the starting conditions. This strategy revealed enantioselectivity for 11 compounds out of 15, of which 10 could be baseline-separated after the proposed optimization steps.
Mangelings
Debby
D
Department of Pharmaceutical and Biomedical Analysis, Pharmaceutical Institute, Vrije Universiteit Brussel-VUB, Brussels, Belgium.
Tanret
Indiana
I
Department of Pharmaceutical and Biomedical Analysis, Pharmaceutical Institute, Vrije Universiteit Brussel-VUB, Brussels, Belgium.
Matthijs
Nele
N
Department of Pharmaceutical and Biomedical Analysis, Pharmaceutical Institute, Vrije Universiteit Brussel-VUB, Brussels, Belgium.
Maftouh
Mohamed
M
Discovery Analytical Department, Sanofi-Synthelabo Recherche, Toulouse, France.
Massart
D Luc
DL
Vander Heyden
Yvan
Y
Department of Pharmaceutical and Biomedical Analysis, Pharmaceutical Institute, Vrije Universiteit Brussel-VUB, Brussels, Belgium.
D000097:Acetonitriles; D002021:Buffers; D020374:Chromatography, Micellar Electrokinetic Capillary / Q000379:methods*; D019075:Electrophoresis, Capillary; D005480:Flurbiprofen / Q000302:isolation & purification; D006591:Hexobarbital / Q000302:isolation & purification; D006863:Hydrogen-Ion Concentration; D007052:Ibuprofen / Q000302:isolation & purification; D004364:Pharmaceutical Preparations / Q000302:isolation & purification*; D011134:Polysaccharides; D013237:Stereoisomerism; D013696:Temperature; D014859:Warfarin / Q000302:isolation & purification
D000097:Acetonitriles; D002021:Buffers; D004364:Pharmaceutical Preparations; D011134:Polysaccharides; D005480:Flurbiprofen; D014859:Warfarin; D006591:Hexobarbital; D007052:Ibuprofen; C032159:acetonitrile
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