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  • Enantioseparation of basic chiral compounds on a clindamycin phosphate-silica/zirconia hybrid monolith by capillary electrochromatography.

Enantioseparation of basic chiral compounds on a clindamycin phosphate-silica/zirconia hybrid monolith by capillary electrochromatography.

Journal of chromatography. A (2014-07-20)
Le Ngoc Tran, Shuchi Dixit, Jung Hag Park
ABSTRACT

An organic-inorganic silica/zirconia hybrid monolithic capillary column was prepared by sol-gel process in a fused-silica capillary by using triethoxysilylpropylcarbamate (TEOSPC) derivative of clindamycin phosphate (CLIP) as a chiral selector. A sol solution consisting of 6 × 10(-3)M of polyethylene glycol, 1 M of water, 2M of acetic acid and 0.04/0.96 ratio of CLIP-TEOSPC/Zr-Bu resulted in homogeneous monolith having well defined through-pores and tightly anchored to the capillary wall. The column was employed for capillary electrochromatographic enantioseparation of eight basic chiral drugs in mobile phases consisting of acetonitrile, methanol and ammonium acetate (AA, as the electrolyte). Effects of the compositions of solvents and electrolyte in the mobile phase, applied voltage and capillary temperature on chiral separation were investigated. The highest resolution values were obtained with mobile phases consisting of 40/60 MeOH/ACN and 100 mM AA (for citalopram, Tröger's base, indapamide, metoprolol, cetirizine and atropine) and 35/65 MeOH/ACN and 100 mM AA (for sertraline and propranolol) using -10 kV applied voltage at 25 °C.

MATERIALS
Product Number
Brand
Product Description

Lysine hydrochloride, European Pharmacopoeia (EP) Reference Standard
Sigma-Aldrich
Methanol, NMR reference standard
Zirconium, rod, 1000mm, diameter 3.0mm, centerless ground, 99.2%
Zirconium, rod, 100mm, diameter 12.7mm, centerless ground, 99.2%
Zirconium, wire reel, 1m, diameter 0.28mm, annealed, 99.2%
Zirconium, rod, 100mm, diameter 19.0mm, centerless ground, 99.2%
Zirconium, tube, 200mm, outside diameter 2.0mm, inside diameter 1.6mm, wall thickness 0.2mm, annealed, 99.2%
Zirconium, foil, not light tested, 50x50mm, thickness 0.006mm, 99.2%
Zirconium, wire reel, 5m, diameter 0.25mm, as drawn, 99.2%
Zirconium, rod, 1000mm, diameter 1.5mm, 99.2%
Zirconium, rod, 100mm, diameter 2.0mm, centerless ground, 99.2%
Zirconium, tube, 200mm, outside diameter 6.35mm, inside diameter 4.55mm, wall thickness 0.9mm, annealed, 99.2%
Zirconium, rod, 500mm, diameter 9.5mm, centerless ground, 99.2%
Zirconium, rod, 200mm, diameter 1.5mm, 99.2%
Zirconium, wire reel, 5m, diameter 0.28mm, annealed, 99.2%
Zirconium, wire reel, 10m, diameter 0.25mm, as drawn, 99.2%
Zirconium, tube, 100mm, outside diameter 1.6mm, inside diameter 1.1mm, wall thickness 0.25mm, hard, 99.2%
Zirconium, rod, 200mm, diameter 5.0mm, centerless ground, 99.2%
Zirconium, rod, 1000mm, diameter 9.5mm, centerless ground, 99.2%
Zirconium, rod, 500mm, diameter 2.0mm, centerless ground, 99.2%
Zirconium, tube, 500mm, outside diameter 1.6mm, inside diameter 1.1mm, wall thickness 0.25mm, hard, 99.2%
Zirconium, sponge, 50g, max. size 25mm, 99.2%
Zirconium, rod, 200mm, diameter 12.7mm, centerless ground, 99.2%
Zirconium, wire reel, 5m, diameter 0.5mm, as drawn, 99.2%
Zirconium, rod, 1000mm, diameter 5.0mm, centerless ground, 99.2%
Zirconium, rod, 1000mm, diameter 6.0mm, centerless ground, 99.2%
Zirconium, rod, 1000mm, diameter 12.7mm, centerless ground, 99.2%
Zirconium, rod, 1000mm, diameter 2.0mm, centerless ground, 99.2%
Supelco
1-Butanol, Pharmaceutical Secondary Standard; Certified Reference Material
Zirconium, foil, 150x150mm, thickness 0.125mm, annealed, 99.2%