Skip to Content
Merck
  • 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

Millipore
Bifido Selective Supplement B, suitable for microbiology
Sigma-Aldrich
Zirconium(IV) oxide, nanoparticles, dispersion, <100 nm particle size (BET), 5 wt. % in H2O
Sigma-Aldrich
Zirconium(IV) oxide, nanoparticles, dispersion, <100 nm particle size (BET), 10 wt. % in H2O
Supelco
Methanol, analytical standard
Sigma-Aldrich
Ammonium acetate solution, BioUltra, for molecular biology, ~5 M in H2O
Sigma-Aldrich
1-Butanol, for molecular biology, ≥99%
Sigma-Aldrich
Ammonium acetate solution, for molecular biology, 7.5 M
Supelco
Acetic acid, analytical standard
Sigma-Aldrich
Acetic acid, for luminescence, BioUltra, ≥99.5% (GC)
Sigma-Aldrich
1-Butanol, anhydrous, 99.8%
USP
Glacial acetic acid, United States Pharmacopeia (USP) Reference Standard
USP
Methyl alcohol, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
5α-Androstan-17β-ol-3-one, ≥97.5%
Supelco
Acetonitrile, analytical standard
Sigma-Aldrich
L-Lysine monohydrochloride, BioUltra, ≥99.5% (AT)
Sigma-Aldrich
L-Lysine monohydrochloride, from non-animal source, meets EP, JP, USP testing specifications, suitable for cell culture, 98.5-101.0%
Sigma-Aldrich
L-Lysine monohydrochloride, reagent grade, ≥98% (HPLC)
Sigma-Aldrich
Methanol, NMR reference standard
Supelco
5α-Androstan-17β-ol-3-one, VETRANAL®, analytical standard
Supelco
L-Lysine monohydrochloride, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Clindamycin Phosphate, Pharmaceutical Secondary Standard; Certified Reference Material
USP
Residual Solvent Class 2 - Acetonitrile, United States Pharmacopeia (USP) Reference Standard
Clindamycin phosphate, European Pharmacopoeia (EP) Reference Standard
Supelco
Methanol, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
1-Butanol, suitable for HPLC, ≥99.7%
Sigma-Aldrich
Acetonitrile, suitable for HPLC, gradient grade, ≥99.9%
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Acetic acid, glacial, ACS reagent, ≥99.7%
Sigma-Aldrich
Methanol, Absolute - Acetone free