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

USP
Methyl alcohol, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Acetonitrile, suitable for HPLC, gradient grade, ≥99.9%
USP
Glacial acetic acid, United States Pharmacopeia (USP) Reference Standard
Clindamycin hydrochloride, European Pharmacopoeia (EP) Reference Standard
USP
Residual Solvent Class 2 - Acetonitrile, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Acetonitrile, suitable for DNA synthesis, ≥99.9% (GC)
Sigma-Aldrich
Acetonitrile, biotech. grade, ≥99.93%
Sigma-Aldrich
Acetonitrile, suitable for HPLC-GC, ≥99.8% (GC)
Sigma-Aldrich
Acetonitrile, for HPLC, for UV, ≥99.9% (GC)
Sigma-Aldrich
Acetonitrile, suitable for HPLC, gradient grade, ≥99.9%
Sigma-Aldrich
Acetonitrile, ACS reagent, ≥99.5%
Sigma-Aldrich
Acetonitrile, ReagentPlus®, 99%
Sigma-Aldrich
Acetonitrile, for chromatography
Sigma-Aldrich
Acetonitrile, ≥99.8%, for residue analysis, JIS 300
Sigma-Aldrich
Acetonitrile, SAJ first grade, ≥99.0%
Sigma-Aldrich
L-Lysine monohydrochloride, SAJ special grade, ≥99.0%
Sigma-Aldrich
Acetonitrile, ≥99.8%, for residue analysis, JIS 1000
Sigma-Aldrich
Acetonitrile, ≥99.8%, suitable for HPLC
Sigma-Aldrich
Acetonitrile, JIS special grade, ≥99.5%
Sigma-Aldrich
Acetonitrile, for residue analysis, JIS 5000
Clindamycin phosphate, European Pharmacopoeia (EP) Reference Standard
Sigma-Aldrich
Acetonitrile, electronic grade, 99.999% trace metals basis
USP
Clindamycin hydrochloride, United States Pharmacopeia (USP) Reference Standard
Lysine hydrochloride, European Pharmacopoeia (EP) Reference Standard
Sigma-Aldrich
Zirconium(IV) oxide, 99.99% trace metals basis (purity excludes ~2% HfO2)
Sigma-Aldrich
LUDOX® TM-50 colloidal silica, 50 wt. % suspension in H2O
Sigma-Aldrich
Zirconium(IV) oxide, powder, 5 μm, 99% trace metals basis
Sigma-Aldrich
LUDOX® AM colloidal silica, 30 wt. % suspension in H2O
Sigma-Aldrich
Zirconium(IV) oxide, nanopowder, <100 nm particle size (TEM)
Supelco
L-Lysine hydrochloride solution, 100 mM amino acid in 0.1 M HCl, analytical standard