Skip to Content
MilliporeSigma
  • 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

Sigma-Aldrich
5α-Androstan-17β-ol-3-one, ≥97.5%
Sigma-Aldrich
Clindamycin hydrochloride, lincosamide antibiotic
USP
Clindamycin hydrochloride, United States Pharmacopeia (USP) Reference Standard
Supelco
Clindamycin hydrochloride, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Methanol solution, NMR reference standard, 4% in methanol-d4 (99.8 atom % D), NMR tube size 3 mm × 8 in.
Sigma-Aldrich
Acetonitrile, ≥99.8%, for residue analysis, JIS 1000
Sigma-Aldrich
Acetonitrile, ≥99.8%, suitable for HPLC
Sigma-Aldrich
Acetonitrile, HPLC Plus, ≥99.9%, poly-coated bottles
Supelco
L-Lysine monohydrochloride, certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland
Supelco
Methanol solution, contains 0.10 % (v/v) formic acid, UHPLC, suitable for mass spectrometry (MS), ≥99.5%
Sigma-Aldrich
Zirconium(IV) oxide, nanoparticles, dispersion, <100 nm particle size (BET), 10 wt. % in H2O
Sigma-Aldrich
Zirconium(IV) oxide, nanoparticles, dispersion, <100 nm particle size (BET), 5 wt. % in H2O
Sigma-Aldrich
Acetonitrile, electronic grade, 99.999% trace metals basis
USP
Clindamycin phosphate, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Zirconium(IV) oxide, nanopowder, <100 nm particle size (TEM)
Sigma-Aldrich
Acetonitrile, ≥99.5%, ACS reagent
Sigma-Aldrich
LUDOX® CL-X colloidal silica, 45 wt. % suspension in H2O
Sigma-Aldrich
LUDOX® HS-40 colloidal silica, 40 wt. % suspension in H2O
Supelco
Acetonitrile, HPLC grade, ≥99.93%
Sigma-Aldrich
Zirconium(IV) oxide, powder, 5 μm, 99% trace metals basis
Supelco
5α-Androstan-17β-ol-3-one, VETRANAL®, analytical standard
Supelco
L-Lysine hydrochloride solution, 100 mM amino acid in 0.1 M HCl, analytical standard
Sigma-Aldrich
Zirconium(IV) oxide, 99.99% trace metals basis (purity excludes ~2% HfO2)
Sigma-Aldrich
L-Lysine monohydrochloride, SAJ special grade, ≥99.0%
Sigma-Aldrich
Acetonitrile, ≥99.8%, for residue analysis, JIS 300
Sigma-Aldrich
Acetonitrile, for residue analysis, JIS 5000
Sigma-Aldrich
Acetonitrile, for chromatography
Sigma-Aldrich
Acetonitrile, JIS special grade, ≥99.5%
Sigma-Aldrich
Acetonitrile, SAJ first grade, ≥99.0%
Supelco
Clindamycin Phosphate, Pharmaceutical Secondary Standard; Certified Reference Material