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
Acetonitrile solution, contains 0.1 % (v/v) trifluoroacetic acid, suitable for HPLC
Sigma-Aldrich
Acetonitrile solution, contains 0.05 % (v/v) trifluoroacetic acid
Sigma-Aldrich
Acetic acid-12C2, 99.9 atom % 12C
Sigma-Aldrich
Acetonitrile solution, contains 0.1 % (v/v) formic acid, suitable for HPLC
Sigma-Aldrich
Zirconium, powder, −100 mesh
Sigma-Aldrich
Acetic acid, natural, ≥99.5%, FG
Sigma-Aldrich
LUDOX® SM colloidal silica, 30 wt. % suspension in H2O
Sigma-Aldrich
LUDOX® LS colloidal silica, 30 wt. % suspension in H2O
Sigma-Aldrich
Zirconium, sponge, ≥99% trace metals basis
Sigma-Aldrich
Ammonium acetate, 99.999% trace metals basis
Sigma-Aldrich
Zirconium(IV) oxide, 99.99% trace metals basis (purity excludes ~2% HfO2)
Sigma-Aldrich
Zirconium, rod, diam. 6.35 mm, ≥99% trace metals basis
Supelco
Ammonium acetate, LiChropur, eluent additive for LC-MS
Sigma-Aldrich
LUDOX® TM-40 colloidal silica, 40 wt. % suspension in H2O
Sigma-Aldrich
LUDOX® CL colloidal silica, 30 wt. % suspension in H2O
Sigma-Aldrich
Zirconium(IV) oxide, powder, 5 μm, 99% trace metals basis
Sigma-Aldrich
Zirconium(IV) oxide, nanopowder, <100 nm particle size (TEM)
Sigma-Aldrich
LUDOX® HS-30 colloidal silica, 30 wt. % suspension in H2O
Sigma-Aldrich
Acetic acid, ≥99.5%, FCC, FG
Sigma-Aldrich
Zirconium, foil, thickness 0.1 mm, 99.98% trace metals basis
Sigma-Aldrich
Silica
Sigma-Aldrich
Clindamycin 2-phosphate, aminoglycoside antibiotic
Sigma-Aldrich
Adrenocorticotropic Hormone Fragment 18-39 human, ≥97% (HPLC)
Sigma-Aldrich
Silica, mesostructured, MSU-F (cellular foam)
Sigma-Aldrich
Ammonium acetate, reagent grade, ≥98%
Sigma-Aldrich
Ammonium acetate, for molecular biology, ≥98%
Sigma-Aldrich
Ammonium acetate, BioUltra, for molecular biology, ≥99.0%
Sigma-Aldrich
Ammonium acetate, BioXtra, ≥98%
Sigma-Aldrich
Acetonitrile solution, contains 0.05 % (w/v) ammonium formate, 5 % (v/v) water, 0.1 % (v/v) formic acid, suitable for HPLC
Sigma-Aldrich
Acetonitrile solution, contains 10.0% acetone, 0.05% formic acid, 40.0% 2-propanol