Skip to Content
Merck
  • Superficially porous particles vs. fully porous particles for bonded high performance liquid chromatographic chiral stationary phases: isopropyl cyclofructan 6.

Superficially porous particles vs. fully porous particles for bonded high performance liquid chromatographic chiral stationary phases: isopropyl cyclofructan 6.

Journal of chromatography. A (2014-08-30)
Daniel A Spudeit, Maressa D Dolzan, Zachary S Breitbach, William E Barber, Gustavo A Micke, Daniel W Armstrong
ABSTRACT

This work reports a comparison of HPLC separations of enantiomers with chiral stationary phases (CSPs) prepared by chemically bonding cyclofructan-6, functionalized with isopropyl carbamate groups on fully and superficially porous particles (SPPs). The chromatographic performance of the superficially porous CSP based column was compared with columns packed with 5 μm and 3 μm fully porous particles (FPPs). At a flow rate of 3.0 mL/min the number of plates on column afforded by the SPP column was ∼7× greater than the number of plates on column (same length) obtained when using the 5 μm FPP based column. The flow rate providing the highest efficiency separation was ∼1.0 mL/min for the SPP column while it was ∼0.5 mL/min for both FPP columns. It was found that the selectivity and resolution of the separations were comparable between fully porous and superficially porous based columns (under constant mobile phase conditions), even though the SPP column contained lower absolute amounts of chiral selector. When tested under constant retention conditions, the SPP based CSP greatly improved resolution compared to the FPP based columns. At high flow rates the efficiency gained by using superficially porous CSP was accentuated. The advantages of columns based on SPPs become more obvious from the viewpoint of plate numbers and resolution per analysis time.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Acetic acid-12C2, 99.9 atom % 12C
Supelco
Ethanol solution, certified reference material, 2000 μg/mL in methanol
Sigma-Aldrich
Triethylamine, ≥99.5%
Sigma-Aldrich
Heptane, biotech. grade, ≥99%
Sigma-Aldrich
Heptane, anhydrous, 99%
Supelco
Dehydrated Alcohol, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Methanol, NMR reference standard
Supelco
Fipronil, certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland
Supelco
Residual Solvent - Toluene, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Toluene, suitable for HPLC, ≥99.8%
Sigma-Aldrich
Toluene, LR, ≥99%
Sigma-Aldrich
Toluene, AR, ≥99.5%
Sigma-Aldrich
Heptane, suitable for HPLC, ≥96%
Sigma-Aldrich
Heptane, HPLC Plus, for HPLC, GC, and residue analysis, 99%
Sigma-Aldrich
Toluene, suitable for HPLC, 99.9%
Sigma-Aldrich
Heptane, suitable for HPLC, ≥99%
Sigma-Aldrich
Toluene, HPLC Plus, for HPLC, GC, and residue analysis, ≥99.9%
Sigma-Aldrich
Heptane, puriss. p.a., reag. Ph. Eur., ≥99% n-heptane basis (GC)
Sigma-Aldrich
Toluene, ACS reagent, ≥99.5%
Sigma-Aldrich
Toluene, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥99.7% (GC)
Sigma-Aldrich
Heptane, ReagentPlus®, 99%
Sigma-Aldrich
Toluene, Laboratory Reagent, ≥99.3%
Sigma-Aldrich
Toluene, ACS reagent, ≥99.5%
Sigma-Aldrich
Toluene, ACS reagent, ≥99.5%
Supelco
Residual Solvent - Acetonitrile, Pharmaceutical Secondary Standard; Certified Reference Material
Supelco
Triethylamine, analytical standard
Supelco
Heptane, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Acetic acid, glacial, puriss., meets analytical specification of Ph. Eur., BP, USP, FCC, 99.8-100.5%
Sigma-Aldrich
Methanol solution, (Methanol:Dimethyl sulfoxide 1:1 (v/v))
Sigma-Aldrich
Methanol solution, contains 0.50 % (v/v) triethylamine