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

USP
Dehydrated Alcohol, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Triethylamine, for amino acid analysis, ≥99.5% (GC)
Sigma-Aldrich
Triethylamine, BioUltra, ≥99.5% (GC)
Sigma-Aldrich
Heptane, anhydrous, 99%
Sigma-Aldrich
Triethylamine, ≥99.5%
Sigma-Aldrich
Triethylamine, puriss. p.a., ≥99.5% (GC)
Sigma-Aldrich
Triethylamine, ≥99.5%
Sigma-Aldrich
Triethylamine, ≥99%
Sigma-Aldrich
Methanol solution, NMR reference standard, 4% in methanol-d4 (99.8 atom % D), NMR tube size 3 mm × 8 in.
Sigma-Aldrich
Methanol solution, (Methanol:Dimethyl sulfoxide 1:1 (v/v))
Sigma-Aldrich
Triethylamine, for protein sequence analysis, ampule, ≥99.5% (GC)
Supelco
Methanol, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
Methanol, HPLC Plus, ≥99.9%
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Methanol, Absolute - Acetone free
Sigma-Aldrich
Acetic acid, glacial, ACS reagent, ≥99.7%
Sigma-Aldrich
Methanol, ACS spectrophotometric grade, ≥99.9%
Sigma-Aldrich
Acetic acid solution, suitable for HPLC
Sigma-Aldrich
Methanol, Laboratory Reagent, ≥99.6%
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Methanol, ACS reagent, ≥99.8%
Sigma-Aldrich
Acetic acid, glacial, ≥99.99% trace metals basis
Supelco
Triethylamine, analytical standard
Sigma-Aldrich
Methanol, BioReagent, ≥99.93%
Sigma-Aldrich
Methanol, suitable for HPLC, ≥99.9%
Sigma-Aldrich
Acetic acid, glacial, ReagentPlus®, ≥99%
Sigma-Aldrich
Methanol, suitable for HPLC, gradient grade, suitable as ACS-grade LC reagent, ≥99.9%
Supelco
Acetic acid, analytical standard
Supelco
Fipronil, PESTANAL®, analytical standard