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  • Cholesterol-based polymeric monolithic columns for capillary liquid chromatography.

Cholesterol-based polymeric monolithic columns for capillary liquid chromatography.

Journal of chromatography. A (2014-12-04)
Michał Szumski, Damian Grzywiński, Bogusław Buszewski
ABSTRACT

A novel, cholesterol-based polymeric monolithic stationary phase for capillary liquid chromatography, was prepared by thermally initiated in-situ polymerization. Cholesteryl methacrylate (CholMA) was used as a functional monomer and trimethylolpropane trimethacrylate (TRIM) was a cross-linker, while azobisisobutyronitrile (AIBN) was an initiator. Isooctane and toluene were chosen as "poor" and "good" solvent, respectively, as constituents of the porogen solvent. Isocratic elutions of alkylbenzenes and separation of the testing mixture of o-terphenyl and triphenylene were conducted for all of the monoliths to assess their hydrophobicity and planar selectivity characteristic for cholesterol-based stationary phases. The synthesized columns demonstrated efficiency exceeding N=10,000 plates and a plate height of ca. H=30 μm. Column preparation was found to be highly reproducible; the relative standard deviation (RSD) values (n=3) for day-to-day and column-to-column were less than 4.08 and 2.02%, respectively, based on retention factor of alkylbenzenes.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
3-(Trimethoxysilyl)propyl methacrylate, 98%
Sigma-Aldrich
Hydroquinone, ReagentPlus®, 99%
Sigma-Aldrich
Hydroquinone, meets USP testing specifications
Sigma-Aldrich
Hydroquinone, ReagentPlus®, ≥99%
Sigma-Aldrich
2,2,4-Trimethylpentane, HPLC Plus, for HPLC, GC, and residue analysis, ≥99.5%
Triphenylene, BCR®, certified reference material
Sigma-Aldrich
2,2,4-Trimethylpentane, suitable for HPLC, ≥99%
Supelco
Hydroquinone, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
2,2,4-Trimethylpentane, ACS reagent, ≥99.0%
USP
Hydroquinone, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
Triethylamine, ≥99.5%
Sigma-Aldrich
Triethylamine, puriss. p.a., ≥99.5% (GC)
Sigma-Aldrich
Triethylamine, BioUltra, ≥99.5% (GC)
Supelco
Cyclohexane, analytical standard
Sigma-Aldrich
Cholesterol, Sigma Grade, ≥99%
Sigma-Aldrich
Triethylamine, ≥99.5%
Sigma-Aldrich
Triethylamine, ≥99%
Sigma-Aldrich
Cholesterol, from sheep wool, ≥92.5% (GC), powder
Sigma-Aldrich
Cyclohexane, ACS reagent, ≥99%
Sigma-Aldrich
Cyclohexane, suitable for HPLC, ≥99.7%
Sigma-Aldrich
Cyclohexane, suitable for HPLC, ≥99.9%
Supelco
Cholesterol, Pharmaceutical Secondary Standard; Certified Reference Material