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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
Triphenylene, 98%
Sigma-Aldrich
Hydroquinone, ReagentPlus®, 99%
Sigma-Aldrich
2,2,4-Trimethylpentane, anhydrous, 99.8%
Sigma-Aldrich
Methacryloyl chloride, 97%, contains monomethyl ether hydroquinone as stabilizer
Sigma-Aldrich
Hydroquinone, meets USP testing specifications
Sigma-Aldrich
3-(Trimethoxysilyl)propyl methacrylate, ≥97%
Sigma-Aldrich
Hydroquinone, ReagentPlus®, ≥99%
Supelco
2,2,4-Trimethylpentane, analytical standard
Triphenylene, BCR®, certified reference material
Sigma-Aldrich
3-(Trimethoxysilyl)propyl methacrylate, 98%
Supelco
Hydroquinone, certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland
Supelco
Hydroquinone, Pharmaceutical Secondary Standard; Certified Reference Material
Sigma-Aldrich
2,2,4-Trimethylpentane, HPLC Plus, for HPLC, GC, and residue analysis, ≥99.5%
USP
Hydroquinone, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
2,2,4-Trimethylpentane, ACS reagent, ≥99.0%
Sigma-Aldrich
Cholesterol, Sigma Grade, ≥99%
Sigma-Aldrich
Cholesterol, from sheep wool, ≥92.5% (GC), powder
Sigma-Aldrich
Cholesterol, powder, BioReagent, suitable for cell culture, ≥99%
Sigma-Aldrich
1-[2-(Trifluoromethyl)phenyl]imidazole
Sigma-Aldrich
Triethylamine, ≥99.5%
Sigma-Aldrich
Triethylamine, ≥99%
Sigma-Aldrich
2,2′-Azobis(2-methylpropionitrile) solution, 0.2 M in toluene
Supelco
Cholesterol solution, certified reference material, 10 mg/mL in chloroform
Sigma-Aldrich
SyntheChol® NS0 Supplement, 500 ×, synthetic cholesterol, animal component-free, aqueous solution, sterile-filtered, suitable for cell culture
Sigma-Aldrich
Triethylamine, ≥99.5%
Sigma-Aldrich
o-Terphenyl, 99%
Sigma-Aldrich
Trimethylolpropane trimethacrylate, contains 250 ppm monomethyl ether hydroquinone as inhibitor, technical grade
Sigma-Aldrich
Triethylamine, for amino acid analysis, ≥99.5% (GC)
Sigma-Aldrich
Triethylamine, BioUltra, ≥99.5% (GC)
Sigma-Aldrich
Triethylamine, puriss. p.a., ≥99.5% (GC)