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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
2,2,4-Trimethylpentane, anhydrous, 99.8%
Sigma-Aldrich
Methacryloyl chloride, 97%, contains monomethyl ether hydroquinone as stabilizer
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3-(Trimethoxysilyl)propyl methacrylate, 98%
Sigma-Aldrich
Hydroquinone, ReagentPlus®, 99%
Sigma-Aldrich
Triphenylene, 98%
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Hydroquinone, meets USP testing specifications
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Hydroquinone, ReagentPlus®, ≥99%
Sigma-Aldrich
3-(Trimethoxysilyl)propyl methacrylate, ≥97%
Supelco
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Triphenylene, BCR®, certified reference material
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Hydroquinone, certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland
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2,2,4-Trimethylpentane, HPLC Plus, for HPLC, GC, and residue analysis, ≥99.5%
Supelco
Hydroquinone, Pharmaceutical Secondary Standard; Certified Reference Material
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2,2,4-Trimethylpentane, ACS reagent, ≥99.0%
USP
Hydroquinone, United States Pharmacopeia (USP) Reference Standard
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SyntheChol® NS0 Supplement, 500 ×, synthetic cholesterol, animal component-free, sterile-filtered, aqueous solution, suitable for cell culture
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o-Terphenyl, 99%
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Triethylamine, ≥99.5%
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Triethylamine, puriss. p.a., ≥99.5% (GC)
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Triethylamine, for amino acid analysis, ≥99.5% (GC)
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Triethylamine, BioUltra, ≥99.5% (GC)
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Cholesterol, tested according to Ph. Eur.
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2,2′-Azobis(2-methylpropionitrile), 98%
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Trimethylolpropane trimethacrylate, contains 250 ppm monomethyl ether hydroquinone as inhibitor, technical grade
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2,2′-Azobis(2-methylpropionitrile), purum, ≥98.0% (GC)
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Cholesterol, Sigma Grade, ≥99%
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Cholesterol, from sheep wool, ≥92.5% (GC), powder
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