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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

Supelco
Density Standard 692 kg/m3, H&D Fitzgerald Ltd. Quality
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
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o-Terphenyl, 99%
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Triethylamine, for protein sequence analysis, ampule, ≥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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Triethylamine, ≥99.5%
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Trimethylolpropane trimethacrylate, contains 250 ppm monomethyl ether hydroquinone as inhibitor, technical grade
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Triethylamine, puriss. p.a., ≥99.5% (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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1-[2-(Trifluoromethyl)phenyl]imidazole
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2,2′-Azobis(2-methylpropionitrile) solution, 0.2 M in toluene
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Cholesterol, powder, BioReagent, suitable for cell culture, ≥99%
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Triethylamine, ≥99%
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Triethylamine, ≥99.5%
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Cholesterol, Pharmaceutical Secondary Standard; Certified Reference Material
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Cyclohexane, ACS reagent, ≥99%
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Cyclohexane, ACS reagent, ≥99%
SAFC
Cholesterol, from sheep wool, Controlled origin, meets USP/NF testing specifications
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Cyclohexane, suitable for HPLC, ≥99.9%
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Hydroquinone, certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland
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Triphenylene, 98%
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Methacryloyl chloride, 97%, contains ~200 ppm monomethyl ether hydroquinone as stabilizer
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3-(Trimethoxysilyl)propyl methacrylate, 98%