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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%
Supelco
2,2,4-Trimethylpentane, analytical standard
Triphenylene, BCR®, certified reference material
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3-(Trimethoxysilyl)propyl methacrylate, 98%
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Triphenylene, 98%
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Hydroquinone, ReagentPlus®, 99%
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Hydroquinone, meets USP testing specifications
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Hydroquinone, ReagentPlus®, ≥99%
Sigma-Aldrich
3-(Trimethoxysilyl)propyl methacrylate, ≥97%
USP
Hydroquinone, United States Pharmacopeia (USP) Reference Standard
Sigma-Aldrich
2,2,4-Trimethylpentane, suitable for HPLC, ≥99%
Supelco
Hydroquinone, Pharmaceutical Secondary Standard; Certified Reference Material
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Hydroquinone, certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland
Sigma-Aldrich
2,2,4-Trimethylpentane, ACS reagent, ≥99.0%
Sigma-Aldrich
2,2,4-Trimethylpentane, puriss. p.a., ≥99.5% (GC)
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2,2,4-Trimethylpentane, ReagentPlus®, ≥99%
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2,2,4-Trimethylpentane, puriss. p.a., ACS reagent, ≥99.5% (GC)
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2,2,4-Trimethylpentane, HPLC Plus, for HPLC, GC, and residue analysis, ≥99.5%
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Cyclohexane, anhydrous, 99.5%
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Triethylamine, ≥99.5%
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o-Terphenyl, 99%
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Cholesterol solution, certified reference material, 10 mg/mL in chloroform
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Triethylamine, ≥99.5%
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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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Cyclohexane, analytical standard
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Cholesterol, from lanolin, ≥99.0% (GC)
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Triethylamine, puriss. p.a., ≥99.5% (GC)