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[Chiral two-phase synergistic effect in high performance liquid chromatography].

Lei Meng, Fanglou Li, Li‐Ming Yuan

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Abstract

Cellulose tribenzoate (CTB) and cellulose triphenylcarbamate (CTPC) were synthesized for the coating of high performance liquid chromatographic stationary phases. Elemental analysis and IR spectra indicated that most of the hydroxy groups of the microcrystalline cellulose had been converted into ester groups. The silanized gel was coated with CTB/CTPC by using tetrahydrofuran as solvent. The enantiomeric resolutions of phenylalanine (flow rate: 0.5 mL/min) and tryptophan were carried out with a hexane/2-propanol (9:1, v/v) mixture at 25 degrees C, when beta-cyclodextrin (beta-CD), dimethyl-beta-cyclodextrin (DM-beta-CD) and trimethyl-beta-cyclodextrin (TM-beta-CD) were used as mobile phase additives. The results showed that TM-beta-CD at the concentrations higher than 0.60 mmol/L had an explicit chiral two-phase synergistic effect with chiral stationary phase, but beta-CD and DM-beta-CD at any concentrations and TM-beta-CD at low concentrations had no effect.

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What this paper is about

Cellulose tribenzoate (CTB) and cellulose triphenylcarbamate (CTPC) were synthesized for the coating of high performance liquid chromatographic stationary phases. Elemental analysis and IR spectra indicated that most of the hydroxy groups of the microcrystalline cellulose had been converted into ester groups. The silanized gel was coated with CTB/CTPC by using tetrahydrofuran as solvent. The enantiomeric resolutions of phenylalanine (flow rate: 0.5 mL/min) and tryptophan were carried out with a hexane/2-propanol (9:1, v/v) mixture at 25 degrees C, when beta-cyclodextrin (beta-CD), dimethyl-beta-cyclodextrin (DM-beta-CD) and trimethyl-beta-cyclodextrin (TM-beta-CD) were used as mobile phase additives. The results showed that TM-beta-CD at the concentrations higher than 0.60 mmol/L had an explicit chiral two-phase synergistic effect with chiral stationary phase, but beta-CD and DM-beta-CD at any concentrations and TM-beta-CD at low concentrations had no effect.

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Available abstract

Cellulose tribenzoate (CTB) and cellulose triphenylcarbamate (CTPC) were synthesized for the coating of high performance liquid chromatographic stationary phases. Elemental analysis and IR spectra indicated that most of the hydroxy groups of the microcrystalline cellulose had been converted into ester groups. The silanized gel was coated with CTB/CTPC by using tetrahydrofuran as solvent. The enantiomeric resolutions of phenylalanine (flow rate: 0.5 mL/min) and tryptophan were carried out with a hexane/2-propanol (9:1, v/v) mixture at 25 degrees C, when beta-cyclodextrin (beta-CD), dimethyl-beta-cyclodextrin (DM-beta-CD) and trimethyl-beta-cyclodextrin (TM-beta-CD) were used as mobile phase additives. The results showed that TM-beta-CD at the concentrations higher than 0.60 mmol/L had an explicit chiral two-phase synergistic effect with chiral stationary phase, but beta-CD and DM-beta-CD at any concentrations and TM-beta-CD at low concentrations had no effect.

Key concepts: Chemistry, High-performance liquid chromatography, Microcrystalline cellulose, Cyclodextrin, Cellulose, Chromatography, Enantiomer, BETA (programming language)

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