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[高效液相色谱中的手性两相协同效应]

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

作者信息

Meng Lei, Li Fanglou, Yuan Liming

机构信息

Basic Science College, Henan Agricultural University, Zhengzhou 450002, China.

出版信息

Se Pu. 2004 Mar;22(2):124-7.

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.

摘要

合成了三苯甲酸纤维素酯(CTB)和三苯基氨基甲酸纤维素酯(CTPC)用于高效液相色谱固定相的涂层。元素分析和红外光谱表明微晶纤维素的大部分羟基已转化为酯基。以四氢呋喃为溶剂,用CTB/CTPC对硅烷化凝胶进行涂层。在25℃下,当使用β-环糊精(β-CD)、二甲基-β-环糊精(DM-β-CD)和三甲基-β-环糊精(TM-β-CD)作为流动相添加剂时,用己烷/2-丙醇(9:1,v/v)混合物对苯丙氨酸(流速:0.5 mL/min)和色氨酸进行对映体拆分。结果表明,浓度高于0.60 mmol/L的TM-β-CD与手性固定相具有明显的手性双相协同效应,但任何浓度的β-CD和DM-β-CD以及低浓度的TM-β-CD均无此效应。

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