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目的:考察毛细管区带电泳法(CZE)中各种因素对β-环糊精衍生物手性分离三唑类化合物的影响。方法:采用CZE对5个三唑类化合物的手性分离进行研究。BECKMAN P/ACE System 5 000毛细管电泳仪,紫外检测器。未涂渍熔融石英毛细管50μm×47 cm(有效长度40 cm);正极压力进样50 mbar×3 s,检测波长200 nm。β-环糊精的3种衍生物做为手性添加剂。结果:羧甲醚-β-环糊精为手性选择剂是5个化合物都能达到较好的手性分离,而硫酸酯-β-环糊精和二氟代羧甲醚-β-环糊精对这5个化合物无手性分离能力。在羧甲醚-β-环糊精环境下,优化选择30 mmol/L的NaH2PO4缓冲液含羧甲醚-β-环糊精5 mmol/L,用H3PO4调节pH2.2,温度20℃,电压20 KV,在此条件下5个化合物都能达到良好的手性分离。结论:β-环糊精的种类和缓冲液的pH是影响这5对三唑类对映异构体分离的关键因素。
Objective: To investigate the influence of various factors in capillary zone electrophoresis (CZE) on the chiral separation of triazole compounds by β-cyclodextrin derivatives. Methods: The chiral separation of 5 triazoles was studied by CZE. BECKMAN P / ACE System 5 000 capillary electrophoresis, UV detector. Uncoated fused silica capillary 50 μm × 47 cm (effective length 40 cm); positive pressure injection 50 mbar × 3 s, detection wavelength 200 nm. Three kinds of β-cyclodextrin derivatives as chiral additives. Results: Carboxymethyl ether-β-cyclodextrin as a chiral selector can achieve better chiral separation of all five compounds. However, sulphate-β-cyclodextrin and difluorocarboxymethylether-β-ring Dextrin has no chiral separation ability for these 5 compounds. In carboxymethyl ether-β-cyclodextrin environment, the optimal selection of 30 mmol / L NaH2PO4 buffer containing carboxymethyl ether-β-cyclodextrin 5 mmol / L, with H3PO4 to adjust pH2.2, temperature 20 ℃, voltage 20 KV, under these conditions all five compounds can achieve good chiral separation. Conclusion: The type of β-cyclodextrin and the pH of the buffer are the key factors affecting the separation of the five pairs of enantiomers.