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目的 :合成β-环糊精硫酸酯并以其作为毛细管电泳手性添加剂对舒必利进行手性拆分研究。方法 :以三氧化硫吡啶复合物作为硫酸酯化试剂合成β-环糊精硫酸酯。以合成的β-环糊精硫酸酯作为手性添加剂利用毛细管电泳对舒必利进行手性拆分。 结果 :对不同反应温度 (6 0、80、10 0、12 0℃ )下产物的纯度进行了初步分析 ,表明在 80℃条件下 ,以吡啶作溶剂、三氧化硫吡啶复合物作为硫酸酯化试剂合成β-环糊精硫酸酯条件易于控制 ,产物纯度较好。用合成的β-环糊精硫酸酯作为毛细管电泳手性添加剂 ,采用未涂渍熔融石英毛细管 5 0μm× 5 8.5 cm (有效长度 5 0 cm) ,优化选择 5 0 m mol/ L Tris缓冲液含 1.3%β-环糊精硫酸酯 (1% H3PO4 溶液调节 p H 3.7) ,温度 2 0℃ ,操作电压 2 4 k V,正极进样 5 0 mbar× 3s(1bar=10 5Pa) ,在检测波长 2 14 nm条件下对舒必利的 D、L -型对映体进行分离 ,结果分离度良好 (Rs>2 .5 )。 结论 :探索得到了一条较为稳定的β-环糊精硫酸酯的合成路线 ,合成的β-环糊精硫酸酯作为毛细管电泳手性添加剂分离舒必利的 D、L -型对映体拆分效果较好。
OBJECTIVE: To synthesize β-cyclodextrin sulfate and use it as a chiral additive for capillary electrophoresis for the chiral resolution of sulpiride. Methods: β-Cyclodextrin sulfate was synthesized by using sulfur trioxide pyridine complex as sulfation agent. Sulpiride was resolved by capillary electrophoresis with synthetic β-cyclodextrin sulfate as a chiral additive. Results: The purity of the products at different reaction temperatures (60, 80, 100, 120 ℃) was analyzed preliminarily. The results showed that pyridine as solvent and sulfur trioxide pyridine complex as sulfuric acid esterification Β-Cyclodextrin reagent synthesis reagent conditions easy to control, product purity is better. The synthesized β-cyclodextrin sulfate was used as a chiral additive in capillary electrophoresis. The uncoated fused silica capillary tube (50 μm × 5 8.5 cm, effective length 50 cm) was used to optimize the 50 mol / L Tris buffer solution 1.3% β-cyclodextrin sulfate (adjusted to pH 3.7 with 1% H3PO4 solution), temperature 20 ° C, operating voltage 24 kV, positive injection 50 mbar x 3 s (1 bar = 105 Pa) The D and L - enantiomers of sulpiride were separated at 2-14 nm with good resolution (Rs> 2.5). CONCLUSION: The synthesis route of β-cyclodextrin sulfate has been explored, and the resolution of D, L-enantiomers of the synthesized compound β-cyclodextrin sulfate as a chiral additive by capillary electrophoresis has been achieved. it is good.