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目的:对高效毛细管电泳法拆分25R、25S-鲁斯可皂苷元混合物的条件进行探讨,以建立一种快速测定鲁斯可皂苷元差向异构体比例的方法。方法:以羟丙基-β-环糊精作为手性添加剂,考察分离电压、缓冲液pH、离子浓度、环糊精浓度对25R、25S-鲁斯可皂苷元拆分的影响。结果:从湖北麦冬制备分离的鲁斯可皂苷元,NMR、IR检测结果显示其是以25 S构型为主要成分、25R和25S 2个差向异构体并存的混合物。以0.018 mol·L-1的羟丙基-β-环糊精为手性添加剂,分离电压6.0 kV,0.075 mol·L-1的pH=10.0磷酸氢二钠缓冲液,25R与25S-鲁斯可皂苷元可实现基线分离(分离度1.52±0.13),在此条件下,测得制备的鲁斯可皂苷元中25 R、25 S异构体含量比为25.4∶74.6。结论:高效毛细管电泳法可用于25R与25S-鲁斯克皂苷元手性拆分。研究结果为鲁斯可皂苷元药理学研究、鲁斯可皂苷元质量控制提供新方法。
OBJECTIVE: To investigate the conditions for the separation of 25R, 25S-russetapogenin mixtures by high performance capillary electrophoresis to establish a rapid method for the determination of russetapogenin epimer. Methods: The hydroxypropyl-β-cyclodextrin was used as a chiral additive to investigate the effects of voltage, buffer pH, ionic strength and cyclodextrin concentration on the resolution of 25R and 25S-russetapine. Results: The results showed that russetaponin isolated from Radix Ophiopogonis was separated and identified by NMR and IR. The results showed that it was a mixture of 25 S and 25 S 2 epimer. With 0.018 mol·L-1 of hydroxypropyl-β-cyclodextrin as chiral additive, 6.0 kV and 0.075 mol·L-1 of pH = 10.0 dibasic sodium phosphate buffer were separated, and 25R and 25S- Sapogenin was able to achieve baseline separation (resolution 1.52 ± 0.13). Under these conditions, the content ratio of 25 R, 25 S isomers in the manufactured ruscogenin was 25.4: 74.6. Conclusion: High performance capillary electrophoresis can be used for the chiral resolution of 25R and 25S-Rusk sapogenin. The results provide a new method for the quality control of russetaponin and the quality control of russetapogenin.