玉屏风口服液多糖特征降解谱的建立和应用

Establishment and application of polysaccharide characteristic degradation profile for Yupingfeng oral liquid

建立了玉屏风口服液多糖(YPF-P)的特征降解谱,并基于此完善该制剂的质量控制,通过体积分数70%乙醇溶液沉淀得到YPF-P,同时去除口服液中的辅料蔗糖.优化的YPF-P部分降解条件为0.5 mol/L盐酸溶液,温度80℃,时间4 h,随后采用毛细管区带电泳法(CZE)对经过1-苯基-3-甲基-5-吡唑啉酮(PMP)衍生后的YPF-P部分降解产物进行测定.CZE条件为未涂层熔融石英毛细管柱(50 cm×50μm i.d.,有效长度41 cm),运行缓冲液40 mmol/L硼砂缓冲液(pH 10.1),检测波长245 nm,运行电压10 kV,重力进样15 cm×20 s,柱温为室温.根据L 9(34)正交设计组合不同来源的玉屏风处方药材,制备9份玉屏风模拟样品,采用中位数法综合各特征降解谱得到YPF-P特征降解谱对照谱图,并对不同批次样品YPF-P特征降解谱进行聚类分析.结果表明:不同来源和组合的YPF-P特征降解谱差异显著,证明多糖特征降解谱可用于YPF-P成分的分析,也可为其他中药复方制剂多糖成分质量控制的深入研究提供参考.

The characteristic degradation profile of Yupingfeng oral liquid polysaccharide(YPF-P)was established in this paper,and the quality control of this preparation was improved based on the profile.YPF-P was obtained by the precipitation of 70%ethanol solution,and the excipient sucrose in the oral liquid was removed in the meantime.The optimized partial degradation conditions of YPF-P were as follows:0.5 mol/L hydrochloric acid solution,temperature 80℃,time 4 h.The degradation products derived by 1-phenyl-3-methyl-5-pyrazolinone(PMP)were separated by capillary zone electrophoresis(CZE)under the following conditions:uncoated fused silica capillary column(50 cm×50μm i.d.,effective length 41 cm)was used,and the running buffer was 40 mmol/L borax buffer(pH 10.1),detection wavelength was set at 245 nm with operating voltage 10 kV,gravity injection 15 cm×20 s was employed,and the column temperature was room temperature.According to the L 9(34)orthogonal design,nine Yupingfeng simulated samples were prepared by combining the prescription medicinal materials with different sources of Yupingfeng.The reference YPF-P characteristic degradation profile was obtained by synthesizing the above nine profiles using median method,and the cluster analysis of the characteristic degradation profiles of YPF-P from different batches was carried on.The results indicated that the characteristic degradation profiles of YPF-P from different batches and simulated samples were significantly different,which proved that the characteristic degradation profiles of polysaccharide could be used for the analysis of YPF-P,and could also provide reference for the in-depth study of the quality control of polysaccharide in other Chinese herbal medicine compound preparations.