关键词: 玉屏风口服液, 多糖, 特征降解谱, 毛细管区带电泳法, 中药复方制剂

Abstract: 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×50 μm 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 L₉(3⁴)orthogonal design,- DOI:10.3969/j.issn.1000-1565.2023.06.007玉屏风口服液多糖特征降解谱的建立和应用马梦楠¹,张钰¹,李欣珂¹,刘进宝¹,刘丹¹,郭怀忠^1,2(1.河北大学 药学院,河北 保定 071002;2.河北省药物质量分析控制重点实验室,河北 保定 071002)摘 要: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 × 50 μm 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L₉(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.关键词:玉屏风口服液;多糖;特征降解谱;毛细管区带电泳法;中药复方制剂中图分类号:R917 文献标志码:A 文章编号:1000-1565(2023)06-0616-08Establishment and application of polysaccharide characteristic degradation profile for Yupingfeng oral liquidMA Mengnan¹,ZHANG Yu¹,LI Xinke¹,LIU Jinbao¹,LIU Dan¹,GUO Huaizhong^1,2(1. College of Pharmaceutical Sciences, Hebei University, Baoding 071002, China; 2. Key Lab of Pharmaceutical Quality Control of Hebei Province, Baoding 071002, China)Abstract: 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×50 μm 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 L₉(3⁴)orthogonal design,- 收稿日期:2023-01-17 基金项目:河北省自然科学基金资助项目(H2021201018;H2016201221);河北省创新能力计划项目(20567605H) 第一作者:马梦楠(1996—),女,河北石家庄人,河北大学在读硕士研究生.E-mail:mmn_0721@163.com 通信作者:郭怀忠(1968—),男,内蒙古商都人,河北大学教授,博士,主要从事中药质量控制及其药效学方向研究.E-mail: ghuaizh@aliyun.com第6期马梦楠等:玉屏风口服液多糖特征降解谱的建立和应用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.

Key words: Yupingfeng oral liquid, polysaccharide, characteristic degradation profile, capillary zone electrophoresis, Chinese herbal medicine compound preparation