复方南板蓝根颗粒中多糖的含量测定及单糖组成分析  

Determination of content and compositional monosaccharide of polysaccharides from compound Nanbanlangen granules

作　　者：张利沙 孙玮玮 徐自慧 郭怀忠[1,2] ZHANG Li-sha SUN Wei-wei XU Zi-hui GUO Huai-zhong(School of Pharmacy, Hebei University, Baoding 071002, China Key Laboratory of Medicinal Chemistry and Molecular Diagnosis, Ministry＂ of Education, Hebei University, Baoding 071002, China)

机构地区：[1]河北大学药学院,保定071002 [2]药物化学与分子诊断教育部重点实验室河北大学,保定071002

出　　处：《药物分析杂志》2017年第10期1845-1850,共6页Chinese Journal of Pharmaceutical Analysis

基　　金：河北省自然科学基金项目(No.H2016201221);国家自然科学基金项目(No.21575033)

摘　　要：目的:测定复方南板蓝根颗粒中多糖的含量及其单糖组成。方法:采用硫酸-苯酚法测定多糖含量;测定条件:5%苯酚溶液1 m L,硫酸5 m L,检测波长490 nm。设计正交试验对该制剂中多糖全降解条件进行优化;以1-苯基-3-甲基-5-吡唑啉酮(PMP)为衍生试剂,采用毛细管区带电泳法,分析其单糖组成;电泳条件:未涂层弹性石英毛细管柱(52 cm×50μm,有效长度43 cm),运行缓冲液40 mmol·L^(-1)硼砂缓冲液(pH 10.1),检测波长245 nm,运行电压12 k V,进样量8 cm×10 s。结果:测得该制剂中多糖含量为1.708%~1.828%;多糖全降解的最优条件为硫酸浓度0.75 mol·L^(-1),温度100℃,时间5 h;其单糖组成为木糖、阿拉伯糖、葡萄糖、鼠李糖、甘露糖、半乳糖、葡萄糖醛酸和半乳糖醛酸。对所建立的毛细管区带电泳法进行方法学验证,结果显示其精密度RSD≤3.8%,重复性RSD≤5.5%,并且稳定性满足要求,回收率结果显示:半乳糖和半乳糖醛酸的平均回收率分别为99.7%~106.9%和94.8%~102.5%,其RSD分别为2.4%~4.9%和1.7%~4.6%。结论:本文为复方南板蓝根颗粒中多糖的测定及其质量标准的完善提供参考。Objective：To determine the content of the polysaccharides from compound Nanbanlangen granules and the monosaccharide composition of the polysaccharides.Methods：The content of polysaccharides was determined by phenol sulfuric acid method：5% phenol solution 1 m L,sulfuric acid 5 m L,the detection wavelength 490 nm.The orthogonal test was designed to optimize the total degradation conditions of polysaccharides in the preparation of traditional Chinese medicine.The monosaccharides were derived by 1-phenyl-3-methyl-5-pyrazolone（PMP）and determined by capillary zone electrophoresis method.The electrophoresis conditions were as follows：uncoated fused silica capillary column（52 cm×50 μm,effective length 43 cm）,40 mmol·L-1 borax solution（pH=10.1） as the running buffer,the detection wavelength 245 nm,the operation voltage 12 k V,hydrodynamic pressure injection（8 cm×10 s）.Results：The content of polysaccharides was 1.708%-1.828%.The optimum hydrolysis conditions were as follows：0.75 mol·L-1 sulfuric acid solution,hydrolysis temperature 100 ℃,and hydrolysis time 5 h.The polysaccharides from compound Nanbanlangen granules were composed of xylose,arabinose,glucose,rhamnose,mannose,galactose,glucuronic acid and galacturonic acid.Results of Methods validation indicated that RSD of the precision test were ≤ 3.8%,as well as ≤ 5.5% in the repeatability test,and the stability of the method was satisfactory;the recovery rate of the method showed that the mean recoveries of galactose and galacturonic acid ranged from 99.7%-106.9% and 94.8%-102.5% respectively,and RSD values fell within 2.4%-4.9% and 1.7%-4.6% respectively.Conclusion：The study provides the reference for the determination of polysaccharides and the improvement of the drug criterion compound Nanbanlangen granules.

关 键 词：南板蓝根 蒲公英 紫花地丁 木糖 阿拉伯糖 葡萄糖 鼠李糖 甘露糖 半乳糖 葡萄糖醛酸 半乳糖醛酸 1-苯基-3-甲基-5-吡唑啉酮 硫酸-苯酚法 毛细管区带电泳法 

分 类 号：R917[医药卫生—药物分析学]