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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 polysaccharide content and the monosaccharide composition of Nansha root granules. Methods: The content of polysaccharides was determined by sulfuric acid - phenol method. The conditions were as follows: 1 mL of 5% phenol solution and 5 mL of sulfuric acid. The detection wavelength was 490 nm. The orthogonal design was used to optimize the conditions for the degradation of polysaccharides in this preparation. The monosaccharide was analyzed by capillary zone electrophoresis with 1-phenyl-3-methyl-5-pyrazolone (PMP) as the derivatization reagent Electrophoresis conditions: uncoated flexible quartz capillary column (52 cm × 50 μm, effective length 43 cm), running buffer 40 mmol·L -1 borax buffer (pH 10.1), detection wavelength 245 nm, running Voltage 12 k V, injection volume 8 cm × 10 s. Results: The content of polysaccharides in the preparation was 1.708% ~ 1.828%. The optimal conditions for total degradation of polysaccharides were sulfuric acid concentration of 0.75 mol·L -1, temperature of 100 ℃ and time of 5 h. Sugar, arabinose, glucose, rhamnose, mannose, galactose, glucuronic acid and galacturonic acid. The established capillary zone electrophoresis method validation, the results showed that the precision RSD ≤ 3.8%, repeatability RSD ≤ 5.5%, and the stability to meet the requirements, the recovery results show that: galactose and galacturonic acid The average recoveries were 99.7% -106.9% and 94.8% -102.5%, respectively, with RSDs of 2.4% -4.9% and 1.7% -4.6%, respectively. Conclusion: This paper provides a reference for the determination of polysaccharide in Nansha root granules and the improvement of its quality standard.