摘要
目的：建立测定冠心丹参片中三七皂苷R1、人参皂苷Rg1和Rb1的含量测定方法。方法：采用Agilent XDB-C18色谱柱（150 mm×4.6 mm,5μm）;流动相为乙腈—水,梯度洗脱;检测波长203 nm,流速0.8 mL/min,柱温20℃。比较了乙醇、正丁醇、水饱和的正丁醇和水四种提取溶剂,并同时考察了回流时间对提取效率的影响。结果：三七皂苷R1在10.536~106.1μg/mL范围内呈良好的线性关系,回归方程为：Y=2.0864X＋0.3302（r=0.9998）,加样回收率为97.10%（RSD=2.43%,n=6）;人参皂苷Rg1在45.44~454.4μg/mL范围内呈良好的线性关系,回归方程为：Y=4.5304X＋6.7317（r=0.9998）,加样回收率为95.14%（RSD=2.22%,n=6）;人参皂苷Rb1在38.32~383.2μg/mL范围内呈良好的线性关系,回归方程为：Y=2.9308X＋3.2983（r=1.0000）,加样回收率为98.05%（RSD=1.76%,n=6）结论：采用水饱和的正丁醇作为提取溶剂,在105℃中回流2 h,样品提取效率高,操作简便,结果准确,可以用于测定冠心丹参片中的三七皂苷R1、人参皂苷Rg1和Rb1的含量,为冠心丹参片质量控制提供参考。
Objective ： To develop an HPLC method for determination of Notoginsenoside Rl , Ginsenoside Rg1 and Ginsenoside Rb1 in Guanxin Dansheng Tablets. Methods： The HPLC analysis was performed on Agilent XDB - C18 （50 mm×4.6 mm,5μm）. The mobile phase was acetonitrile- water in a gradient elution. The detection wavelength was 203 nm and the column temperature was 20 ℃. We compared the ethanol, n - butanol and water saturation of n - butyl alcohol and water extraction solvent was as the extraction solvent. At the same time, we investigated the influence of reflux time and temperature on the extraction efficiency. Results： Notoginsenoside R1 had a good linear relationship in the range of 10. 536 - 106.10 g/mL and the regression equation was Y = 2. 0864X ＋ 0. 3302 （ r = 0. 9998 ）. The average rate of recovery was 97.10% （RSD = 2.43 % , n = 6）. Ginsenoside Rg1 had a good linear relationship in the range of 45.44 N 454.4 μg/ mL and the regression equation was Y =4. 5304X ＋6. 7317 （ r =0. 9998）. The average rate of recovery was 95.14% （RSD = 2.22% , n = 6 ）. Ginsenoside Rbl had a good linear relationship in the range of 38.32 ~ 383.2 μg/mL and the regression equation was Y = 2. 9308X ＋ 3. 2983 （ r = 1. 0000）. The average rate of recovery was 98.05% （ RSD = 1.76%, n = 6）. Conclusion： We used water saturation of n -butyl alcohol as solvent extraction, reflux in 105 ℃ for two hours. The sample extraction efficiency is high and the method is accurate, simple and can be used for quality control of Guanxin Dansheng Tablets.
出处
《中华中医药学刊》
CAS
2014年第11期2773-2776,共4页
Chinese Archives of Traditional Chinese Medicine
基金
蚌埠医学院研究生科研创新计划项目(Byycx1330)
