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作 者:钟浩[1] 邓祖磊 葛德洲 刘浩[1] 崔田[2] 宋雅彤
机构地区:[1]蚌埠医学院药学系,安徽蚌埠233000 [2]蚌埠市食品药品检验所,安徽蚌埠233000
出 处:《中华中医药学刊》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)
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.
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