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机构地区:[1]西南民族大学少数民族药物研究所,成都610041
出 处:《西南民族大学学报(自然科学版)》2014年第3期388-393,共6页Journal of Southwest Minzu University(Natural Science Edition)
基 金:科技部十二五支撑计划资助(2012BAI27B07);西南民族大学研究生创新项目资助(CX2014SP262)
摘 要:目的:建立二十一味寒水石丸中总鞣质、没食子酸和鞣花酸的含量测定方法.方法:以干酪素作为吸附剂,碱性条件下显色,以磷钼钨酸为氧化剂,用紫外可见分光光度法测定鞣质含量;采用HPLC法同时测定没食子酸和鞣花酸的含量.使用迪马Diamonsil-2 C18(4.6 mm×250mm,5μm)色谱柱,以乙腈-0.1磷酸水梯度洗脱,体积流量分别为1.0mL/min,柱温为30℃;检测波长270nm,测定.结果:以没食子酸计的鞣质含量在0.5~ 5μg·ml-1的范围内线性关系良好(r=0.9991),平均回收率为95.77%,RSD为0.70%(n=6);没食子酸在0.32~1.6μg范围内线性关系良好(r=0.9999),平均回收率为98.70%,RSD为1.01%(n=9),鞣花酸在0.372~.1.86μg范围内线性关系良好(r=0.9999),平均回收率为99.63%,RSD为0.75%(n=9).结论:本方法准确、可靠简便,具有较强专属性,可用于常用藏药二十一味寒水石丸中总鞣质、没食子酸和鞣花酸的含量测定.Objective: To establish a stable method for determination of total tannins, gallic acid and ellagic acid in Ershiyiwei Hanshuishi pill. Methods: The UV-vis method was used to determine the content of total tannins of Ershiyiwei Hanshuishi pill with casein as sorbent, phosphorus molybdenum-tungsten acid as oxidant. Gallic acid and ellagic acid were determined by HPLC. The Diamonsil-2 Cls column(4.6 mmx250 mm, 5μm) column was used with gradient elution. Mobile phase was composed of acetonitrile-0.1% phosphoric acid in solution, and the flow rate was 1 mL/min. The column temperature was kept at 25 ℃.The detection wavelength was set at 270 nm. Results: The linear relationship of standard curve was good within the range of 0.5-5μg/mL, r = 0.9991,and the average recovery was 95.77% with RSD of 0.70% (n=6). The linear range of gallic acid was 0.32-1.6μg(r=0.9999), and the average recovery rate was 98.70%, with RSD of 1.01%. The linear range of ellagic acid was 0.372-1.86txg(r=0.9999), the average recovery rate was 99.63% with RSD of 0.75% respectively. Conclusion: The method is accurate, reliable, specific and can be used to determine the total tannins, gallic acid and ellagic acid in Ershiyiwei Hanshuishi pill.
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