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目的建立十味盆安颗粒中9种成分(没食子酸、丹参素钠、绿原酸、芍药苷、虎杖苷、苯甲酸、丹酚酸B、大黄素、大黄素甲醚)的定量测定及指纹图谱研究方法,为十味盆安颗粒的质量控制提供依据。方法采用HPLC法,色谱柱为Thermo C18柱(250 mm×4.6 mm,5μm);以乙腈-0.1%磷酸水溶液为流动相,梯度洗脱:0~16 min,5%~14%乙腈;16~20 min,14%~17%乙腈,20~35 min,17%~19%乙腈;35~60 min,19%~35%乙腈;60~62 min,35%~75%乙腈;62~78 min,75%乙腈;体积流量1.0 m L/min;检测波长230 nm(定量测定与指纹图谱用)。结果没食子酸、丹参素钠、绿原酸、芍药苷、虎杖苷、苯甲酸、丹酚酸B、大黄素、大黄素甲醚9种成分均达到基线分离,在线性范围内线性关系良好,r均>0.999 9,加样回收率分别为100.15%(RSD为1.39%)、99.89%(RSD为1.71%)、99.92%(RSD为0.67%)、99.28%(RSD为0.60%)、99.89%(RSD为0.80%)、99.72%(RSD为1.83%)、99.91%(RSD为0.79%)、100.06%(RSD为0.94%)、99.97%(RSD为1.36%);利用中药指纹图谱相似度评价系统(2012版)对15批十味盆安颗粒指纹图谱进行分析,15批样品指纹图谱与对照指纹图谱相似度达0.976以上。结论该方法简便可行、快速准确,可以作为评价十味盆安颗粒质量的有效方法。
OBJECTIVE To establish a quantitative determination and fingerprinting of nine components (gallic acid, sodium danshensu, chlorogenic acid, paeoniflorin, catalase, benzoic acid, salvianolic acid B, emodin and physcion) Map research methods for the quality control of Shiwei pellets to provide the basis. Methods HPLC was performed on a Thermo C18 column (250 mm × 4.6 mm, 5 μm) using acetonitrile-0.1% phosphoric acid as mobile phase with gradient elution from 0 to 16 min and 5% to 14% acetonitrile. 20 min, 14% -17% acetonitrile, 20-35 min, 17% -19% acetonitrile, 35-60 min, 19-35% acetonitrile, 60-62 min, 35-75% acetonitrile, , 75% acetonitrile; volume flow 1.0 m L / min; detection wavelength 230 nm (for quantitative determination and fingerprinting). Results The contents of gallic acid, sodium danshensu, chlorogenic acid, paeoniflorin, polydatin, benzoic acid, salvianolic acid B, emodin and physcion were all baseline-separated and had a good linearity in the linear range. R (RSD = 1.39%), 99.89% (RSD = 1.71%), 99.92% (RSD = 0.67%), 99.28% (RSD = 0.60%) and 99.89% (RSD: 0.80%), 99.72% (RSD: 1.83%), 99.91% (RSD: 0.79%), 100.06% (RSD: 0.94%) and 99.97% (RSD: 1.36% (2012 edition) 15 batches of ten flavor Pan’an particles fingerprint analysis, 15 batches of fingerprints and control fingerprints similarity of 0.976 or more. Conclusion The method is simple and feasible, rapid and accurate, and can be used as an effective method to evaluate the granule quality of Shiwei Wei’an.