目的:建立HPLC法同时测定双石通淋胶囊中丹参素钠、京尼平苷酸、黄柏碱、丹酚酸B、巴马汀、小檗碱、苍术素、丹参酮Ⅱ A 8个成分的含量.方法:采用Capcell Pak MG Ⅱ C18(250 mm ×4.6 mm,5μm)色谱柱,流动相为乙腈-0.1％磷酸水-水(含0.1％磷酸和0.2％三乙胺,pH=6.0),梯度洗脱,流速为1.0 mL·min-1,柱温为30℃,进样量为10 μL,检测波长分别为280 nm(0～13.4 min,丹参素钠)、238 nm(13.5～17.0 min,京尼平苷酸)、280 nm(17.1～51.0 min,黄柏碱和丹酚酸 B)、345 nm(51.1.1～70.0 min,巴马汀和盐酸小檗碱)、336 nm(70.1～78.0 min,苍术素)和 268 nm(78.1～90.0 min,丹参酮ⅡA).结果:丹参素钠、京尼平苷酸、黄柏碱、丹酚酸B、巴马汀、小檗碱、苍术素、丹参酮ⅡA8个成分在各自线性范围内线性关系良好,相关系数均≥0.999 5;精密度、稳定性、重复性试验的RSD均小于2.0％;平均回收率分别为 101.3％、98.2％、97.3％、98.1％、96.6％、97.9％、98.7％、99.6％,RSD 均小于2.0％.3批样品中上述8个成分的含量范围分别为4.47～5.51、0.93～1.44、1.00～1.07、5.72～8.67、0.64～0.69、1.62～1.90、0.055～0.088、0.29～0.44 mg·g-1.结论:该方法快速、灵敏,专属性高,可用于同时测定双石通淋胶囊中8个成分的含量.
Simultaneous determination of eight components in Shuangshi Tonglin capsules by HPLC
Objective:To establish an HPLC method for the simultaneous determination of eight components inclu-ding salvianic acid A sodium,geniposidic acid,phellodendrine,salvianolic acid B,palmatine,berberine,atrac-tylodin,tanshinone Ⅱ A in Shuangshi Tonglin capsules.Methods:The determination was performed on a Capcell Pak MG Ⅱ C18 column(250 mm ×4.6 mm,5 μm)with the mobile phase consisting of acetonitrile-water(con-taining 0.1％phosphoric acid)-water(containing 0.1％phosphoric acid and 0.2％triethylamine,pH 6.0)in a gradient mode at a flow rate of 1.0 mL·min-1.The column temperature was set at 30 ℃,the injection volume was 10 μL,and the detection wavelength was 280 nm(0-13.4 min)for salvianic acid A sodium,238 nm(13.5-17.0 min)for geniposidic acid,280 nm(17.1-51.0 min)for phellodendrine,salvianolic acid B,345 nm(51.1.1-70.0 min)for palmatine,berberine,336 nm(70.1-78.0 min)for atractylodin and 268 nm(78.1-90.0 min)for tanshinone ⅡA.Results:Salvianic acid A sodium,geniposidic acid,phellodendrine,salvianolic acid B,palmatine,berberine,atractylodin,tanshinone Ⅱ A had good linearities in their respective line-ar ranges with all linear correlation coefficients ≥ 0.999 5 and RSDs of the precision,repeatability and stability less than 2.0％.The average recoveries were 101.3％,98.2％,97.3％,98.1％,96.6％,97.9％,98.7％,99.6％,with RSDs lower than 2.0％.The contents of the above eight components in three batches of samples was 4.47-5.51 mg·g-1,0.93-1.44 mg·g-1,1.00-1.07 mg·g-1,5.72-8.67 mg·g-1,0.64-0.69 mg·g-1,1.62-1.90 mg·g-1,0.055-0.088 mg·g-1,0.29-0.44 mg·g-1,respectively.Conclusion:The proposed method is rapid,sensitive and specific,which can be used for determination the contents of eitht compo-nents in Shuangshi Tonglin capsules.
Shuangshi Tonglin capsulesHPLCsalvianic acid A sodiumgeniposidic acidphellodendrinesalvianolic acid Bpalmatineberberineatractylodintanshinone Ⅱ A
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