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ⅡA 8个成分的含量。方法: 采用Capcell Pak MGⅡC18(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ⅡA 8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。
Abstract
Objective: To establish an HPLC method for the simultaneous determination of eight components including salvianic acid A sodium, geniposidic acid, phellodendrine, salvianolic acid B, palmatine, berberine, atractylodin, tanshinone ⅡA 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(containing 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, tanshinoneⅡA had good linearities in their respective linear 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 components in Shuangshi Tonglin capsules.
关键词
双石通淋胶囊 /
高效液相色谱法 /
丹参素钠 /
京尼平苷酸 /
盐酸黄柏碱 /
丹酚酸B /
巴马汀 /
小檗碱 /
苍术素 /
丹参酮ⅡA
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Key words
Shuangshi Tonglin capsules /
HPLC /
salvianic acid A sodium /
geniposidic acid /
phellodendrine /
salvianolic acid B /
palmatine /
berberine /
atractylodin /
tanshinone ⅡA
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