曲春雁,崔国方,范广慈,等.反向高效液相色谱法检测正心降脂片中丹参酮 ⅡA、葛根素和大黄素含量[J].安徽医药,2021,25(11):2174-2177. |
反向高效液相色谱法检测正心降脂片中丹参酮 ⅡA、葛根素和大黄素含量 |
Research RP-HPLC method for determination tanshinone ⅡA, puerarin and emodin in Zhengxin Jiangzhi tabets |
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DOI:10.3969/j.issn.1009-6469.2021.11.012 |
中文关键词: 降血脂药物 反向高效液相色谱法 正心降脂片 葛根素 大黄素 含量 |
英文关键词: Hypolipidemic agents RP-HPLC Zhengxin Jiangzhi Tabets Puerarin Emodin Content |
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中文摘要: |
目的建立检测正心降脂片中丹参酮 ⅡA、葛根素和大黄素 3种成分含量的方法。方法采用反向高效液相色谱( RPHPLC)法。取正心降脂片,除去包衣,研细,取约 0.2 g,精密称定,置滤膜滤过, Lichrospher RP-C18色谱柱分离,检测波长为 259 nm,流动相 A为乙腈,流动相 B为 0.2%磷酸溶液,梯度洗脱,洗脱程序为 0~6 min 12% A、6~15 min 12%~63% A、15~25 min 63%~92% A、25~27 min 91%A、27~30 min 91% ~12% A、30~35 min 12% A,流速为 1.0 mL/min,柱温为 30℃,进样体积为 10 μL,二极管阵列检测器定量检测。结果葛根素、大黄素和丹参酮 ⅡA分别在 0.763~76.3 μg/mL、0.768~76.8 μg/mL和 0.199~19.9 μg/mL范围内,线性关系良好,平均加标回收率分别为 98.5%,99.3%和 99.6%,重复性相对标准偏差( RSD)分别为 1.29%、2.05%和 1.72%;稳定性 RSD分别为 2.03%、1.72%和 1.33%。结论实验建立的方法具有简便、快速、准确等特点,适用于正心降脂片产品的质量控制,为进一步完善和提高该品种的质量标准提供技术参考。 |
英文摘要: |
Objective To establish method for determination 3 contents of tanshinone ⅡA, puerarin and emodin in Zhengxin Jiang? zhi tabets.Methods The coating of Zhengxin Jiangzhi Tabets samples was removed and grinded to powder. Weighing about 0.2 g pretreated samples precisely to 50 mL volumetric flask, ultrasonic treatment was performed with 95% methanol solution for 25 min. Volume the samples to 50 mL and shook it well. Samples was filtered by 0.45 μm membrane filter and separated on Lichrospher RP-C18 column. Detection wavelength: 259 nm. Mobile phase: acetonitrile (A)-0.2% phosphoric acid solution (B). Gradient elution procedure: 0-6 min 12% A, 6-15 min 12%-63% A,15-25 min 63%-92% A, 25-27 min 91%A, 27-30 min 91% -12% A, 30-35 min 12% A. flow rate: 1.0 mL/min, column temperature: 30℃ and injection volume was 10 μL. Diode array detector was for quantitative detection.Re? sults Puerarin, emodin and Tanshinone ⅡA showed good linear relationships in following concentration range 1.526-76.3 μg/mL, 1.536-76.8 μg/mL and 0.398-19.9 μg/mL, respectively. Average recoveries were 98.5%, 99.3% and 99.6%, respectively. Relative standard deviation (RSD) of repeatability (n=6) was 1.3%, 1.7% and 1.1%, respectively. The stability of RSD was 2.03%, 1.72% and 1.33%, respectively.Conclusion The method is simple, rapid and accurate, which is suitable for the quality control of Zhengxin Ji? angzhi Tabets. It also provides technical reference for further improving quality standard of this breed. |
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