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作 者:覃芳[1] 李广胜[1] 郭兴辉[2] QIN Fang;LI Guang-sheng;GUO Xing-hui(Department of Pharmacy,Third Affiliated Hospital of Henan University of Traditional Chinese Medicine,Zhengzhou 450008,China;Henan Institute of Drug and Food Control,Zhengzhou 450003,China)
机构地区:[1]河南中医药大学第三附属医院药学部,河南郑州450008 [2]河南省食品药品检验所,河南郑州450003
出 处:《现代药物与临床》2021年第2期240-244,共5页Drugs & Clinic
基 金:河南省中医药科学研究专项课题(2017ZY2027)。
摘 要:目的建立高效液相色谱法同时测定痛风定胶囊中龙胆苦苷、马钱苷酸、獐牙菜苦苷、獐牙菜苷、杯苋甾酮、泽泻醇F、泽泻醇A、24-乙酰泽泻醇A和23-乙酰泽泻醇B。方法采用HPLC法,Waters Symmetry C18色谱柱(250 mm×4.6 mm,5μm);流动相:乙腈–0.1%磷酸水溶液,梯度洗脱;检测波长:240nm(0~27min检测龙胆苦苷、马钱苷酸、獐牙菜苦苷、獐牙菜苷和杯苋甾酮)和208nm(27~55min检测泽泻醇F、泽泻醇A、24-乙酰泽泻醇A、23-乙酰泽泻醇B);体积流量:1.0 mL/min;柱温:30℃;进样量:10μL。结果龙胆苦苷、马钱苷酸、獐牙菜苦苷、獐牙菜苷、杯苋甾酮、泽泻醇F、泽泻醇A、24-乙酰泽泻醇A、23-乙酰泽泻醇B分别在45.84~1 146.00、9.02~225.50、12.86~321.50、4.69~117.25、0.88~22.00、0.59~14.75、0.77~19.25、0.66~16.50、3.37~84.25μg/mL与峰面积线性关系良好(r≥0.999 1),平均加样回收率分别为100.03%、99.55%、99.78%、98.56%、97.98%、96.95%、98.21%、97.75%、100.06%,RSD值分别为0.61%、0.95%、0.71%、1.17%、1.63%、1.09%、1.73%、1.20%、0.84%。结论所建立的方法结果准确,操作便捷,重复性好,为全面评价痛风定胶囊的整体质量提供了参考依据。Objective To establish an HPLC method for simultaneous determination of gentiopicrin, loganic acid, swertiamain, sweroside, cyasterone, alisol F, alisol A, 24-acetate alisol A, and 23-acetate alisol B in Tongfengding Capsules. Methods The separation by HPLC was performed on Waters Symmetry C18 column(250 mm × 4.6 mm, 5 μm) with mobile phase of acetonitrile-0.1% phosphoric acid in gradient elution. The detection wavelength were set at 240 nm(for gentiopicrin, loganic acid, swertiamain, sweroside, and cyasterone) and 208 nm(for alisol F, alisol A, 24-acetate alisol A, and 23-acetate alisol B). The flow rate was 1.0 mL/min, the column temperature was 30 ℃, and the volume of injection was 10 μL. Results Gentiopicrin, loganic acid, swertiamain, sweroside, cyasterone, alisol F,alisol A, 24-acetate alisol A, and 23-acetate alisol B had good linear relationships in the ranges of 45.84—1 146.00, 9.02—225.50, 12.86—321.50, 4.69—117.25, 0.88—22.00, 0.59—14.75, 0.77—19.25, 0.66—16.50, and 3.37—84.25 μg/mL(r ≥ 0.999 1). The average recoveries were 100.03%, 99.55%,99.78%, 98.56%,97.98%, 96.95%, 98.21%, 97.75%, and 100.06% with the RSD values of 0.61%, 0.95%, 0.71%, 1.17%, 1.63%, 1.09%, 1.73%, 1.20%, and 0.84%. Conclusion The established method is accurate, convenient, and reproducible, which provides a reference for the comprehensive evaluation of the overall quality of Tongfengding Capsules.
关 键 词:痛风定胶囊 龙胆苦苷 马钱苷酸 獐牙菜苦苷 獐牙菜苷 杯苋甾酮 泽泻醇F 泽泻醇A 24-乙酰泽泻醇A 23-乙酰泽泻醇B 高效液相色谱
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