[关键词]
[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,5 μm);流动相:乙腈-0.1%磷酸水溶液,梯度洗脱;检测波长:240 nm(0~27 min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208 nm(27~55 min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:10 μL。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、3.37~84.25 μg/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。
[Key word]
[Abstract]
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.
[中图分类号]
R284.1
[基金项目]
河南省中医药科学研究专项课题(2017ZY2027)