[关键词]
[摘要]
目的 建立HPLC波长切换法测定益坤宁酊中梓醇、麦角甾苷、马替诺皂苷、氧化芍药苷、芍药内酯苷、芍药苷和α-香附酮的方法。方法 采用Agilent Eclipse XDB-C18色谱柱(250 mm×4.6 mm,5μm);流动相A:乙腈–甲醇(1∶3),流动相B:0.2%磷酸溶液,梯度洗脱;检测波长210 nm(梓醇)、330 nm(麦角甾苷、马替诺皂苷)和230 nm(氧化芍药苷、芍药内酯苷、芍药苷、α-香附酮);体积流量0.8 mL/min;柱温25℃;进样量10 μL。结果 梓醇、麦角甾苷、马替诺皂苷、氧化芍药苷、芍药内酯苷、芍药苷和α-香附酮在2.66~66.50、1.59~39.75、0.76~19.00、1.38~34.50、7.02~175.50、9.91~247.75、1.19~29.75 μg/mL线性关系良好。平均加样回收率分别为97.97%、98.31%、96.99%、97.78%、99.28%、100.03%、97.43%,RSD值分别为1.42%、0.92%、1.30%、1.13%、1.08%、0.65%、1.27%。结论 本法操作便捷、数据准确、灵敏度高,重复性好,可为益坤宁酊的质量控制提供参考。
[Key word]
[Abstract]
Objective To develop an HPLC with wavelength switching method for determination of catalpol, acteoside, martinoside, oxypaeoniflorin, albiflorin, paeoniflorin and α-cyperone in Yikunning Tincture. Methods The separation was performed on Agilent Eclipse XDB-C18 column (250 mm×4.6 mm, 5 μm). The mobile phase consisted of mobile phase A acetonitrile-methanol (1:3) and mobile phase B 0.2% phosphoric acid solution with gradient elution. The detection wavelengths were set at 210 nm (catalpol), 330 nm (acteoside and martinoside), and 230 nm (oxypaeoniflorin, albiflorin, paeoniflorin, and α-cyperone). The flow rate was 0.8 mL/min, temperature of column was set at 25℃, and volume of injection was 10 μL. Results The linear ranges of catalpol, acteoside, martinoside, oxypaeoniflorin, albiflorin, paeoniflorin, and α-cyperone were 2.66-66.50, 1.59-39.75, 0.76-19.00, 1.38-34.50, 7.02-175.50, 9.91-247.75, and 1.19-29.75 μg/mL, respectively. The average recoveries were 97.97%, 98.31%, 96.99%, 97.78%, 99.28%, 100.03%, and 97.43% with RSD 1.42%, 0.92%, 1.30%, 1.13%, 1.08%, 0.65%, and 1.27%, respectively. Conclusion The method is convenient, accurate, sensitive, and reproducible, which can provide reference for quality control of Yikunning Tincture.
[中图分类号]
[基金项目]
广东省中医药强省项目(20142167)