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[摘要]
目的 建立HPLC法同时测定复方前列舒丸中大车前苷、柚皮苷、橙皮苷、新橙皮苷、朝藿定C、淫羊藿苷6个活性成分的方法。方法 采用安捷伦Zorbax C18色谱柱(250 mm×4.6 mm,5 μm);流动相为乙腈-0.1%磷酸水溶液,梯度洗脱;检测波长为330 nm(0~20 min,测定大车前苷)、283 nm(20~40 min,测定柚皮苷、橙皮苷、新橙皮苷)、270 nm(40~50 min,测定朝藿定C、淫羊藿苷);柱温为35 ℃;体积流量为1.0 mL/min;进样量为5 μL。结果 大车前苷、柚皮苷、橙皮苷、新橙皮苷、朝藿定C、淫羊藿苷在10.11~202.20、49.62~992.40、15.46~309.20、44.62~892.40、18.39~367.80、52.18~1 043.60 ng与峰面积线性关系良好。大车前苷、柚皮苷、橙皮苷、新橙皮苷、朝藿定C、淫羊藿苷的平均回收率分别为97.4%、98.8%、99.5%、98.9%、97.2%、95.6%,RSD值分别为0.83%、1.2%、1.4%、1.5%、1.5%、1.0%。结论 该方法稳定可靠、简便易行,同时测定复方前列舒丸中大车前苷、柚皮苷、橙皮苷、新橙皮苷、朝藿定C、淫羊藿苷6个特征性成分,为全面控制复方前列舒丸的质量提供了参考。
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[Abstract]
Objective To establish an HPLC method for simultaneous determination of six active ingredients plantamajoside, naringin, hesperidin, neohesperidin, epimedin C, and icariin in Compound Qianlieshu Pills. Methods The determination was carried out with Agilent Zorbax C18 column (250 mm × 4.6 mm, 5 μm). The mobile phase consisted of acetonitrile-0.1% phosphoric acid solution with gradient elution. The detection wavelengths were 330 nm in 0—20 min (determination of plantamajoside), 283 nm in 20—40 min (determination of naringin, hesperidin, and neohesperidin), and 270 nm in 40—50 min ( determination of epimedin C and icariin). The column temperature was set at 35 ℃, and the flow rate was 1.0 mL/min with injection volume of 5 μL. Results There were good linear relationships of plantamajoside, naringin, hesperidin, neohesperidin, epimedin C, and icariin in the concentration ranges of 10.11—202.20, 49.62—992.40, 15.46—309.20, 44.62—892.40, 18.39—367.80, and 52.18—1 043.60 ng. The average recoveries were 97.4%, 98.8%, 99.5%, 98.9%, 97.2%, and 95.6% with RSD 0.83%, 1.2%, 1.4%, 1.5%, 1.5%, and 1.0%, respectively. Conclusion The method is simple and valid, and can simultaneously determine six active ingredients plantamajoside, naringin, hesperidin, neohesperidin, epimedin C, and icariin, which can be used in quantity control for Compound Qianlieshu Pills.
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