目的 建立HPLC法同時(shí)測(cè)定復(fù)方前列舒丸中大車前苷、柚皮苷、橙皮苷、新橙皮苷、朝藿定C、淫羊藿苷6個(gè)活性成分的方法。方法 采用安捷倫Zorbax C₁₈色譜柱(250 mm×4.6 mm,5 μm);流動(dòng)相為乙腈-0.1%磷酸水溶液,梯度洗脫;檢測(cè)波長(zhǎng)為330 nm(0~20 min,測(cè)定大車前苷)、283 nm(20~40 min,測(cè)定柚皮苷、橙皮苷、新橙皮苷)、270 nm(40~50 min,測(cè)定朝藿定C、淫羊藿苷);柱溫為35 ℃;體積流量為1.0 mL/min;進(jìn)樣量為5 μL。結(jié)果 大車前苷、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與峰面積線性關(guān)系良好。大車前苷、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別為97.4%、98.8%、99.5%、98.9%、97.2%、95.6%,RSD值分別為0.83%、1.2%、1.4%、1.5%、1.5%、1.0%。結(jié)論 該方法穩(wěn)定可靠、簡(jiǎn)便易行,同時(shí)測(cè)定復(fù)方前列舒丸中大車前苷、柚皮苷、橙皮苷、新橙皮苷、朝藿定C、淫羊藿苷6個(gè)特征性成分,為全面控制復(fù)方前列舒丸的質(zhì)量提供了參考。

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.