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[摘要]
目的 建立HPLC波长切换法同时测定养阴降压胶囊中马兜铃酸I、氧化芍药苷、芍药内酯苷和芍药苷。方法 采用HPLC法,Venusil MP C18色谱柱(250 mm×4.6 mm,5 μm);流动相:[甲醇-乙腈(2∶1)]-0.02%磷酸溶液,梯度洗脱;0~16 min在390 nm波长下检测马兜铃酸Ⅰ,16~40 min时在230 nm波长下检测氧化芍药苷、芍药内酯苷和芍药苷;体积流量1.0 mL/min;柱温35 ℃;进样量10 μL。结果 马兜铃酸I、氧化芍药苷、芍药内酯苷和芍药苷质量浓度分别在4.72~94.40(r=0.999 8)、3.95~79.00(r=0.999 9)、6.39~127.80(r=0.999 9)、19.81~396.20 μg/mL(r=0.999 1)与峰面积呈良好的线性关系;平均回收率分别为97.47%、99.09%、100.09%、98.88%,RSD值分别为1.19%、1.60%、0.84%、0.65%。结论 所建立的方法简便,重复性好,为有效控制养阴降压胶囊的质量提供了依据。
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[Abstract]
Objective To develop an HPLC-wavelength switching method for simultaneous determination of aristolochic acid I, oxypaeoniflorin, alibiflorin, and paeoniflorin in Yangyin Jiangya Capsules. Method HPLC method was adopted. The determination was carried out on Venusil MP C18 chromatographic column (250 mm×4.6 mm, 5 μm). The mobile phase consisted of methanol-acetonitrile (2:1) and 0.02% phosphoric acid solution with gradient elution. The detection wavelengths were set at 390 nm in 0-16 min (determination of aristolochic acid I) and 230 nm in 16-40 min (determination of oxypaeoniflorin, alibiflorin, and paeoniflorin). The flow rate was 1.0 mL/min, temperature of column was set at 35℃, and volume of injection was 20 μL. Results There were good linear relationships of aristolochic acid I, oxypaeoniflorin, alibiflorin, and paeoniflorin in the concentration ranges of 4.72-94.40 μg/mL (r=0.999 8), 3.95-79.00 μg/mL (r=0.999 9), 6.39-127.80 μg/mL (r=0.999 9), and 19.81-396.20 μg/mL (r=0.999 1) between peak areas, respectively. The average recoveries were 97.47%, 99.09%, 100.09%, and 98.88% with RSD 1.19%, 1.60%, 0.84%, and 0.65%, respectively. Conclusion The established method is simple and has good repeatability which can be used in quantity control for Yangyin Jiangya Capsules.
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