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[摘要]
目的 建立HPLC波长切换联合梯度洗脱法同时测定调中四消丸中咖啡酸、芦荟大黄素、大黄酸、大黄素甲醚、圆柚酮、α-香附酮。方法 采用Agilent TC-C18色谱柱(250 mm×4.6 mm,5 μm);流动相:乙腈–0.1%磷酸溶液,梯度洗脱;0~21 min在325 nm波长下检测咖啡酸;21~37 min在254 nm波长下检测芦荟大黄素、大黄酸和大黄素甲醚,37~55 min在242 nm波长下检测圆柚酮和α-香附酮;体积流量:0.9 mL/min;柱温:30 ℃;进样量为10 μL。结果 咖啡酸、芦荟大黄素、大黄酸、大黄素甲醚、圆柚酮、α-香附酮分别在2.48~49.60、17.56~351.20、4.59~91.80、6.76~135.20、1.92~38.40、4.26~85.20 μg/mL与峰面积线性关系良好;平均回收率分别为98.01%、99.27%、97.61%、99.41%、96.90%、98.58%,RSD值分别为0.77%、1.18%、0.96%、1.25%、1.48%、1.17%(n = 6)。结论 本方法简单快速,可作为调中四消丸的质量控制方法。
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[Abstract]
Objective To establish an HPLC wavelength switching combined gradient elution method for simultaneous determination of six major components, including caffeic acid, aloe-emodin, rhein, physcion, nootkatone and α-cyperone in Tiaozhong Sixiao Pills. Methods The determination was carried out on Agilent TC-C18 column (250 mm × 4.6 mm, 5 μm). The mobile phase was consisted of acetonitrile -0.05% phosphoric acid solution with gradient elution. The detection wavelengths were 325 nm (for caffeic acid), 254 nm (for aloe-emodin, rhein, and physcion), and 242 nm (for nootkatone and α-cyperone). The column temperature was set at 30 ℃, and the flow rate was 0.9 mL/min with injection volume of 10 μL. Results There were good linear relationships of caffeic acid, aloe-emodin, rhein, physcion, nootkatone, and α-cyperone in the concentration ranges of 2.48-49.60, 17.56-351.20, 4.59-91.80, 6.76-135.20, 1.92-38.40, and 4.26-85.20 μg/mL, respectively. The average recoveries were 98.01%, 99.27%, 97.61%, 99.41%, 96.90%, and 98.58% with RSD of 0.77%, 1.18%, 0.96%, 1.25%, 1.48%, and 1.17% (n=6), respectively. Conclusion The method is simple and rapid, which can be used as quality control methods for Tiaozhong Sixiao Pills.
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