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目的:建立柔肝胶囊含量测定的质量控制方法。方法:应用HPLC-DAD法测定其中丹酚酸B、姜黄素、去甲氧基姜黄素、双去甲氧基姜黄素的含量。采用Apollo C18柱(4.6 mm×250 mm,5μm),以4%醋酸水溶液和乙腈为流动相,梯度洗脱,流速为1.0 mL.min-1,柱温30℃,检测波长286,426 nm。应用HPLC-ELSD法测定其中牛磺熊去氧胆酸的含量。采用A-pollo C18柱(4.6 mm×250mm,5μm),以乙腈-乙酸-乙酸铵缓冲液(pH 4.5)为流动相,等度洗脱,流速为0.8 mL.min-1,ELSD漂移管温度80℃,雾化气体压力35 psi,喷雾器温度36℃。结果:丹酚酸B、姜黄素类成分、牛磺熊去氧胆酸的线性关系良好(r=0.999 3～0.999 9),线性范围分别为0.148 0～1.850,0.125 6～1.570,0.043 2～0.540 0,0.033 6～0.420 0,0.972 0～12.15μg;精密度、重复性、稳定性的RSD都低于3%;加样回收率为97.8%～101.7%。结论:本方法简便快捷、结果准确且重现性好,可用于柔肝胶囊的质量控制。
Objective: To establish a quality control method of Rougan capsule. Methods: The contents of salvianolic acid B, curcumin, demethoxycurcumin and bis-demethoxycurcumin were determined by HPLC-DAD. Apollo C18 column (4.6 mm × 250 mm, 5 μm) was used with a mobile phase of 4% acetic acid and acetonitrile as the mobile phase. The flow rate was 1.0 mL.min-1. The column temperature was 30 ℃ and the detection wavelength was 286,426 nm. Determination of tauroursodeoxycholic acid content by HPLC-ELSD method. The sample was eluted with an A-pollo C18 column (4.6 mm × 250 mm, 5 μm) with isocratic elution using acetonitrile-acetic acid-ammonium acetate buffer (pH 4.5) as the mobile phase at a flow rate of 0.8 mL.min-1. 80 ° C, atomizing gas pressure 35 psi, sprayer temperature 36 ° C. Results: The linear relationship between salvianolic acid B, curcumin and tauroursodeoxycholic acid was good (r = 0.999 3 ~ 0.999 9). The linear range was 0.148 0 ~ 1.850,0.125 6 ~ 1.570,0.043 2 ~ 0.540 0,0.033 6-0.420 0,0.972 0-12.15μg. The RSDs of precision, repeatability and stability were all less than 3%. The recoveries of samples were 97.8% -101.7%. Conclusion: The method is simple, rapid, accurate and reproducible. It can be used for the quality control of Rougan capsule.