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作 者:束艳[1] 宿树兰[1] 钱大玮[1] 段金廒[1] 蒋海峰[1]
机构地区:[1]南京中医药大学江苏省方剂研究重点实验室,南京210046
出 处:《中国实验方剂学杂志》2010年第18期71-75,共5页Chinese Journal of Experimental Traditional Medical Formulae
摘 要: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 determination method for quality control of Rougan capsule.Method: The contents of salvianolic acid B,curcumin,demethoxycurcumin and bisdemethoxycurcumin in Rougan capsule were determined by HPLC-DAD.These compounds were analyzed with a Apollo C18 column(4.6 mm × 250 mm,5 μm) by gradient elution using 4% acetic acid-acetonitrile as the mobile phase,the flow rata was 1.0 mL.min^-1,the column temperature was maintained at 30 ℃ and the wavelength was detected at 286 and 426 nm. The content of tauroursodeoxycholic acid in Rougan capsule was determined by HPLC-ELSD. It was analyzed with a Apollo Cls column (4.6 mm × 250 mm, 5 μm) by isocratic elution using acetonitrile-acetic acid-ammonium acetate solution (pH 4.5 ) as the mobile phase, the flow rate was 0. 8 mL. min^-1, the temperature of the drift tube was set at 80℃, the pressure of nebulizing gas (air) was at 35 psi, the temperature of the atomizer was at 36 ℃. Result: All these compounds were linear in the range of 0. 148 0-1. 850, 0. 125 6-1. 570, 0. 043 2-0. 540 0, 0. 033 6-0. 420 0 and 0. 972 0-12. 15 μg (r =0. 999 3-0. 999 9), respectively. The RSDs of the precision, reproducibility and stability test were less than 3% ; the average recovery of the method was in the range of 97.8%-101.7%. Conclusion: The established method is simple, accurate, and repeatable and can be used for quality control of Rougan capsule.
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