摘要
目的:建立高效液相色谱法测定牛膝和决津颗粒中β-蜕皮甾酮的方法。方法:分别采用回流法和超声法提取牛膝和决津颗粒中β-蜕皮甾酮,并对提取方法进行优化;采用HPLC测定β-蜕皮甾酮的含量,Kromasil C18色谱柱(4.6 mm×250mm,5μm)色谱柱,乙腈-水(17∶83)为流动相,流速1.0 mL·min-1,检测波长242 nm,柱温30℃。结果:牛膝的最佳提取条件为加入15倍量70%乙醇回流提取2次,每次1 h,决津颗粒的最佳提取条件为以水为溶剂超声提取30 min;β-蜕皮甾酮的线性范围为10.37~103.7 mg·L-1,回归方程为Y=24 867X+1 563(r=0.999 5),牛膝和决津颗粒的平均回收率分别为98.5%,98.4%,RSD分别为1.6%,1.4%(n=9)。结论:方法准确可行,重复性好,可为评价决牛膝和决津颗粒质量提供依据。
Objective: To develop a HPLC method for determining the content of ecdysterone in Achyranthis bidentatae and Juejin Granula.Method: Ecdysterone was extracted from Radix Achyranthis bidentatae and Juejin Granula using reflux and ultrasonic extraction and optimizing the extraction condition.Determining the content of ecdysterone was determined by HPLC,the chromatography was performed on a Kromasil C18 column(250 mm×4.6 mm,5 μm) at 30 ℃ with acetonitrile-water(17∶ 83) as mobile phase.The flow rate was 1.0 mL·min-1 and UV detection wavelength was at 242 nm.Result: The optimal extraction condition of Radix Achyranthis bidentatae: reflux extracting two times by adding 15 times of 70% ethanol and once for 1 hour,the optimal extraction condition of Juejin Granula: ultrasonic extracting with warter as solvent for 30 min.The linear range of ecdysterone was 10.37-103.7 mg·L-1(r=0.999 5),the regress equation was Y=24 867X+1 563(r=0.999 5),the recoveries were 97.8% and 97.9%,RSDs were 1.8% and 1.4%(n=9).Conclusion: The method is accurate,available and reduplicate,and providing the basis for evaluating the quality of Radix Achyranthis bidentatae and Juejin Granula.
出处
《中国实验方剂学杂志》
CAS
北大核心
2012年第9期122-125,共4页
Chinese Journal of Experimental Traditional Medical Formulae