摘要
目的:建立同时测定复方消痔栓中没食子酸、大黄酸和大黄素含量的方法。方法:采用高效液相色谱法。色谱柱为Kromasil C18,流动相为0.5%磷酸-乙腈(梯度洗脱),流速为1.0 ml/min,检测波长为273 nm(没食子酸)、254 nm(大黄酸和大黄素),柱温为28℃,进样量为20μl。结果:没食子酸、大黄酸、大黄素的检测质量浓度线性范围分别为0.296 4-14.82、0.215 0-10.75、0.307 2-15.36μg/ml(r=0.999 6、0.999 9、0.999 9);精密度、稳定性、重复性试验的RSD〈3.0%;加样回收率分别为95.1%-97.2%、95.4%-97.2%、96.5%-99.4%,RSD分别为0.64%、0.42%、1.10%(n=6)。结论:该方法操作简便、结果准确,可用于复方消痔栓中没食子酸、大黄酸和大黄素含量的同时测定。
OBJECTIVE:To establish a method for the simultaneous determination of gallic acid,rhein and emodin in Compound xiaozhi suppository. METHODS:HPLC was performed on the column of Kromasil C18 with mobile phase of 0.5% phosphoric acid-Acetonitrile solution(gradient elution)at a flow rate of 1.0 ml/min,the detection wavelength was 273 nm for gallic acid and254 nm for rhein and emodin,the column temperature was 28 ℃,and the injection volume was 20 μl. RESULTS:The linear range was 0.296 4-14.82 μg/ml for gallic acid(r=0.999 6),0.215 0-10.75 μg/ml for rhein(r=0.999 9)and 0.307 2-15.36 μg/ml for emodin(r=0.999 9);RSDs of precision,stability and reroducibility tests were lower than 3.0%;recoveries were 95.1%-97.2%(RSD=0.64%,n=6),95.4%-97.2%(RSD=0.42%,n=6)and 96.5%-99.4%(RSD=1.10%,n=6),respectively. CONCLUSIONS:The method is simple and accurate,and can be used for the contents determination of gallic acid,rhein and emodin in Compound xiaozhi suppository.
出处
《中国药房》
CAS
北大核心
2016年第15期2138-2140,共3页
China Pharmacy