HPLC法同时测定复方消痔栓中3种成分的含量

Simultaneous Determination of Three Kinds of Components in Compound Xiaozhi Suppository by HPLC

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.