摘要: |
目的:采用高效液相色谱法测定抗菌消炎片中绿原酸、黄芩苷、黄芩素和大黄酚的含量。方法:抗菌消炎片去包衣粉末用50%甲醇超声提取30 min;色谱柱为Agilen Eclipse Plus-C18柱(4.6 mm×250 mm,5 μm);流动相:A相为0.1%磷酸水溶液,B相为甲醇,C相为乙腈,梯度洗脱;流速:0.8 ml/min;温度:30℃;进样量:10 μl;检测波长:254 nm。结果:绿原酸、黄芩苷、黄芩素和大黄酚4种成分在45 min内基线分离。峰面积(Y)对浓度(X)的标准曲线分别为:绿原酸 Y=12.89X-12.66,r=0.999 9;黄芩苷 Y=13.96X-1.013,r=1.0;黄芩素 Y=35.82X-4.923,r=0.999 9;大黄酚 Y=44.16X-3.280,r=0.999 9。方法学考察表明,日内及日间精密度、最低检测限均符合相关标准,加样回收率分别为(n=3):绿原酸101.5%(RSD=1.6%);黄芩苷103.4%(RSD=1.4%);黄芩素99.3%(RSD=2.0%);大黄酚98.1%(RSD=1.7%)。结论:采用高效液相色谱法同时测定抗菌消炎片中绿原酸、黄芩苷、黄芩素和大黄酚的含量,样品处理简便,测定结果准确,可用于该制剂的质量控制。 |
关键词: 高效液相色谱法 抗菌消炎片 绿原酸 黄芩苷 黄芩素 大黄酚 |
DOI:10.3724/SP.J.1008.2009.01191 |
投稿时间:2009-05-09修订日期:2009-09-02 |
基金项目: |
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High performance liquid chromatography in determination of chlorogenic acid,baicalin,emodin and chrysophanol contents in Kangjunxiaoyan tablet |
FEI Yang,ZHAO Liang,ZHANG Hai,JIN Rou-nan,LV Lei,ZHANG Guo-qing* |
(Department of Pharmacy,Eastern Hepatobiliary Hospital,Second Military Medical University,Shanghai 200438,China) |
Abstract: |
Objective:To establish an HPLC method for determination of chlorogenic acid,baicalin,emodin and chrysophanol contents in Kangjunxiaoyan tablet. Methods: After removing the coating,the powder of Kangjunxiaoyan tablet was extracted by 50% methanol for 30 min using the following condition: analytical column,Agilent Eclipse Plus-C18 column(4.6 mm×250 mm,5 μm); mobile phase:A,0.1% (v/v) phosphoric acid-water,B,methanol,C,acetonitrile with gradient elution. The flow rate was 0.8 ml/min; the detection wavelength was set at 254 nm; the temperature of column was 30℃; and the injection volume was 10 μl. Results: The title compounds were separated at baseline within 45 min with good linear,with the regression being Y=12.89X-12.66,r=0.999 9 for chlorogenic acid,Y=13.96X-1.013,r=1.000 0 for baicalin,Y=35.82X-4.923,r=0.999 9 for emodin,and Y=44.16X-3.280,r=0.999 9 for chrysophanol. The intra-day and inter-day precisions and the limits of detection were all within the normal range. The recovery rates(n=3) were:chlorogenic acid 101.5%(RSD=1.6%),baicalin 103.4%(RSD=1.4%),emodin 99.3%(RSD=2.0%),and chrysophanol 98.1%(RSD=1.7%). Conclusion: HPLC is a simple,accurate,stable,and reliable method in determining the contents of chlorogenic acid,baicalin,emodin,and chrysophanol in Kangjunxiaoyan tablet,and it can be used for quality control of this preparation. |
Key words: high performance liquid chromatography Kangjun Xiaoyan table chlorogenic acid baicalin emodin chrysophanol |