| 摘要: |
| 目的将本院协定处方清肝散结方制成颗粒剂后,对清肝散结颗粒中所含化学成分熊果酸及齐墩果酸进行含量测定,建立制剂质量控制方法。方法采用高效液相色谱法,色谱柱Chromsil-C18 (4.6 mm×250 mm,5 μm),流动相A相为0.1％甲酸水溶液,B相为甲醇,A∶B=12∶88,流速为1.0 ml/min,柱温25℃,紫外检测波长210 nm,进样量50 μl,运行时间为25 min。结果熊果酸和齐墩果酸能够达到基线分离,二者分别在6.1~97.6、6.4~102 μg/ml范围内呈良好的线性关系(r>0.999),日内和日间精密度均小于2%(n=3),平均回收率分别为95.4%(RSD 1.54%,n=6)、99.2%(RSD 1.97%,n=6)。结论该法简便、快捷,结果准确、重复性好,可用于清肝散结颗粒中熊果酸和齐墩果酸的质量控制。 |
| 关键词: 清肝散结颗粒 熊果酸 齐墩果酸 高压液相色谱法 |
| DOI：10.3724/SP.J.1008.2012.001263 |
| 投稿时间：2012-09-12修订日期：2012-10-18 |
| 基金项目: |
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| High performance liquid chromatography in determining ursolic acid and oleanolic acid contents in Qinggansanjie granules |
| ZHAO Liang1,WANG Xin-xia1,LI Yue-dan2,ZHOU Jin1,ZHANG Hai1,Lü Lei1,ZHANG Guo-qing1,CHAI Yi-feng3* |
(1. Department of Pharmacy, Eastern Hepatobiliary Surgery Hospital, Second Military Medical University, Shanghai 200438, China
2. Department of Pharmacy, No. 161 Hospital of PLA, Wuhan 430010, Hubei, China
3. School of Pharmacy, Second Military Medical University, Shanghai 200433, China
*Corresponding author.) |
| Abstract: |
| Objective To establish a method for determining the contents of ursolie acid and oleanolic acid in Qinggansanjie granules for quality control of the preparation. MethodsHigh-performance liquid chromatography with a diode-array detector (HPLC-DAD) was used for determination at the following conditions: The column was Chromsil-C18 (4.6 mm×250 mm, 5 μm), mobile phase was A: 0.1% (V/V) formic acid solution, B: methanol, A∶B = 12∶88. The flow rate was 1.0 ml/min, the temperature of column was 25℃, the detection wavelength was set at 210 nm, the injection volume was 50 μl, and the running time was 25 min. Results Ursolic acid and oleanolic acid could be separated on baseline, with the linear range being 6.1-97.6 μg/ml for ursolic acid and 6.4-102 μg/ml for oleanolic acid. The results of intra-day and inter-day precisions were both within 2% (n=3), and the average recovery was 95.4% (RSD 1.54%, n=6) and 99.2% (RSD 1.97%, n=6). Conclusion The present method is simple, rapid, accurate, and with satisfactory repeatability; it can be used for quality control of ursolic acid and oleanolic acid in Qinggansanjie granules. |
| Key words: Qinggansanjie granules ursolic acid oleanolic acid high pressure liquid chromatography |
