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| 高效液相色谱法测定小柴胡汤中黄芩苷、汉黄芩苷的含量 |
| 纪松岗1,刘晓帆2,朱臻宇2,梁珊珊3,赵亮3,张海3,,柴逸峰2* |
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| (1. 解放军401 医院药剂科,青岛266071;2. 第二军医大学药学院药物分析学教研室,上海200433;3. 第二军医大学东方肝胆外科医院药材科,上海200438) |
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| 摘要: |
| 目的 采用高效液相色谱法测定小柴胡汤中黄芩苷、汉黄芩苷的含量。方法 饮片粉末用水回流提取,色谱柱:Agilent Zorbax XDB-C18(150 mm×4.6 mm, 5 μm)；流动相为乙腈和水；A 相为0.2%磷酸-水,B 相为乙腈,梯度洗脱；流速1 ml/min ,柱温25℃,检测波长275 nm,进样量15 μl。结果 黄芩苷和汉黄芩苷在30 min内基线分离。以峰面积(Y)对浓度(X)的标准曲线分别为:黄芩苷Y=44.16X-36.22(r=0.999 9)； 汉黄芩苷Y=52.08X-28.69(r=0.999 9)。日内及日间精密度均小于1%,黄芩苷和汉黄芩苷的定量限分别为0.615 6 μg/ml和0.220 8 μg/ml,黄芩苷和汉黄芩苷加样回收率(n=6)分别为95.73%(RSD=0.8%)及97.02%(RSD=1.56%)。结论 该方法稳定性好,测定结果准确可靠,可用于小柴胡汤的质量控制研究。 |
| 关键词: 高压液相色谱法 小柴胡汤 黄芩苷 汉黄芩苷 含量测定 |
| DOI：10.3724/SP.J.1008.2010.00 |
| 投稿时间：2010-05-10修订日期：2010-06-30 |
| 基金项目:国家自然科学基金 (30873196). |
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| High performance liquid chromatography in determination of baicalin and wogonoside contents in Xiaochaihu decoction |
| JI Song-gang1, LIU Xiao-fan2, ZHU Zhen-yu2, LIANG Shan-shan3, ZHAO Liang3, ZHANG Hai3,,CHAI Yi-feng2* |
| (1. Department of Pharmacy, No. 401 Hospital of PLA, Qingdao 266071, Shangdong, China;2. Department of Drug Analysis, School of Pharmacy, Second Military Medical University, Shanghai 200433, China;3. Department of Pharmacy, Eastern Hepatobiliary Surgery Hospital, Second Military Medical University, Shanghai 200438, China) |
| Abstract: |
| Objective To establish an HPLC method for determination of baicalin and wogonoside contents in Xiaochaihu decoction. Methods Decoction pieces were mixed and decocted with water. The chromatographic column was Agilent Zorbax XDB-C18(150 mm×4.6 mm, 5 μm); the mobile phase was composed of 0.2% phosphate acid-water(A) and acetonitrile (B) with gradient elution at a flow rate of 1 ml/min. The detection wavelength was set at 275 nm, the temperature of column was 25℃, and the injection volume was 15 μl. Results Baicalin and wogonoside were separated at baseline within 30 min with good linearity; the standard curves for baicalin and wogonoside were Y=44.16X-36.22 (r=0.999,9) and Y=52.08X-28.69(r=0.999,9), respectively. The intra-day and inter-day precisions were both less than 1%, and the limits of qualification were 0.615,6 μg/ml for baicalin and 0.220,8 μg/ml for wogonoside. The recovery rates (n=6) were 95.73% (RSD=0.8%) for baicalin and 97.02% (RSD=1.56%) for wogonoside. Conclusion The method is simple, accurate, stable, and reliable in determining the contents of baicalin and wogonoside in Xiaochaihu decoction, and it can be used for the quality control of this preparation. |
| Key words: high performance liquid chromatography Xiaochaihu decoction baicalin wogonoside determination |
