摘要: |
目的 采用HPLC法测定不同产地淫羊藿药材中7种主要黄酮类成分的含量。 方法 色谱柱为SHISEIDO MG-C18柱 (3.0 mm×100 mm, 3.0 μm);流动相为乙腈(A)和0.1%的甲酸水溶液(B),梯度洗脱,A相含量随时间的变化:25%(0~10 min),25%~40%(10~12 min),40%~45% (12~22 min), 45%~75% (22~25 min), 75%(25~30 min);流速0.6 mL/min;检测波长270 nm;柱温25℃;进样量5 μL。淫羊藿药材以70%乙醇超声提取。 结果 7种黄酮类成分朝藿定A、朝藿定B、朝藿定C、淫羊藿苷、淫羊藿次苷Ⅰ、淫羊藿次苷Ⅱ、脱水淫羊藿素在30 min内基线分离。方法学验证表明,线性关系良好(r=0.999 9),日内、日间精密度RSD均小于2.0%,回收率在98%~102%之间,稳定性和重复性RSD也均小于 2.0%,符合方法学要求。测定了对照药材及辽宁、甘肃、湖北3个产地淫羊藿中7种黄酮类成分的含量。 结论 该方法快速简便,可为淫羊藿药材的质量控制提供依据,也为进一步开展淫羊藿中黄酮类成分的药动学及组织分布研究奠定了良好的基础。 |
关键词: 淫羊藿 黄酮类 高效液相色谱法 含量测定 |
DOI:10.3724/SP.J.1008.2015.01352 |
投稿时间:2015-04-02修订日期:2015-05-22 |
基金项目: |
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HPLC in simultaneous determination of seven main flavonoids in Epimedium of different places of origin |
HUANG Mi-naΔ,ZHOU Yan-niΔ,LIU Qiang,ZHOU Jin,LV Lei* |
(Department of Pharmacy, Eastern Hepatobiliary Surgery Hospital, Second Military Medical University, Shanghai 200438, China △Co-first authors. *Corresponding author.) |
Abstract: |
Objective To determine the contents of seven main flavonoids in Epimedium of different places of origin by high performance liquid chromatography (HPLC). Methods The HPLC condition was as follows: SHISEIDO MG-C18 column (3.0 mm×100 mm,3.0 μm); the mobile phase consisted of acetonitrile and water containing 0.1% formic acid was used as gradient elute; the gradient of acetonitrile was 25% (0-10 min), 25%-40% (10-12 min), 40%-45% (12-22 min), 45%-75% (22-25 min) and 75%(25-30 min); flow rate was 0.6 mL/min; UV detection wavelength was set at 270 nm; column temperature was 25℃; and injection volume was 5 μL. The sample was ultrasonically extracted with 70% ethanol solution. Results The seven flavonoids, including epimedin A, epimedin B, epimedin C, icariin, icariside Ⅰ, icariside Ⅱ and anhydroicaritin were separated at baseline within 30 min. The standard curves had good linearity (r=0.999 9), with the RSD% of intraday and interday precision being both less than 2.0%, the recovery being 98%-102%, and the RSD% of stability and repeatability also being less than 2.0%. The results showed that the method could meet the requirements of method validation. The contents of seven flavonoids in reference crude meterial and Herba Epimedii from Liaoning, Gansu and Hubei province were determined. Conclusion The present method is rapid and simple, and can be used for quality control of Epimedium, which may lay a foundation for studying the pharmacokinetics and tissue distribution of the flavonoids of Epimedium. |
Key words: Epimedium flavonoids high performance liquid chromatography determination |