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目的:研究“武当二号金银花”藤中主要有效成分含量测定方法,为评价其品质奠定基础。方法:采用超声法考察提取溶剂、超声时间、超声功率及料液比4个因素对样品中芦丁和木犀草苷成分提取的影响,并使用4因素3水平的正交试验方法优化提取条件。含量测定色谱条件:色谱柱:绿原酸为C18柱(Phenomenex Luna,250 mm×4.6 mm,5μm);马钱苷、芦丁与木犀草苷均为苯基柱(Fortis Xi phenyl,250 mm×4.6 mm,5μm);流动相:绿原酸、马钱苷为乙腈-0.4%磷酸溶液(15∶85);芦丁与木犀草苷为乙腈-0.5%冰醋酸溶液梯度洗脱;柱温:30℃;检测波长分别为327,237,354,348 nm。结果:提取“武当二号金银花”藤中芦丁与木犀草苷成分的最佳条件:提取溶剂均为60%乙醇;料液比均为1∶30,超声功率分别为350,250 w;超声时间分别为50,60 min。样品中有效成分绿原酸、马钱苷、芦丁和木犀草苷的平均含量分别为10.27,6.33,0.401,0.450 mg·g-1。结论:该方法简便、准确、重现性好,为其质量控制及进一步开发利用提供参考。
Objective: To study the method of determination of main active ingredients in “Wudang No.2 honeysuckle”, and lay the foundation for the evaluation of its quality. Methods: The effects of extraction solvent, ultrasonic time, ultrasonic power and solid-to-liquid ratio on the extraction of rutin and luteolin in samples were studied by ultrasonic method. The extraction conditions were optimized by orthogonal experiment with 4 factors and 3 levels. Content determination Chromatographic conditions: Column: chlorogenic acid C18 column (Phenomenex Luna, 250 mm × 4.6 mm, 5μm); loganin, rutin and luteolin are phenyl column (Fortis Xi phenyl, 250 mm × 4.6 mm, 5 μm); mobile phase: chlorogenic acid, loganin as acetonitrile-0.4% phosphoric acid solution (15:85); gradient of rutin and luteolin as acetonitrile- 30 ℃; detection wavelength were 327,237,354,348 nm. Results: The optimum extraction conditions of rutin and luteolin in “Wudang No.2 honeysuckle” were as follows: the solvent was 60% ethanol, the ratio of material to liquid was 1:30, the ultrasonic powers were 350 and 250 w, respectively. Time was 50,60 min. The average contents of chlorogenic acid, loganin, rutin and luteolin in the samples were 10.27, 6.33, 0.401 and 0.450 mg · g-1, respectively. Conclusion: The method is simple, accurate and reproducible, providing reference for its quality control and further development and utilization.