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作 者:曹园[1,2] 吴永平[3] 周晓雯[1,2] 钱芳[1,2] 范慧佳[4] 王强[4]
机构地区:[1]南京中医药大学附属医院 [2]江苏省中医院肿瘤临床研究中心,江苏南京210036 [3]江苏省药物研究所,江苏南京210009 [4]中国药科大学中药分析教研室,江苏南京210009
出 处:《中国中药杂志》2012年第9期1254-1258,共5页China Journal of Chinese Materia Medica
基 金:国家"重大新药创制"科技重大专项(2009ZX09308-04)
摘 要:目的:采用HPLC-DAD,同时测定不同产地的10批卷柏和12批垫状卷柏中2种炔多酚(selaginellin,selaginellinB)和4种双黄酮(穗花杉双黄酮,穗花杉双黄酮-7-甲醚,扁柏双黄酮,异柳杉双黄酮)的含量。方法:采用Agilent 1100高效液相色谱系统,Waters Cosmosil C18色谱柱(4.6 mm×250 mm,5μm),流动相乙腈-0.1%甲酸水溶液,梯度洗脱,流速1.0 mL.min-1,检测波长280,337 nm,柱温30℃。结果:所测样品中6种活性成分的量差异较大,穗花杉双黄酮在卷柏中的质量分数(5.628~9.184 mg.g-1)普遍高于垫状卷柏(0.823~7.131 mg.g-1),而selaginellin在垫状卷柏中的质量分数(0.123~0.593 mg.g-1)普遍高于卷柏(0.067~0.133 mg.g-1)。此方法加样回收率和线性范围均符合要求。结论:该方法简便快速、分离效果好、灵敏度高、重现性好,可为全面控制卷柏药材的质量提供参考。Objective: To establish a HPLC-DAD model for the simultaneous determination of two selaginellins(selaginellin and selaginellin B) and four biflavones(amentoflavone,sequoiaflavone,hinokiflavone and isocryptomerin) contained in 10 batches of Selaginella tamariscina and 12 batches of S.pulvinata produced in different areas.Method: The analysis was performed on a Waters Cosmosil C18 column(4.6 mm×250 mm,5 μm) eluted with acetonitril-0.1% formic acid as mobile phase in a linear gradient mode.The detection wavelength was set at 280,337 nm.The flow rate was kept at 1.0 mL·min-1,and the column temperature was 30 ℃.Result: The six active constituents showed significant different in content.Amentoflavone in S.tamariscina contains(5.628-9.184 mg·g^-1) is more than that contained in S.pulvinata(0.823-7.131 mg·g^-1),while selaginellin in S.pulvinata(0.123-0.593 mg·g^-1) is more than that contained in S.tamariscina(0.067-0.133 mg·g^-1).All the calibration curves showed good linear correlation coefficients(r〉0.999 7) over the wide test ranges.Conclusion: The developed HPLC-DAD method is simple,sensitive and accurate and has the good repeatability in separation,which is available for the quality control of S.tamariscina and S.pulvinata.
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