[关键词]
[摘要]
目的 在大叶冬青Ilex latifolia化学成分研究基础上,建立测定大叶冬青中大叶冬青皂苷F(latifoloside F)、大叶冬青皂苷H(latifoloside H)、大叶冬青皂苷C(latifoloside C)、大叶冬青皂苷D(latifoloside D)、苦丁冬青皂苷F(kudinoside F)、苦丁茶冬青皂苷E(ilekudinoside E)6种三萜皂苷的HPLC测定方法。方法 采用Wonda Cract ODS-2(250 mm×4.6 mm,5 μm)色谱柱,乙腈-水为流动相,梯度洗脱,体积流量1 mL/min,检测波长为210 nm,柱温35℃。结果 6个皂苷分离度良好,具有良好的线性关系(r>0.999 2),平均加样回收率在99.52%~100.96%,RSD<2%。结论 该方法简单、准确,具有良好的重复性和稳定性,可为大叶冬青药材质量控制提供实验依据。
[Key word]
[Abstract]
Objective Based on the study of chemical composition research of Ilex latifolia, to develop an HPLC method for the simultaneous determination of latifoloside F, latifoloside H, latifoloside C, latifoloside D, kudinoside F and ilekudinoside E. The purity of the six saponins was confirmed by LC-MS. Methods Chromatographic separation was performed on a Wonda Cract ODS-2 column (250 mm×4.6 mm, 5 μm) with linear gradient elution of acetonitrile and water at a flow rate of 1 mL/min, and the detection wavelength was 210 nm. The mass spectrum was negative ion mode, the capillary temperature was 250℃, the solvent gas was nitrogen, the flow rate was 0.75 L/min, the spray voltage was 4.0 kV, and the lens voltage was 125V. Results The six saponins were well separated and all calibration curves showed good linearity within the test ranges (r> 0.999 2). The average recoveries were between 99.52% and 100.96%, and RSD values were less than 2%. Conclusion An accurate and simple method is first established for the qualitation and quantification of six saponins in I. latifolia. The results demonstrate that the method could be applied as a reliable quality control method for the seed of I. latifolia.
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[基金项目]
吉林省科技发展计划项目(20150311037YY);吉林省卫生计生科研计划项目(2014Z206);吉林省中医药科技项目(2014-ZD28)