[关键词]
[摘要]
目的 建立桂花Osmanthus fragrans果实HPLC指纹图谱及9种化学成分的含量测定方法,为桂花果实的质量控制提供科学依据。方法 采用YMC-Pack ODS-A色谱柱(250 mm×4.6 mm,5 μm),以乙腈-水(含0.1%磷酸)溶液为流动相进行梯度洗脱,体积流量1.0 mL/min,柱温25℃,进样量10 μL,检测波长210 nm,对不同产地桂花果实样品进样分析;采用国家药典委员会“中药色谱指纹图谱相似度评价系统”(2012版),建立桂花果实的指纹图谱,同时测定其中9种化学成分含量。结果 对不同产地20批桂花果实样品进行指纹图谱研究,共标定了24个峰,指认出其中9个色谱峰。含量测定结果表明,女贞苷G13、特女贞苷、新女贞苷及红景天苷为桂花果实中主要化学成分。经方法学考察,测定方法的精密度和重复性良好,样品在24 h内稳定;红景天苷、毛蕊花糖苷、新女贞苷、特女贞苷、异麦角甾苷、女贞苷G13、槲皮素、芹菜素、山柰酚在一定质量浓度范围内线性良好,加样回收率均在95%~105%。结论 建立的桂花果实HPLC指纹图谱及9种化学成分的含量分析方法稳定、可靠,可为桂花果实的质量控制及综合开发提供参考。
[Key word]
[Abstract]
Objective To establish the HPLC fingerprint and simultaneously determination method for nine chemical components from fruits of Guihua (Osmanthus fragrans, OF), so as to provide reference for the quality control of OF fruits. Methods The separation was developed on YMC-Pack ODS-A column (250 mm×4.6 mm, 5 μm) by gradient elution with acetonitrile-water (containing 0.1% of phosphoric acid) as mobile phase. The flow rate was 1.0 mL/min, the column temperature was 35 ℃, the injection volume was 10 μL, and the detection wavelength was set as 210 nm. The fingerprint of OF fruits was established by using the similarity evaluation system of chromatographic fingerprint of TCM of the State Pharmacopoeia Committee (2012 Edition), and the contents of nine chemical components were determined simultaneously. Results The fingerprints of 20 batches of OF fruits from different areas were studied and a total of 24 peaks were calibrated and nine of them were quantitative analyzed. The results revealed that nuezhenide G13, spenuezhenide, neonuezhenide, and salidroside were the major compounds for OF fruits. According to the methodological investigation, the precision and repeatability were good, and the sample was stable within 24 h. Moreover, the linear ranges of nine chemicals, named salidroside, verbascoside, neonuezhenide, spenuezhenide, isoergosteroside, nuezhenide G13, quercetin, apigenin and kaempferol were all good and their recovery rate ranged from 95% to 105%. Conclusion The HPLC fingerprint combined with the simultaneous determination of nine chemical components analysis method established in this study are stable and reliable, which can provide the basis for the quality control and comprehensive utilization of OF fruits.
[中图分类号]
R286.2
[基金项目]
湖南省教育厅优秀青年项目(18B407);长沙市科技计划项目(kq2009024)