[关键词]
[摘要]
目的 建立皂角刺的HPLC指纹图谱,并同时测定皂角刺中7,3',5'-三羟基-5-甲氧基二氢黄酮醇、3,3',5,5',7-五羟基二氢黄酮醇、槲皮素3种黄酮类成分的量。方法 采用Waters symmetry C18(250 mm×4.6 mm,5 μm)色谱柱,流动相为乙腈(A)-0.1%甲酸水(B)溶液,梯度洗脱,0~5 min,5%~13% A;5~20 min,13%~16% A;20~45 min,16%~20% A;45~50 min,20%~25% A;50~65 min,25% A;65~80 min,25%~40% A;体积流量0.9 mL/min;柱温25 ℃;检测波长338 nm。结果 对13批皂角刺药材进行研究,所得HPLC指纹图谱共标定14个共有峰,并对其中3个成分进行了测定,其质量浓度分别在0.091 3~5.840 0、0.176 3~11.280 0、0.014 0~0.895 0 mg/mL与峰面积呈良好线性关系(r≥0.999 2),平均加样回收率为98.97%~99.66%,RSD<2.5%。结论 该法具有较好的稳定性和重复性,为皂角刺药材的质量控制提供科学依据。
[Key word]
[Abstract]
Objective An HPLC method was developed to evaluate the quality of Gleditsiae Spina through three components determination and fingerprint analysis. Methods The assay was performed on Waters symmetry C18 (250 mm×4.6 mm, 5 μm) column. The mobile phase consisted of acetonitrile and 0.1% methanoic acid in water with gradient elution by PDA detection at 338 nm. Results Thirteen batches of Gleditsiae Spina were analyzed with the established method. In the fingerprint, 14 common peaks were marked and three of them were determined. The three compounds showed good linearity (r≥0.999 2) in the range of 0.091 3-5.840 0, 0.176 3-11.280 0, and 0.014 0-0.895 0 mg/mL, respectively. The average recoveries were 98.97%-99.66% with RSD<2.5%. Conclusion This method has good repeatability and stability and provides a new method for the quality control of Gleditsiae Spina.
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[基金项目]
山东省科学院科学技术发展计划项目(2014QN02);山东省科学院——枣庄产学研联合基金;泰山学者岗位专家;山东省科学院先导项目