一点红药材中异槲皮苷的分离鉴定及指纹图谱研究
Isolation and identification of isoquercitrin and HPLC fingerprint study of Herba Emiliae
分类号:
出版年·卷·期(页码):2012,32 (5):0-0
DOI:
10.16155/j.0254-1793.2017.01.01
-----摘要:-------------------------------------------------------------------------------------------
目的: 从一点红药材中分离黄酮类化合物异槲皮苷,同时建立一点红的HPLC指纹图谱分析方法。 方法: 采用半制备高效液相色谱法分离异槲皮苷,并以氢谱(1H-NMR)、碳谱(13C-NMR)、质谱(MS)确定其结构。采用高效液相色谱技术分析指纹图谱;色谱条件:苏州环球C18(250 mm×4.6 mm,5 μm)色谱柱,乙腈-0.4%醋酸为流动相,梯度洗脱,流速1 mL·min-1,检测波长273 nm。 结果: 分离得到异槲皮苷,其纯度>98%;按照中国药典规定,11批一点红指纹图谱相似度均在0.9以上,确定了16个共有峰。 结论: 半制备高效液相色谱法制备异槲皮素方法简单、高效,指纹图谱分析方法准确性高、重复性较好,可作为一点红质量评价的依据。
-----英文摘要:---------------------------------------------------------------------------------------
Objective: To isolate the flavonoid compound isoquercitrin from Herba Emiliae and establish the HPLC fingerprint of Herba Emiliae. Methods: Isoquercitrin was isolate from Herba Emiliae by semi-preparative HPLC, and its chemical structures was elucidated by 13C-NMR, 1H-NMR and MS. The fingerprint was analyzed by HPLC; chromatographic conditions: Suzhou universal C18(250 mm×4.6 mm, 5 μm) chromatographic column was adopted, the mobile phase was acetonitrile-0.4% acetic acid with elution gradient at the flow rate of 1 mL·min-1, the detection wavelength was set at 273 nm. Result: The purity of isoquercitrin was above 98%. In accordance with the provisions of China pharmacopoeia, 11 batches of Herba Emiliae fingerprint had good similarity. Sixteen common peaks in chromatograms were determined. Conclusion: Semi-preparative HPLC is a simple and efficient method to prepare isoquercitrin. Fingerprint analysis method, being with high accuracy and repeatability, can be used in the quality control of Herba Emiliae.
-----参考文献:---------------------------------------------------------------------------------------
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