一点红药材中异槲皮苷的分离鉴定及指纹图谱研究

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,5μm)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。

Isolation and identification of isoquercitrin andHPLC fingerprint study of Herba Emiliae

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.