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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。
OBJECTIVE: To isolate flavonoid isoquercitrin from reddish medicinal herbs and to establish a little red HPLC fingerprinting method. Methods: Isoquercitrin was separated by semi-preparative high performance liquid chromatography and its structure was confirmed by 1H-NMR, 13C-NMR and MS. The chromatographic conditions were: C18 (250 mm × 4.6 mm, 5 μm) column with acetonitrile-0.4% acetic acid as mobile phase and gradient elution with a flow rate of 1 mL · min-1 Wavelength 273 nm. Results: The isoquercitrin was isolated with the purity of> 98%. According to the Chinese Pharmacopoeia, the similarity of fingerprints of 11 batches of red spots was above 0.9, and 16 common peaks were identified. Conclusion: The method of semi-preparative high performance liquid chromatography for the preparation of isoquercetin is simple and efficient. The fingerprinting method has the advantages of high accuracy and repeatability, and can be used as the basis for the evaluation of the red quality.