玳玳果黄酮提取物效应组分新橙皮苷及柚皮苷敲出分离制备

Preparation and Knockout Separation of Effective Components Including Neohesperidin and Naringin in Daidai Flavonoid Extracts

目的对玳玳果黄酮提取物主要效应组分新橙皮苷及柚皮苷进行敲出分离纯化。方法采用制备薄层色谱法结合高压制备液相色谱分离技术,以氯仿-甲醇-水(13∶6∶2)下层溶液为展开体系,碘蒸气为定位显色剂,初步敲出分离新橙皮苷及柚皮苷;再用色谱性高压制备柱Ultiamte XB-C18(10 mm×250 mm,5μm),保护柱XB-C18(5μm),流速3.0 mL/min,检测波长284 nm,温度为室温,进样量100μL,进一步分离纯化新橙皮苷与柚皮苷,高效液相色谱法检测其纯度。结果制备薄层色谱法敲出分离得柚皮苷及新橙皮苷纯度为69.24%和75.45%,得率分别为23.15%和26.77%;高压制备液相色谱法进一步分离得柚皮苷及新橙皮苷纯度为98.81%和98.84%,得率分别为21.73%和24.87%。结论采用制备薄层色谱结合高压制备液相色谱可从玳玳果黄酮提取物敲出分离纯度大于98%的主要效应组分新橙皮苷及柚皮苷。

Objective:To isolate and purify the neohesperidin and naringin,which are the main effective components of the flavonoid extracts from Citrus Aurantiμm L.var daidai Tanaka.Methods:The preparative thin-layer chromatography,combined with preparative high-pressure liquid chromatography separation technology,was used to separate neohesperidin and naringin.The lower layer solution of chloroform-methanol-water(13:6:2)was used as the developing system,and iodine vapor was used as the local color developer.A preparative high-pressure column Ultiamte XB-C18(10×250 mm,5μm),with flow rate 3.0 mL/min,detection wavelength 284 nm and injection volume 100μL,was used for further separation and purification of neohesperidin and naringin.The purities of neohesperidin and naringin were measured by high-pressure liquid chromatography.Results:The purities of naringin and neohesperidin isolated by preparative thin-layer chromatography were 69.24%and 75.45%,and the yields were 23.15%and 26.77%respectively.After further separation by preparative high-pressure liquid chromatography,the purities of neohesperidin and naringin increased to 98.81%and 98.84%respectively,and the yields were 21.73%and 24.87%respectively.Conclusion:The preparative thin-layer chromatography combined with high-pressure preparative liquid chromatography can knock out the main effective components(neohesperidin and naringin)of the flavonoid extracts from Citrus Aurantiμm L.var daidai Tanaka with a purity greater than 98%.