中低压制备色谱制备新绿原酸对照品的研究  

Preparation of Neochlorogenic Acid Reference Substances by Medium-low-pressure Preparative Chromatography

作　　者：倪付勇[1] 宋亚玲[1] 刘露[1] 赵祎武[1] 洪奎[1] 黄文哲[1] 王振中[1] 萧伟[1] 

机构地区：[1]江苏康缘药业股份有限公司/中药制药过程新技术国家重点实验室,连云港222000

出　　处：《世界科学技术-中医药现代化》2015年第9期1818-1822,共5页Modernization of Traditional Chinese Medicine and Materia Medica-World Science and Technology

基　　金：科学技术部国家重大新药创制项目(2013ZX09402203):现代中药创新集群与数字制药技术平台;负责人:王振中

摘　　要：目的:建立从金银花中分离制备新绿原酸对照品的方法。方法:利用HPD200A大孔树脂对金银花水提液中的新绿原酸富集,经中低压制备色谱分离制备金银花中新绿原酸单体,运用HPLC对新绿原酸进行含量测定。采用现代波谱技术ESI-MS、1H-NMR、13C-NMR进行结构鉴定。结果:新绿原酸的最佳纯化工艺为加5 BV水洗脱,收集水洗液,浓缩、干燥,得新绿原酸粗品;以乙腈-0.5%甲酸溶液(10:90)为流动相,流速20 m L?min-1,检测波长326 nm,进行分离纯化,分离制备的新绿原酸的纯度达98.86%,收率为89.1%。结论:该方法可有效制备高纯度的新绿原酸对照品,以用于中药新药中定性鉴别和含量测定。This study was aimed to establish a separation method for neochlorogenic acid reference substances from Lonicera japonica. Refined neochlorogenic acid in L. japonica water extract was separated and concentrated by HPD200 A macroporous resin, which was isolated and purified by medium-low-pressure preparative chromatography and determined by HPLC. The structure was identified by various spectroscopic data including ESI-MS, 1H-NMR and 13C-NMR. The results showed that the optimal purification technology conditions were as follows： washed with 5BV of water, collected elution, concentration, drying; neochlorogenic acid crude products were eluted with acetonitrile-0.5% formic acid solution（10：90） with the flow rate of 20 m L·min-1; and the detection wavelength was 326 nm. The contents of the prepared neochlorogenic acid reached to 98.86% and the yield was 89.1%. It was concluded that the method was effective for the preparation of neochlorogenic acid with high purity. It can be used to prepare the reference substances for quantitative analysis and content determination of Chinese materia medica.

关 键 词：新绿原酸 金银花 对照品 中低压制备色谱 

分 类 号：R284.2[医药卫生—中药学]