朝鲜蓟中2种木犀草素类化合物液相制备条件优化  

Optimization of two luteolin derivatives preparation from artichoke by HPLC

作　　者：师明月 曹清明[1] 李群 钟文惠 王元清 刘志文 张喜平 SHI Ming-yue;CAO Qing-ming;LI Qun;ZHONG Wen-hui;WANG Yuan-qing;LIU Zhi-wen;ZHANG Xi-ping(Faculty of Food Science and Engineering,Central South University of Forestry and Technology,Changsha,Hunan 410004,China;Huiniei Agricultural Science and Technology Co.,Ltd,Changde,Hunan 415137,China;Changde Agriculture and Forestry Research Institute,Changde,Hunan 415000,China)

机构地区：[1]中南林业科技大学食品科学与工程学院,湖南长沙410004 [2]汇美农业科技有限公司,湖南常德415137 [3]常德市农林科学研究院,湖南常德415000

出　　处：《食品与机械》2019年第3期176-181,共6页Food and Machinery

基　　金：湖南省自然科学基金(编号:2016JJ5016);中南林业科技大学大学生研究性学习与创新性实验计划项目(编号:2018075)

摘　　要：研究了一种通过制备液相色谱从朝鲜蓟中分离得到2种木犀草素糖苷的方法。朝鲜蓟与70%乙醇浸提液通过AB-8型大孔树脂吸附,分别用20%,50%,80%乙醇洗脱,得到50%乙醇洗脱部位A27～29(4g);A27～29用RP-C18层析柱(270mm×80mm,40～60μm)吸附,分别用30%,48%,100%甲醇洗脱,得到C16～19目标组分0.32g,其中含目标组分H-01(10.4%)和H-02(5.1%);以目标组分的分离度和峰形为优化条件,研究了5种不同流动相组合及2种流速对目标峰分离效果的影响,基于最优条件制备,得到了纯度分别为97.8%和96.5%的H-01和H-02;通过质谱、~1 H-NMR和^(13) C-NMR表征,确定H-01和H-02分别为木犀草苷-7-芸香糖苷和木犀草素7-O-β-D-葡萄糖苷。该方法优化了木犀草素类化合物的分离纯化生产工艺,并在保证高回收率的条件下有效降低了杂质水平。This study describes a method for isolating two luteolin glycosides from artichokes(Cynara scolymus L.)by preparative liquid chromatography.The partion A27~29(4 g)of 50% ethanol eluent was achieved by two steps,70%ethanol extract of artichoke adsorbed by AB-8 macroporous resin and eluted with20% ethanol,50% ethanol and 80% ethanol successively.0.32 g of target part C16~19 with target components H-01(10.4%)and H-02(5.1%)was achieved by two steps,A27~29 adsorbed by RP-C18 stationary phase column(270 mm×80 mm,40~60μm)and eluted with 30%,48% and 100% methanol successively.Taking the resolution and shape of target peaks as optimization conditions,the effects of five different mobile phase combinations and two kinds of flow rates on the separation of target peaks were studied.Based on the optimal conditions,H-01 and H-02 with purity of 97.8% and 96.5%,respectively,were obtained.H-01 and H-02 were identified as luteolin-7-rutinoside and luteolin-7-O-β-D-glucoside,respectively,by mass spectrometry,1 H-NMR and 13 C-NMR analysis.This method can effectively reduce the impurity level under the condition of high recovery,and provide a new method for the development of the separation and purification process of luteolin compounds.

关 键 词：朝鲜蓟 木犀草素类化合物 制备 优化 

分 类 号：TQ28[化学工程—有机化工]