高速逆流色谱法分离白葡萄皮中多酚类化合物  

Separation of polyphenols from white grape skin by high-speed counter-current chromatography

作　　者：罗兰馨 吴迪[2] 吴加辉[2] 张舒婷[3] 崔艳[2] 孙宝山[2] LUO Lan-xin WU Di WU Jia-hui ZHANG Shu-ting CUI Yan SUN Bao-shan(School of Traditional Chinese Materia Medica ,Shenyang Pharmaceutical University, Shenyang 110016, China School of Functional Food and Wine, Shenyang Pharmaceutical University, Shenyang 110016, China School of Pharmacy, Shenyang Pharmaceutical University, Shenyang 110016, China)

机构地区：[1]沈阳药科大学中药学院,辽宁沈阳110016 [2]沈阳药科大学功能食品与葡萄酒学院,辽宁沈阳110016 [3]沈阳药科大学药学院,辽宁沈阳110016

出　　处：《沈阳药科大学学报》2017年第3期261-265,共5页Journal of Shenyang Pharmaceutical University

摘　　要：目的建立分离白葡萄皮中多酚类化合物的高速逆流色谱(high speed counter-current chromatography,HSCCC)方法。方法采用正己烷-乙酸乙酯-水(体积比为1:50:50)的溶剂系统对白葡萄皮多酚粗提物进行HSCCC分离,采用超高效液相色谱-四级杆-飞行时间串联质谱(ultra performance liquid chromatography-quadrupole-time of flight-mass spectrometry,UPLC-Q-TOF-MS)对所得馏分进行定性分析,进一步采用制备液相分离制备多酚化合物单体。结果高速逆流分离得到3个馏分,经制备液相分离得到6个多酚化合物单体,经质谱鉴定和对照品对照鉴别为儿茶素(catechin,1)、表儿茶素(epicatechin,2)、山奈酚-3-O-葡萄糖苷(kaempferol 3-O-glucoside,3)、异槲皮苷(quercetin 3-O-glucoside,4)、fertaric acid(5)和槲皮素-3-O-葡萄糖醛酸苷(quercetin 3-O-glucuronide,6),其中化合物6为首次采用HSCCC分离得到。结论所建立的高速逆流色谱方法适用于分离白葡萄皮中的多酚化合物。Objective To develop an efficient method for the separation of polyphenols from white grape skins by high-speed counter-current chromatography（HSCCC）.Methods An optimized HSCCC condition with two-phase solvent system composed of Hex-EtOAc-H_2O（V：V：V=1：50：50） was used to separate grape skin polyphenols into various fractions.The tail to head elution mode was used with a flow rate of6.0 mL·min^-1 and a rotary speed of 800 r·min^-1.Moreover,an UPLC-Q-TOF/MS was applied to identify individual polyphenol in each of the fractions from HSCCC and the identified individual polyphenol was obtained by preparative-HPLC separation.Results Under the optimized condition,3 fractions in total were obtained from HSCCC.After identified by UPLC-Q-TOF/MS,6 compounds were obtained by preparativeHPLC separation with high yield and high purity.Conclusions The established method of HSCCC coupled with preparative-HPLC appeared to be very efficient,fast and economic for separation of six different polyphenols from white grape skins at industrial-scale.Compound 6 was separated by HSCCC for the first time.

关 键 词：高速逆流色谱 超高效液相色谱-四级杆-飞行时间串联质谱 高效液相色谱分离 多酚化合物 白葡萄皮 

分 类 号：R28[医药卫生—中药学]