Page 122 - 精细化工2019年第8期

第 36 卷第 8 期 精 细 化 工 Vol.36, No.8
201 9 年 8 月 FINE CHEMICALS Aug. 2019

催化与分离提纯技术
橙皮苷酶解液中橙皮素单糖苷的分离纯化

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王 幻 ，朱思明 1,4* ，夏 娜 1,2 ，王玉涛 ，陈 良 ，王振东
（1. 华南理工大学 食品科学与工程学院，广东 广州 510640；2. 喀什大学 生命与地理科学学院，新疆
喀什 844006；3. 山东奔月生物科技有限公司，山东 东营 257000；4. 广东省天然产物绿色加工与产品
安全重点实验室，华南理工大学，广东 广州 510640）

摘要：采用 6 种大孔吸附树脂和半制备液相色谱分离纯化橙皮苷酶解液中的橙皮素单糖苷（hesperetin-7-
O-glucoside，HMG），并通过红外、紫外和 XRD 验证了产物结构，同时采用羟基自由基清除实验探讨其抗氧化
活性。结果表明：HPD300 大孔树脂最适于酶解液中 HMG 的分离，且其对酶解液中主要组分的静态和动态总吸
附量分别为 48.35 和 35.82 mg/g，主要用于分离糖类杂质；以 10 BV 的体积分数 45%乙醇为洗脱剂，洗脱流速
1.2 mL/min，洗提物中 HMG 的质量分数经 HPLC 测定从 80.37%提高到 97.83%；洗提物经半制备液相进一步分
离纯化后得到单体 HMG，最终质量分数可达 98.21%，且 HMG 的羟基自由基清除能力（72.31%±1.00%）略高
于橙皮素，远高于橙皮苷。
关键词：橙皮苷酶解液；橙皮素单糖苷；分离纯化；大孔树脂；半制备液相
中图分类号：TS202.3 文献标识码：A 文章编号：1003-5214 (2019) 08-1610-07

Separation and Purification of Hesperetin-7-O-glucoside from
Hesperidin Hydrolysate

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WANG Huan , ZHU Si-ming 1,4* , XIA Na , WANG Yu-tao , CHEN Liang , WANG Zhen-dong
（1. School of Food Science and Engineering, South China University of Technology, Guangzhou 510640, Guangdong,
China; 2. College of Life and Geography Science, Kashi University, Kashi 844006, Xinjiang, China; 3. Shandong
Benyue Biological Technology Co., Ltd., Dongying 257000, Shandong, China; 4. Guangdong Province Key Laboratory
for Green Processing of Natural Products and Product Safety, South China University of Technology, Guangzhou
510640, Guangdong, China）
Abstract: Hesperetin-7-O-glucoside (HMG) from hesperidin hydrolysate was separated and purified by six
macroporous adsorption resins and high performance semi-preparative liquid chromatography. The
structure of the product was characterized by IR, UV-Vis and XRD. And the antioxidant activity of HMG
was investigated by hydroxyl radical scavenging test. The results showed that HPD300 macroporous resin
was the most suitable resin for the purification of HMG from enzymatic hydrolysis solution. The static and
dynamic total adsorption amounts of HPD300 resin to the main components of enzymatic hydrolysis
solution were 48.35 mg/g and 35.82 mg/g, respectively, which were mainly used for separation of sugar
impurities. The mass fraction of HMG in the eluent was increased from 80.37% to 97.83% using 10 BV of
45% ethanol as eluent at a flow rate of 1.2 mL/min. The final mass fraction of monomer HMG was 98.21%
after further separation and purification by semi-prepared liquid chromatography. And the hydroxyl radical
scavenging capacity of HMG was (72.31%±1.00%), slightly higher than that of hesperetin, much higher
than that of hesperidin.
Key words: hesperidin hydrolysate; hesperetin-7-O-glucoside; separation and purification; macroporous
resin; semi-preparative liquid chromatography

收稿日期：2019-01-29; 定用日期：2019-03-25; DOI: 10.13550/j.jxhg.20190099
基金项目：国家自然科学基金（U1203183）；高等学校学科创新引智计划资助（B17018）
作者简介：王 幻（1994—），女，硕士生，E-mail：569417247@qq.com。联系人：朱思明（1976—），男，教授，E-mail：lfsmzhu@scut.edu.cn。