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林产化学与工业 ›› 2015, Vol. 35 ›› Issue (6): 133-140.doi: 10.3969/j.issn.0253-2417.2015.06.022

• 研究报告 • 上一篇    下一篇

桑叶总多酚筛选和分离纯化工艺研究

周昊, 李文君, 张俊, 张宇思, 颜新培, 王成章   

  1. 1. 1.湖南省蚕桑科学研究所, 湖南 长沙 410127;
    2. 中国林业科学研究院 林产化学工业研究所;生物质化学利用国家工程实验室;国家林业局 林产化学工程重点开放性实验室;江苏省 生物质能源与材料重点实验室, 江苏 南京 210042
  • 收稿日期:2015-06-20 出版日期:2015-12-25 发布日期:2015-12-28
  • 通讯作者: 颜新培,男,研究员,博士,硕士生导师,主要从事种质创新与资源生态利用研究;E-mail:yanxinpei@sina.com E-mail:yanxinpei@sina.com
  • 作者简介:周昊(1982—),女,江苏盐城人,助理研究员,硕士,主要从事生物质化学提取加工利用研究
  • 基金资助:
    “十二五”国家科技支撑计划资助项目(2012BAD36B07)

Screening, Separation and Purification of Mulberry Leaf Polyphenols

ZHOU Hao, LI Wen-jun, ZHANG Jun, ZHANG Yu-si, YAN Xin-pei, WANG Cheng-zhang   

  1. 1. The Sericultural Research Institute of Hunan Province, Changsha 410127, China;
    2. Institute of Chemical Industry of Forest Products, CAF;National Engineering Lab.for Biomass Chemical Utilization;Key and Open Lab.of Forest Chemical Engineering, SFA;Key Lab.of Biomass Energy and Material, Jiangsu Province, Nanjing 210042, China
  • Received:2015-06-20 Online:2015-12-25 Published:2015-12-28

摘要: 采用超声波和微波协同提取桑叶总多酚,Folin-Ciocalte法分析不同品种桑叶的总多酚含量,运用单因素试验和响应面法优化提取工艺,并考察不同种类大孔树脂对桑叶总多酚的纯化效果。结果表明,18个品种桑叶中大墨斗的总多酚质量分数最高,达到2.072 %;灃24×苗33总多酚质量分数最低,仅为1.035 %。湖桑87桑叶总多酚最佳提取工艺为:1 g桑叶粉末,液料比20 :1(mL :g),提取时间93 s,微波功率326 W,超声波功率304 W,粗提物得率为14.7 %,纯度为10.87 %。筛选得到的较适合桑叶总多酚纯化的H103树脂的吸附量为15.57 mg/g,解吸率为88.67 %,且较短时间内达到吸附平衡与解吸平衡。上样时吸附柱体积40 mL,上样量15 g粗提物,桑叶总多酚的最佳质量浓度为3 g/L,此时最佳洗脱条件为乙醇体积分数60 %、洗脱流速2 mL/min、洗脱体积80 mL,此条件下,桑叶总多酚纯度由10.87 %提高到65.45 %,纯化过程中桑叶总多酚得率为84.7 %。

关键词: 桑叶总多酚, 超声波微波协同提取, 响应面优化, 大孔树脂纯化

Abstract: Ultrasonic-microwave combined technology was used to extract polyphenols from the mulberry leaves and Folin-Ciocalte method was applied to analyze the content of polyphenols in different types and parts of mulberry leaves.The single factor and response surface methodology were successfully used to optimize the extraction conditions.Furthermore, the purification effects of different macroporous resins on the polyphenols were analyzed.The results showed that the highest content of polyphenols was 2.072 % from the type of Damodou, and the polyphenols content of Feng 24×Miao 33 was the lowest(1.035%) among eighteen varieties of mulberry leave.The optimal extraction conditions were 1 g Hu-sang87, liquid to solid ratio 20:1(mL:g), the extraction time 93 s, microwave power 326 W, ultrasonic power 304 W.Meanwhile, the yield of crude extracts was 1.598 % and the purity was 10.87 %.The most suitable resin for this purification was H103 with adsorbing capacity of 15.57 mg/g, desorption ratio of 88.67 % and short adsorption and desorption equilibrium time.The best adsorbing condition of polyphenols sample solution were adsorption column volume 40 mL, loading quantity of 15 g crude extract, mass concentration 3 g/L and the best elution conditions were ethanol volume fraction 60 %, flow rate 2 mL/min, elution volume 80 mL.Then, the purity of polyphenol increased from 10.87 % to 65.45 % under these conditions, and in the process of purification, the total yield was 84.7 %.

Key words: mulberry leaf polyphenols, ultrasonic-microwave combined extraction, response surface optimization, macroporous absorbent resins

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