食品科学

• 分析检测 • 上一篇    下一篇

二维多通道色谱法分离松多酚的条件优化

曾祥宏1,王振宇1,2,*,李 辉1,左丽丽1   

  1. 1.哈尔滨工业大学食品科学与工程学院,极端环境研究所,黑龙江 哈尔滨 150090;
    2.东北林业大学林学院,黑龙江 哈尔滨 150040
  • 出版日期:2014-05-25 发布日期:2014-05-29
  • 通讯作者: 王振宇

Optimization of Two-Dimensional Multi-Channel Chromatographic Separation of Pine Polyphenols

ZENG Xiang-hong1, WANG Zhen-yu1,2,*, LI Hui1, ZUO Li-li1   

  1. 1. School of Food Science and Engineering, Institute of Extreme Environment, Harbin Institute of Technology, Harbin 150090, China;
    2. School of Forestry, Northeast Forestry University, Harbin 150040, China
  • Online:2014-05-25 Published:2014-05-29
  • Contact: WANG Zhen-yu

摘要:

以东北红松松塔为原料,采用本课题组设计的二维多通道色谱分离设备,确定其分离松多酚的最佳工艺条件。首先通过静态吸附解吸实验,筛选二维多通道色谱分离设备的固相介质和洗脱剂;然后进行单因素动态试验,考察影响二维多通道色谱设备分离效果的4 个因素:上样量、上样质量浓度、洗脱速率和色谱柱数量。结果表明:X-5大孔树脂为二维多通道色谱设备分离松多酚的最佳固相介质,0.5%甲酸-60%乙醇溶液为其最佳洗脱剂,其对松多酚的最大吸附量为 38.74 mg/g,解吸率达72.08%;二维多通道色谱设备分离松多酚的最佳工艺条件:上样量256 mg、上样质量浓度2.0 mg/mL、洗脱速率(200±20)mL/min和色谱柱联用数量4 根。在此条件下,松多酚纯度由2.37%提高到了23.257%,产率达到46.81%。

关键词: 二维多通道色谱, 松多酚, 分离纯化, 大孔树脂

Abstract:

A two-dimensional multi-channel chromatographic separator designed by our research group was used to purify
polyphenols extracted from the pinecones of Pinus koraiensis Sieb. et Zucc. from north-eastern China. The chromatographic
conditions were optimized. The stationary and eluent were selected by static adsorption and desorption experiments. Onefactor-
at-a-time design was used to investigate four factors influencing the separation efficiency of polyphenols by dynamic
adsorption, sample loading amount, sample concentration, eluent flow rate, and number of chromatographic columns used.
Results indicated that X-5 macroporous resin was the best stationary phase for polyphenol separation and the best elutent
comprised a mixture of 0.5% formic acid and 60% ethanol in water, providing maximum adsorption quantity of 38.74 mg/g and
maximum desorption rate of 72.08%. The optimal experimental conditions for chromatographic separation of polyphenols
were 256 mg of sample at a concentration of 2.0 mg/mL, eluent flowing at a rate of (200±20) mL/min and using 4
chromatographic columns. Under these conditions, the purity of polyphenols was increased from 2.37% to 23.257%, and the
recovery was 46.81%.

Key words: two-dimensional multi-channel chromatographic separator, pine polyphenols, separation and purification, macroporous resin

中图分类号: