论文总字数：17572字

摘 要

基于转糖基反应的酶转化法是目前生产α-熊果苷的主要手段，但该法获得酶转化液中含有高浓度的糖类底物与副产物，增加了熊果苷的分离纯化难度。

本研究针对目前熊果苷分离纯化受到高浓度残糖干扰的问题，采用了活性炭吸附法分离纯化熊果苷。以模拟高糖体系熊果苷溶液为原料，首先进行熊果苷静态吸附与解吸过程的研究，考察了不同操作工艺对颗粒活性炭吸附及解吸熊果苷性能的影响，研究了其吸附熊果苷以及去除糖类杂质的规律。研究表明，在180g/ L的高葡萄糖浓度下，单位质量颗粒活性炭对熊果苷的吸静态附量量为107.2mg/ g，而对葡萄糖的静态吸附量为219.7mg/ g。在使用750ml 40℃的去离子水洗涤杂质和100ml 40℃的80%（v / v）乙醇以及50ml 40℃的70%（v / v）乙醇洗脱时，熊果苷的分离效率最高，葡萄糖的解吸率是82.50%，熊果苷的洗脱率是60.18%。

在此基础上，对颗粒活性炭柱进行了动态吸附和解吸熊果苷的考察。在优化的条件下（上样吸附体积为4床体积（BV），洗脱体积为8 BV，吸附流速为2BV/h，洗杂流速为1.2BV/h，洗脱流速为2.8BV/h，洗杂和洗脱温度为40℃），活性炭对熊果苷的实际吸附量达到117.44mg/g，熊果苷的洗脱率为81%，结晶后α-熊果苷的纯度≥99%，一次结晶收率达70%。

综上所述，颗粒活性炭在高糖体系中对熊果苷具有一定的吸附选择性，但解吸过程相对困难，因此需要从源头上减少残糖的积累。

关键词：熊果苷 活性炭 分离纯化 高糖体系

Separation and Purification of Arbutin Used by Activated Carbon in High-glucose System

Abstract

Enzymatic conversion based on transglycosylation is currently the main method of producing α-arbutin. However, the enzyme conversion solution obtained by this method contains high concentration of sugar substrates and byproducts, which increases the difficulty of separation and purification of α-arbutin.

In order to solve the problem that the separation and purification of arbutin interfered by high concentration of residual glucose, this study plans to use activated carbon to separate and purify arbutin. First, using the simulated high-glucose arbutin solution as raw material to study the static adsorption and desorption process of arbutin. Also, the effects of different operating processes on the adsorption and desorption were investigated, and the rules of adsorption of arbutin and removal of sugary impurities by activated carbon were studied. Studies have shown that at a high glucose concentration of 180 g/L, the amount of static adsorption of arbutin per unit mass of granular activated carbon is 107.2 mg/g, while the static adsorption of glucose is 219.7 mg/g. The arbutin separation efficiency is highest when using 750ml of deionized water at 40°C to remove impurities and 100ml of 80% (v / v) ethanol at 40°C and 50ml of 70% (v / v) ethanol at 40°C to desorb arbutin. . At this point, the desorption rate of glucose was 82.50%, and the elution rate of arbutin was 60.18%.

On this basis, the dynamic adsorption and desorption of arbutin from activated carbon columns was investigated. Under optimized conditions (adsorption volume is 4 bed volumes (BV), elution volume is 8 BV, adsorption flow rate is 2 BV/h, wash flow rate is 1.2 BV/h, elution flow rate is 2.8 BV/h, washing and elution temperature is 40°C) , the actual amount of arbutin adsorbed by per unit mass of activated carbon reaches 117.44 mg/g, the elution rate of arbutin is 81%. The purity of α-arbutin after evaporation and crystallization is ≥99%, and the yield of primary crystallization reaches 70%.

In summary, granular activated carbon has to some extend adsorption selectivity

for arbutin in a high- glucose system, but the desorption process is relatively difficult. Therefore, it is necessary to reduce the accumulation of residual glucose from the source.

Keywords: Arbutin; Activated carbon; Separation and purification; High-glucose system

目录

摘要 Ⅰ

Abstract Ⅱ

第一章 文献综述 ⒈

1.1 熊果苷 1

1.2 熊果苷的制备 1

1.2.1 合成法 2

1.2.2 酶转化法 2

1.3 熊果苷的分离纯化 3

1.3.1 大孔树脂吸附法 3

1.3.2 有机溶剂萃取法 3

1.3.3 活性炭吸附法 3

1.4 活性炭 4

1.4.1 活性炭对糖类物质的吸附 4

1.4.2 活性炭对苷类物质的吸附 4

1.5 检测方法 4

1.6 研究目的和内容 4

第二章 实验材料与方法 6

2.1 实验试剂 6

2.2 仪器与设备 6

2.3 实验方法 7

2.3.1 熊果苷模拟液的静态吸附与解吸 7

2.3.2 熊果苷模拟液的动态吸附与解吸 8

2.3.3 熊果苷结晶回收 9

2.4 分析方法 9

2.4.1 葡萄糖的检测 9

2.4.2 熊果苷的检测与计算 9

2.4.3 本文相关计算方法 9

第三章 结果与讨论 10

3.1 熊果苷静态吸附与解吸 10

3.1.1 静态条件下活性炭对熊果苷的吸附性能 10

3.1.2 静态洗杂工艺条件优化 10

3.1.3 静态洗脱工艺条件优化 11

3.2 熊果苷动态吸附与解吸 12

3.2.1 动态吸附熊果苷 12

3.2.2 动态洗杂的影响 13

3.2.3 动态洗脱 14

3.2.4 回收与结晶 16

第四章 结论与展望 17

4.1 结论 17

4.2 展望 17

参考文献 18

致 谢 20

第一章 文献综述

1.1 熊果苷

熊果苷(arbutin)是一种在熊果的叶子细胞里发现的天然成份。熊果苷具有较高的天然美白活性，而且能有效抑菌、镇咳、祛痰、平喘、抗炎等，在临床以及化妆品行业应用广泛^[1-2]。

熊果苷通常为白色的针状结晶或粉末，易溶于水、甲醇、乙醇等^[3]。此外，熊果苷稳定性不是很高，容易在酸性条件下被水解，加入适量的维生素E可使其更稳定，而加入适量的亚硫酸氢钠可防止熊果苷变黑。

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