Method for improving yield of sucrose-6-acetate synthesized by enzyme means

An enzymatic synthesis and acetate technology, which is applied in the field of sweeteners, can solve problems such as low purification yield, complicated operation and post-processing, and excessive heavy metals in the product, so as to improve the reaction process, reduce the residual sugar content, and improve the reaction rate. Yield effect

Pending Publication Date: 2021-07-23
NANTONG CHANGHAI FOOD ADDITIVE
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Problems solved by technology

[0003] Sucrose-6-acetate is the key intermediate for the synthesis of sucralose. The current synthesis methods are mostly chemical methods, mainly the orthoester method and the dibutyltin oxide method, but these two chemical synthesis methods are also There are corresponding disadvantages: the orthoester method is simple to operate, but the yield is low; while the organotin method has a high yield, but there are disadvantages of complicated operation and post-processing, and there may be a risk of excessive heavy metals in the product, and the chemical method It is easy to cause chemical pollution and other problems
Enzymatic synthesis is an ideal green synthesis method with mild reaction conditions and less pollution. However, the yield of enzymatic synthesis is generally not high and unstable. Improve the yield of enzymatic synthesis of sucrose-6-acetate rate has become a technology hotspot
[0004] The Chinese invention patent with the publication number CN101886100A provides a method for enzymatically preparing sucrose-6-acetate, using non-aqueous system tert-butanol-dimethyl sulfoxide as the reaction medium, lipase catalyzes sucrose and vinyl acetate for Esterification reaction has mild reaction conditions and short reaction time; but its overall sucrose-6-acetate yield (conversion rate) is low; column chromatography is used for purification, which is not suitable for large-scale production, and the purification yield is also low. lower

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example 1

[0025] Resin pretreatment: Wash ECR-1030M lipase-immobilized resin (Hangzhou Chuangke Biotechnology Co., Ltd.) with 95% alcohol. After washing, wash with distilled water to remove ethanol, and obtain the pretreated resin by suction filtration.

[0026] Take 10L of deionized water, add disodium hydrogen phosphate and sodium dihydrogen phosphate to prepare a buffer solution with a pH of 7.5. Dissolve 50g (≥700u / mg enzyme activity) Candida lipase (Venoxin, Denmark) in the buffer, stir to dissolve the enzyme, and filter to remove insoluble components to obtain an enzyme solution. Add 180 g of pretreated resin to the enzyme solution, stir and adsorb at room temperature for 3 hours; the immobilization rate is 97.2% after testing. After the adsorption is completed, filter, and vacuum-dry the filter cake at 35°C until the water content is less than 5%, to obtain immobilized lipase.

Embodiment 1

[0028] Weigh 30g of sucrose into a four-necked flask, then pour 750ml of DMF into it, stir and dissolve in a 60°C water bath for about 40min. After the dissolution is complete, lower the temperature of the water bath to 35°C, pour 1000ml of tert-amyl alcohol into it, weigh and add 550g of vinyl acetate, stir and mix well, and when the temperature of the solution in the flask drops to 35°C, weigh and add 10g of Immobilized lipase, 35°C, 200r / min stirring reaction for 10h. After the reaction, filter with suction to remove the immobilized lipase and recover it. The filtrate is distilled under reduced pressure at 80° C. to remove the organic solvent at a pressure of -0.09 to -0.1 MPa to obtain sucrose-6-acetate. Sampling was carried out for liquid chromatography detection, and the calculated yield of sucrose-6-acetic acid was 89.8%.

Embodiment 2

[0030] Weigh 30g of sucrose into a four-neck flask, then pour 1000ml of DMF into it, stir and dissolve in a 50°C water bath for about 40min. After the dissolution is complete, lower the temperature of the water bath to 30°C, pour 1200ml of tert-amyl alcohol into it, weigh and add 625g of vinyl acetate, stir and mix well, and wait until the temperature of the solution in the flask drops to 35°C, weigh and add 15g of Immobilized lipase, 35°C, 200r / min stirring reaction for 10h. After the reaction, filter with suction to remove the immobilized lipase and recover it. The filtrate is distilled under reduced pressure at 85° C. to remove the organic solvent at a pressure of -0.09 to -0.1 MPa to obtain sucrose-6-acetate. Sampling was carried out for liquid chromatography detection, and the calculated yield of sucrose-6-acetic acid was 92.2%.

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Abstract

The invention relates to the technical field of sweeteners, in particular to a method for improving yield of sucrose-6-acetate synthesized by an enzyme means. The method for improving the yield of the sucrose-6-acetate synthesized by the enzyme means is characterized by comprising the following steps: adding cane sugar into a container, adding a DMF (Dimethyl Formamide) solvent, carrying out heating and stirring until the cane sugar is completely dissolved to obtain a DMF solution of the cane sugar; adding tert-amyl alcohol and vinyl acetate when the DMF solution of the cane sugar is cool, and carrying out uniform stirring and mixing; adding immobilized lipase, and allowing reaction under stirring; and then, carrying out suction filtration to remove the immobilized lipase after completion of the reaction and carrying out recovering, and performing reduced pressure distillation on the filtrate to remove the organic solvent, thereby obtaining the sucrose-6-acetate. According to the method for improving the yield of the sucrose-6-acetate synthesized by the enzyme means, the reaction yield of the sucrose-6-acetate is increased with content of residual sugar reduced and purity improved by adjusting types and dosages of solvents along with improvement of reaction process; and thus, the highest yield of the sucrose-6-acetate can be up to 97%.

Description

technical field [0001] The invention relates to the technical field of sweeteners, and relates to a method for improving the yield of enzymatic synthesis of sucrose-6-acetate. Background technique [0002] Sucralose is a functional sweetener made of sucrose. It has high sweetness, pure taste, low calorie, good solubility and stability, and many other advantages. It is an ideal sweetener. [0003] Sucrose-6-acetate is the key intermediate for the synthesis of sucralose. The current synthesis methods are mostly chemical methods, mainly the orthoester method and the dibutyltin oxide method, but these two chemical synthesis methods are also There are corresponding disadvantages: the orthoester method is simple to operate, but the yield is low; while the organotin method has a high yield, but there are disadvantages of complicated operation and post-processing, and there may be a risk of excessive heavy metals in the product, and the chemical method It is easy to cause chemical ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C12P19/12
CPCC12P19/12
Inventor 庄勇陈文华倪水华黄卫
Owner NANTONG CHANGHAI FOOD ADDITIVE
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