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Method for enzymatic reaction-based synthesis of maltitol esters in nonaqueous phase and purification preparation of the maltitol esters

An enzymatic reaction, maltitol technology, applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of difficult control of the system, uniform preparation of sugar alcohols and fatty acids, high cost, and improve application pertinence. , high food safety, the effect of clean production process

Inactive Publication Date: 2012-07-18
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The biggest problem in the synthesis reaction is that sugar alcohols and fatty acids are incompatible with each other. Therefore, a suitable reaction system must be selected. At present, there are microemulsion systems, but the system is difficult to control and the separation of the final product is difficult; ionic liquid systems, but the viscosity is too high. The quality is slow and the cost is high; there are also supercritical systems and solvent-free systems, such as patent 99113469.9 (homogeneous solvent-free production of sucrose esters)
At present, the research on enzymatic synthesis of sugar esters in non-aqueous phase is mainly carried out in a single organic solvent, but it is difficult to prepare sugar alcohols and fatty acids into a uniform system with a single organic solvent. If a mixed solvent system is used, both Satisfy the high hydrophobicity to ensure the enzyme activity and satisfy the solubility of the substrate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The reaction solvent is dimethyl sulfoxide (DMSO): tert-amyl alcohol=1:4 (v / v), maltitol: fatty acid=1:3 (m / m), the raw materials are placed in dimethyl sulfoxide, After all dissolved, add a certain volume ratio of tert-amyl alcohol, equilibrate for 2 hours, add 10g / L immobilized lipase NOV435 to the reaction solution, immediately add 60g / L 4A molecular sieve to remove the water generated by the reaction. The reaction solution was placed in a Erlenmeyer flask with a cover, and reacted at 50°C, 180rpm constant temperature oscillation for 24h, 4A molecular sieve was activated at 250°C for 6h, and the reaction solvent was dehydrated by molecular sieve for more than 48h for later use.

[0015] After the reaction, the reaction solution was filtered to remove molecular sieves and immobilized lipase, and the solvent was removed by rotary evaporation. The concentrated reaction solution was subjected to chromatography on a silica gel column. The eluent was n-hexane: isopropanol: ...

Embodiment 2

[0017] The reaction solvent is dimethyl sulfoxide (DMSO): tert-amyl alcohol=1:4 (v / v), maltitol: fatty acid=1:4 (m / m), the raw materials are placed in dimethyl sulfoxide, After all dissolved, add a certain volume ratio of tert-amyl alcohol, equilibrate for 3 hours, add 15g / L immobilized lipase NOV435 to the reaction solution, and add 60g / L 4A molecular sieve after 12 hours to remove the water generated by the reaction. The reaction solution was placed in a Erlenmeyer flask with a cover, and reacted at 55°C and 180rpm constant temperature oscillation for 48h, 4A molecular sieve was activated at 250°C for 6h, and the reaction solvent was dehydrated by molecular sieve for more than 48h for later use.

[0018] After the reaction, the reaction solution was filtered to remove molecular sieves and immobilized lipase, and the solvent was removed by rotary evaporation. The concentrated reaction solution was subjected to chromatography on a silica gel column. The eluent was n-hexane: iso...

Embodiment 3

[0020] The reaction solvent is dimethyl sulfoxide (DMSO): tert-amyl alcohol=1:4 (v / v), maltitol: fatty acid=1:5 (m / m), the raw materials are placed in dimethyl sulfoxide, After all dissolved, add a certain volume ratio of tert-amyl alcohol, equilibrate for 3 hours, add 20g / L immobilized lipase NOV435 to the reaction solution, and add 60g / L 4A molecular sieve after 24 hours to remove the water generated by the reaction. The reaction solution was placed in a Erlenmeyer flask with a cover, and reacted at 60°C and 180rpm constant temperature oscillation for 120h. 4A molecular sieve was activated at 250°C for 6h, and the reaction solvent was dehydrated by molecular sieve for more than 48h for later use.

[0021] After the reaction, the reaction solution was filtered to remove molecular sieves and immobilized lipase, and the solvent was removed by rotary evaporation. The concentrated reaction solution was subjected to chromatography on a silica gel column. The eluent was n-hexane: is...

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Abstract

The invention discloses a method for enzymatic reaction-based synthesis of maltitol esters in a nonaqueous phase and purification preparation of the maltitol esters. In a nonaqueous phase, maltitol and fatty acids are synthesized into the maltitol esters in the presence of an immobilized lipase as a catalyst and then the maltitol esters are purified and treated by silica gel column chromatography and semi-prepared liquid phase preparation. The maltitol esters obtained by the method mainly are maltitol monoesters and through the purification preparation, the maltitol esters has high purity and comprise 91 to 93% of a maltitol monooctoate, 94 to 97% of a maltitol monolaurate, 93 to 95% of a maltitol monostearate and 90 to 92% of a maltitol monooleate. The method provided by the invention follows the trend that the existing emulsifier will be developed into a natural emulsifier having rich nutrients, multiple functions and low heat, realizes synthesis of the maltitol esters by an environmentally-friendly high-selectivity enzymatic synthesis method, realizes preparation of a series of high-purity maltitol monoester products through silica gel column chromatography and semi-prepared liquid phase preparation, improves the application pertinency of the maltitol esters, and richens emulsifier types.

Description

technical field [0001] The invention provides a method for synthesizing maltitol ester in a non-aqueous phase based on an enzymatic reaction and purifying and preparing it, belonging to the field of food biotechnology. Background technique [0002] At present, food emulsifiers in my country mainly include five categories: glycerin fatty acid esters, sucrose fatty acid esters, Span and Tween, soybean lecithin, sodium stearoyl lactylate and calcium stearoyl lactylate. With the trend of natural, nutritious, multi-functional and low-calorie development, maltitol esters are gradually being valued by people. Maltitol ester is a new type of nonionic surfactant, which is formed by condensation and esterification of maltitol and fatty acid. At present, there are very few research reports on maltitol ester at home and abroad. Maltitol ester not only has the same emulsifying effect as monoglyceride and sucrose ester, but also has a thickening effect. In particular, its emulsification ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C12P19/44C07H15/06C07H1/06
Inventor 陈洁何志勇王洁秦昉陶冠军曾茂茂
Owner JIANGNAN UNIV
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