CN105624234A - Preparation method of solvent-free system sugar ester - Google Patents
Preparation method of solvent-free system sugar ester Download PDFInfo
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- CN105624234A CN105624234A CN201410600272.5A CN201410600272A CN105624234A CN 105624234 A CN105624234 A CN 105624234A CN 201410600272 A CN201410600272 A CN 201410600272A CN 105624234 A CN105624234 A CN 105624234A
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Abstract
The invention relates to a preparation method of sugar ester, and belongs to the fields of a food additive and a preparation method thereof. The preparation method of the solvent-free system sugar ester comprises the following steps: heating sucrose and lauric acid in a water bath according to a certain molar-mass ratio, oscillating and uniformly mixing; then, adding lipase and regulating pH value; continuing to stir and react for 12h, adding sodium pyrophosphate and reacting for 50h; and after the reaction, adding a chloroform lysate, filtering so as to obtain filtrate, and separating by virtue of thin layer chromatography, so that a finished product, namely the sugar ester, is obtained. According to the preparation method of the solvent-free system sugar ester, upon determination, the esterification rate of the finished product reaches 34.7% or above; and the prepared product, through HPLC analysis, contains 85% of monoester and 15% of diester. Moreover, the preparation method is simple and safe in process, strong in operability and applicable to industrial production.
Description
Technical field
The preparation method that the present invention relates to a kind of sugar ester, belongs to food additive and preparation method thereof field.
Background technology
Sugar ester is the nonionic surfactant that a big class is widely used in the industries such as food, medicine, chemical industry, and it has the advantages such as nontoxic, nothing sound of sighing, non-stimulated, easily biological-degradable.
Sugar ester product in the market is adopt chemical method synthesis mostly, and synthetic reaction carries out under high temperature, high pressure, and condition is harsher, and product is with color, and catalytic reaction poor selectivity, there is a lot of by-products to generate. And enzyme process overcomes these shortcomings, reaction condition is gentle, and product is prone to purification, lighter color; And enzyme has highly-solid selectively, regiospecificity and regioselectivity, chemical pure sugar ester can be synthesized, medical industry attracts attention very much, therefore there is important theory significance and using value. Become study hotspot about the enzymatic clarification of sugar ester in organic facies in recent years, but be substantially all employing substrate and modify (complicated operation, cost are high) and intensive polar solvent (poisonous).
Therefore it provides a kind of technique is simple, safe, workable, it is adaptable to the preparation method of industrialized production and the high sugar ester of product quality has good application prospect.
Summary of the invention
It is desirable to provide a kind of technique is simple, safe, workable, it is adaptable to the preparation method of industrialized production and the high sugar ester of product quality.
The preparation method of described Sugar Esters in Solvent-free System, comprises the following steps:
Vibrate under heating in water bath than by sucrose and lauric acid mixing by certain molal weight, it is subsequently adding lipase, and regulate pH value, after continuously stirred lower reaction 12 hours, add sodium pyrophosphate to react 50 hours, after reaction terminates, add chloroform lysate, filter to get filtrate, with the separating obtained product of thin layer chromatography and sugar ester.
Preferably, sucrose of the present invention is ground be dried into Powdered, and lauric acid is for 1:5 with molten state, sucrose and lauric molal weight ratio;
It is furthermore preferred that bath temperature of the present invention is 60 DEG C, pH value is 7.5, and mixing speed is 200rpm;
It is further preferred that the developing solvent of thin layer chromatography of the present invention is chloroform by volume: methanol: glacial acetic acid: water=81:9:8; 2 mixed liquors, developer is 10% phosphomolybdic acid ethanol solution.
The synthesis of sugar ester is a kind of more difficult reaction carried out, due to sugar with fatty acid respectively hydrophilic and hydrophobic material, immiscible as reaction substrate. Preparation method of the present invention as the solvent of reaction system, then can form syrup through the sugar ground using the lauric acid of molten state, adds the contact area of acid simultaneously, and lipase is as the enzyme of a kind of interfacial catalysis, thus can synthesize sugar ester relatively easily.
The preparation method of Sugar Esters in Solvent-free System of the present invention, after measured, product esterification yield reaches 34.7%, and preparation-obtained product is analyzed through HPLC, and monoester content is 85%, and diester is 15%. And technique is simple, safe, workable, it is adaptable to industrialized production.
Detailed description of the invention
Embodiment one:
Little triangular flask adds lmmol sucrose (ground be dried into Powdered) and 5mmo1 lauric acid (molten state), mix with the water bath chaders of 60 DEG C, rear addition 50mg lipase, and regulate pH value to 7.5, rotating speed 200rpm, add 0.6g sodium pyrophosphate after reaction 12h to react 50 hours, after reaction terminates, add chloroform lysate, filter to get filtrate, separate with thin layer chromatography, with chloroform: methanol: glacial acetic acid: water=81:9:8; 2 (V/V) launch as developing solvent, and developer is 10% phosphomolybdic acid ethanol solution, and dries about 15min, products therefrom and sugar ester through 105 DEG C. After measured, product esterification yield reaches 34.7%, and preparation-obtained product is analyzed through HPLC, and monoester content is 85%, and diester is 15%.
Claims (4)
1. the preparation method of Sugar Esters in Solvent-free System, comprises the following steps:
Vibrate under heating in water bath than by sucrose and lauric acid mixing by certain molal weight, it is subsequently adding lipase, and regulate pH value, after continuously stirred lower reaction 12 hours, add sodium pyrophosphate to react 50 hours, after reaction terminates, add chloroform lysate, filter to get filtrate, with the separating obtained product of thin layer chromatography and sugar ester.
2. the preparation method of Sugar Esters in Solvent-free System as claimed in claim 1, it is characterised in that described sucrose is ground be dried into Powdered, and lauric acid is for 1:5 with molten state, sucrose and lauric molal weight ratio.
3. the preparation method of Sugar Esters in Solvent-free System as claimed in claim 1 or 2, it is characterised in that described bath temperature is 60 DEG C, and pH value is 7.5, and mixing speed is 200rpm.
4. the preparation method of Sugar Esters in Solvent-free System as claimed in claim 1 or 2, it is characterised in that the developing solvent of described thin layer chromatography is chloroform by volume: methanol: glacial acetic acid: water=81:9:8; 2 mixed liquors, developer is 10% phosphomolybdic acid ethanol solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410600272.5A CN105624234A (en) | 2014-10-31 | 2014-10-31 | Preparation method of solvent-free system sugar ester |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410600272.5A CN105624234A (en) | 2014-10-31 | 2014-10-31 | Preparation method of solvent-free system sugar ester |
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| Publication Number | Publication Date |
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| CN105624234A true CN105624234A (en) | 2016-06-01 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201410600272.5A Pending CN105624234A (en) | 2014-10-31 | 2014-10-31 | Preparation method of solvent-free system sugar ester |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023197278A1 (en) * | 2022-04-15 | 2023-10-19 | 广州嘉德乐生化科技有限公司 | Solvent-free synthesis method for sucrose ester having high monoester content |
-
2014
- 2014-10-31 CN CN201410600272.5A patent/CN105624234A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023197278A1 (en) * | 2022-04-15 | 2023-10-19 | 广州嘉德乐生化科技有限公司 | Solvent-free synthesis method for sucrose ester having high monoester content |
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Application publication date: 20160601 |
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| WD01 | Invention patent application deemed withdrawn after publication |