CN102965405A - Method for preparing 1, 3-diglyceride-containing cream through hydrolytic esterification method - Google Patents
Method for preparing 1, 3-diglyceride-containing cream through hydrolytic esterification method Download PDFInfo
- Publication number
- CN102965405A CN102965405A CN2012104800670A CN201210480067A CN102965405A CN 102965405 A CN102965405 A CN 102965405A CN 2012104800670 A CN2012104800670 A CN 2012104800670A CN 201210480067 A CN201210480067 A CN 201210480067A CN 102965405 A CN102965405 A CN 102965405A
- Authority
- CN
- China
- Prior art keywords
- butterfat
- dag
- cream
- lipid acid
- reaction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Preparation Of Compounds By Using Micro-Organisms (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
The invention relates to a method for preparing 1,3-diglyceride-containing cream through a hydrolytic esterification method. The method comprises the following steps: (1) fresh milk is selected and is centrifugally separated under normal temperature, and superstratum golden yellow clear oily liquid is taken, i.e. the cream; (2) the cream is put in a container, is added with deionized water which accounts for 25%-35% of the mass of the cream and fatty hydrolase which accounts for 0.4%-0.6% of the mass of the cream and is stirred in a constant temperature water bath to be subjected to hydrolysis reaction; a hydrolytic product is centrifugally separated, and superstratum fatty acid is taken; (3) glycerol is added into the fatty acid according to the molar ratio of (3:1)-(1.5:1) to be mixed, 1,3-specific lipase which accounts for 2%-4% of the mass of the fatty acid is then added, and the mixture is put in a reactor to be subjected to oscillating reaction; and the reaction liquid is taken to be centrifugally separated, and the bottom fatty acid and glycerol are discarded so as to obtain the functional cream with the 1, 3-diglyceride content of above 39%.
Description
Technical field
The invention belongs to functional edible butterfat preparing technical field, the method preparation that particularly is hydrolyzed first resterification contains the method for 1,3-DAG butterfat.
Background technology
The 4th national nutrition of China and investigation of health conditions show that China has 200,000,000 body weight for humans overweight approximately, and more than 6,000 ten thousand people suffer from obesity.The adult of the U.S. 1/3rd suffers from obesity.In Canada, half population overweight is suffered from obesity population and is accounted for 13%, and the morbidity of European 16 state's obesities is 15%～30%.According to World Health Organization's prediction, by 2015, the whole world will have adult more than 700,000,000 fat.And obesity has obvious correlationship with diseases such as type ii diabetes, cardiovascular and cerebrovascular diseases, some tumour and sleep disordered breathings, and anti-obesity has become the key areas of health diet and protective foods research.
1,3-DAG (1,3-diacylglycerol, DAG) is the natural component of grease, is obtained by two molecules of fatty acids and glycerine esterification.Majority studies show that 1,3-DAG has the empty stomach of improvement and postprandial lipid metabolism level, reduces the functions such as body fat gathers, and has long-term edible safety.1,3-DAG has passed through the U.S. FDA authentication, be the food of " universally acknowledged safety (GRAS) ", and mouthfeel, color and luster, local flavor and common triglyceride level (triacy1g1ycerol, TAG) is as good as.In Japan, 1,3-DAG culinary art oil is classified as the nourishing function ester with reduction postprandial lipid metabolism and fat-reducing by the audit of Japan medical science alliance by government.In the U.S., 1,3-DAG can be used in the food such as spread food component, salad sauce, bakery, leisure snack.Lipid content accounts for 3%～4% in the fresh milk, and wherein triglyceride level accounts for more than 98%.The animal derived triglyceride level of excessive absorption has the risk of diseases such as causing hypertension, atherosclerosis, and this has limited the consumption of milk to a certain extent.Effectively triglyceride level in the cow's milk fat is changed into the 1,3-DAG with nutrient health-care function, both had the nutrition of the butterfat of improvement, have again the meaning of development of new function butterfat.
Common triglyceride level method of modifying all is chemical method basically, has large, the severe reaction conditions of energy consumption, and product color and weak flavor, has limited its application at field of food.Higher, the product color of gentleness, environmental friendliness, selectivity and better flavor become the research emphasis of food oils modification technology to biological enzyme because of reaction.(number of patent application: employed method is a step full-enzyme method to existing patented technology " method of preparing 1,3-diglyceride-containing milk fat in solvent-free system with all-enzymatic method " 2010105079365), can obtain 1,3-DAG content at the butterfat more than 31%.
Summary of the invention
In order to improve target product content, the present invention adopts hydrolysis esterification legal system for containing 1, the processing technology routine of 3-triglyceride butterfat, the fat in elder generation hydrolyzed bovine Ruzhong obtains lipid acid, again lipid acid and glycerine generation esterification are generated 1, the 3-triglyceride makes that the 1,3-DAG dairy fat content reaches more than 39% in the butterfat.
To achieve these goals, the present invention is by the following technical solutions:
Hydrolysis esterification legal system is as follows for the operation steps that contains 1,3-DAG butterfat:
(1) get fresh milk, centrifugation 30 min under rotating speed 5000r/min condition get the golden yellow limpid oily liquids in upper strata, are butterfat;
(2) in butterfat, add based on the deionized water of butterfat quality 25%～35% with based on the fat hydrolase of butterfat quality 0.4%～0.6%, in 45 ℃～55 ℃ constant temperature gas baths, stir hydrolysis reaction 12h～16h; With hydrolysate centrifugation 30min under rotating speed 5000 r/min conditions, get the lipid acid on upper strata;
(3) be that the ratio of 3:1～1.5:1 is mixed lipid acid and glycerine in molar ratio, add again based on 1 of lipid acid quality 2%～4% 3-specific lipase, concussion reaction 10h～16h under ℃ condition of temperature 50 C～60; With reaction solution centrifugation 10min under rotating speed 10000r/min condition, discard lipase and the glycerine of bottom, obtain being rich in the butterfat of 1,3-DAG, the content of 1,3-DAG reaches more than 39% in the butterfat.
The enzymic activity of fat hydrolase described in the step (2) under pH value 7.0,37 ℃ of conditions of temperature is 1200～1300 U/g.
Described in the step (3) 1, the enzymic activity of 3-specific lipase under pH value 6.8,37 ℃ of conditions of temperature is 500～600 U/g.
The present invention has adopted brand-new enzymolysis process, obtains lipid acid with enzymic hydrolysis butterfat first, again through sn-1,3 immobilized lipases (the commercial enzyme of using) esterification obtains 1,3-triglyceride butterfat, novel technique can make the content of 1,3-DAG in the butterfat bring up to more than 39% from 31%.The present invention has the meaning that significant process innovation and target product increase substantially.
The present invention compared with prior art has following advantage and beneficial effect:
(1) content of 1,3-DAG can reach more than 39% in the product of the present invention.Preparation condition of the present invention is gentle, and it is little to consume energy, and it is golden yellow solid-state that the cream product that contains 1,3-DAG of acquisition becomes at normal temperatures, and lovely luster has light fragrance, taste lubrication;
(2) the present invention is converted into 1,3-DAG with the triglyceride level in the cow's milk effectively, has improved the nourishing function of cow's milk, makes cow's milk be more suitable for the special populations such as obesity, hyperglycemia and eats;
(3) among the preparation method of the present invention, except a small amount of interpolation deionized water, glycerine, enzyme, do not add other poisonous and harmful solvents, reaction process comprises enzymolysis and enzyme process esterification, there is not hazardous and noxious substances to produce, products therefrom comprise can safe edible triglyceride level, triglyceride, Tegin 55G, lipid acid, guaranteed edible safety and the environment friendly of product;
(4) cream product that contains 1,3-DAG of the present invention's acquisition can improve the postprandial lipid metabolism level, minimizing body fat gathers.This product can be used in the numerous food such as ice cream, instant drink, bakery product, also can use in medicine, makeup and chemical industry.
Embodiment
Example below in conjunction with concrete is described further the present invention.
Embodiment 1:
The standby method that contains 1,3-DAG butterfat of hydrolysis esterification legal system comprises following operation steps:
(1) get fresh milk, centrifugation 30 min under rotating speed 5000r/min condition get the golden yellow limpid oily liquids in upper strata, are butterfat;
(2) in butterfat, add based on the deionized water of butterfat quality 30% with based on the fat hydrolase of butterfat quality 0.5%, in 50 ℃ of constant temperature gas baths, stir hydrolysis reaction 14h; The water intaking hydrolysis products, centrifugation 30min under rotating speed 5000 r/min conditions gets upper strata lipid acid;
(3) be that the ratio of 2.3:1 is mixed lipid acid and glycerine in molar ratio, add again 2.5% based on 1 of lipid acid quality, 3-specific lipase, concussion reaction 12.5h in 55 ℃ of reactors; Extract reaction solution, centrifugation 10min under rotating speed 10000r/min condition discards lipase and the glycerine of bottom, obtains being rich in the butterfat of 1,3-DAG; The content of 1,3-DAG is 40.16% in the butterfat.
Embodiment 2:
Step (1), (2) are with embodiment 1;
Step (3): the ratio that is in molar ratio 1.8:1 is mixed lipid acid and glycerine, adds 2.8% based on 1 of lipid acid quality again, 3-specific lipase, concussion reaction 14h in 58 ℃ of reactors; Extract reaction solution, centrifugation 10min under rotating speed 10000r/min condition discards lipase and the glycerine of bottom, obtains being rich in the butterfat of 1,3-DAG; The content of 1,3-DAG is 39.03% in the butterfat.
Embodiment 3:
Step (1), (2) are with embodiment 1;
Step (3): the ratio that is in molar ratio 2:1 is mixed lipid acid and glycerine, adds 3% based on 1 of lipid acid quality, the 3-specific lipase again; Concussion reaction 12h in 50 ℃ of reactors; Extract reaction solution, centrifugation 10min under rotating speed 10000r/min condition discards lipase and the glycerine of bottom, obtains being rich in the butterfat of 1,3-DAG; The content of 1,3-DAG is 39.34% in the butterfat.
Embodiment 4:
Step (1), (2) are with embodiment 1;
Step (3): the ratio that is in molar ratio 2.5:1 is mixed lipid acid and glycerine, adds 3.3% based on 1 of lipid acid quality, the 3-specific lipase again; Concussion reaction 13h in 53 ℃ of reactors; Extract reaction solution, centrifugation 10min under rotating speed 10000r/min condition discards lipase and the glycerine of bottom, obtains being rich in the butterfat of 1,3-DAG; The content of 1,3-DAG is 41.73% in the butterfat.
Claims (3)
1. hydrolysis esterification legal system is characterized in that comprising following operation steps for the method that contains 1,3-DAG butterfat:
(1) get fresh milk, centrifugation 30 min under rotating speed 5000r/min condition get the golden yellow limpid oily liquids in upper strata, are butterfat;
(2) in butterfat, add based on the deionized water of butterfat quality 25%～35% with based on the fat hydrolase of butterfat quality 0.4%～0.6%, in 45 ℃～55 ℃ constant temperature gas baths, stir hydrolysis reaction 12h～16h; With hydrolysate, centrifugation 30min under rotating speed 5000 r/min conditions gets the lipid acid on upper strata;
(3) be that the ratio of 3:1～1.5:1 is mixed lipid acid and glycerine in molar ratio, add again based on 1 of lipid acid quality 2%～4% 3-specific lipase, concussion reaction 10h～16h under ℃ condition of temperature 50 C～60; With reaction solution centrifugation 10min under rotating speed 10000r/min condition, discard lipase and the glycerine of bottom, obtain being rich in the butterfat of 1,3-DAG, the content of 1,3-DAG reaches more than 39% in the butterfat.
2. the method for claim 1, it is characterized in that: the enzymic activity of fat hydrolase described in the step (2) under pH value 7.0,37 ℃ of conditions of temperature is 1200～1300 U/g.
3. the method for claim 1 is characterized in that: described in the step (3) 1, the enzymic activity of 3-specific lipase under pH value 6.8,37 ℃ of conditions of temperature is 500～600 U/g.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210480067.0A CN102965405B (en) | 2012-11-23 | 2012-11-23 | Method for preparing 1, 3-diglyceride-containing cream through hydrolytic esterification method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210480067.0A CN102965405B (en) | 2012-11-23 | 2012-11-23 | Method for preparing 1, 3-diglyceride-containing cream through hydrolytic esterification method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102965405A true CN102965405A (en) | 2013-03-13 |
| CN102965405B CN102965405B (en) | 2014-05-28 |
Family
ID=47795841
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210480067.0A Expired - Fee Related CN102965405B (en) | 2012-11-23 | 2012-11-23 | Method for preparing 1, 3-diglyceride-containing cream through hydrolytic esterification method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102965405B (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103355419A (en) * | 2013-08-08 | 2013-10-23 | 陈昊然 | 1,3-diglyceride-enriched cream and preparation method thereof |
| CN109463458A (en) * | 2018-10-26 | 2019-03-15 | 安徽农业大学 | A kind of fresh cheese using controlled micro crystallization oat bran emulsification diglyceride substitution butterfat |
| CN116268103A (en) * | 2023-03-27 | 2023-06-23 | 厦门取福健康科技有限公司 | Probiotic milk shake containing MCT component and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101720821A (en) * | 2008-10-10 | 2010-06-09 | 花王株式会社 | Process for producing oil and fat rich in diacylglycerol |
| CN102008078A (en) * | 2010-10-12 | 2011-04-13 | 安徽农业大学 | Method for preparing 1,3-diglyceride-containing milk fat in solvent-free system with all-enzymatic method |
-
2012
- 2012-11-23 CN CN201210480067.0A patent/CN102965405B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101720821A (en) * | 2008-10-10 | 2010-06-09 | 花王株式会社 | Process for producing oil and fat rich in diacylglycerol |
| CN102008078A (en) * | 2010-10-12 | 2011-04-13 | 安徽农业大学 | Method for preparing 1,3-diglyceride-containing milk fat in solvent-free system with all-enzymatic method |
Non-Patent Citations (2)
| Title |
|---|
| 《中国油脂》 20090320 杨继国等 全酶法制备甘油二酯的研究(Ⅱ)__脂肪酸酶法酯化反应的工艺优化 摘要、2.1.2-2.1.3部分 1-3 第34卷, 第03期 * |
| 杨继国等: "全酶法制备甘油二酯的研究(Ⅱ)――脂肪酸酶法酯化反应的工艺优化", 《中国油脂》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103355419A (en) * | 2013-08-08 | 2013-10-23 | 陈昊然 | 1,3-diglyceride-enriched cream and preparation method thereof |
| CN103355419B (en) * | 2013-08-08 | 2015-01-21 | 陈昊然 | 1,3-diglyceride-enriched cream and preparation method thereof |
| CN109463458A (en) * | 2018-10-26 | 2019-03-15 | 安徽农业大学 | A kind of fresh cheese using controlled micro crystallization oat bran emulsification diglyceride substitution butterfat |
| CN116268103A (en) * | 2023-03-27 | 2023-06-23 | 厦门取福健康科技有限公司 | Probiotic milk shake containing MCT component and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102965405B (en) | 2014-05-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101940240B (en) | Method for preparing fish oil ethyl ester microcapsule from fish pomace | |
| CN107751418A (en) | A kind of preparation method of human milk fat structure fat substitutes | |
| CN104041817B (en) | Method for preparing longan ferment from longan kernel | |
| CN102965405B (en) | Method for preparing 1, 3-diglyceride-containing cream through hydrolytic esterification method | |
| CN103053713A (en) | Enzymatic catalysis prepared special grease for quick-frozen food and preparation method thereof | |
| CN106086098A (en) | The method improving enzyme process esterification enrichment fish oil n 3 fatty acid with ionic liquid | |
| JP2015530109A (en) | Method for producing ginkgo fermented liquor using thermostable amylase | |
| CN103865714B (en) | A kind of method utilizing low strength intermittent type ultrasonic assistant yellow rice wine brewage | |
| CN103598541A (en) | Avocado powder and preparation method thereof | |
| CN102429215A (en) | Linolenic acid microcapsules and preparation method thereof | |
| CN104996726B (en) | Utilize the method for the flat angle stratiomyiid larva production functional feedstuff additive of speck | |
| CN107937470B (en) | Method for synthesizing phytosterol ester in ionic liquid system by enzyme method | |
| CN1537946A (en) | Method of extracting dietary fiber from sogbean drges and chewing tablet | |
| Cerón et al. | Analysis of a biorefinery based on Theobroma grandiflorum (copoazu) fruit | |
| CN101100691A (en) | Method for extracting small peptides from pine pollen by using enzyme | |
| CN113416599A (en) | Passion fruit seed oil and preparation method thereof | |
| CN102578521A (en) | Scallop skirt seafood sauce and preparation method thereof | |
| CN101720905B (en) | Flavor yeast albumen powder and preparation method thereof | |
| CN102008078B (en) | Method for preparing 1,3-diglyceride-containing milk fat in solvent-free system with all-enzymatic method | |
| CN103734852B (en) | Preparation method of aspergillus-oryzae fermented beverage based on wheat-bran bean pulp | |
| CN101204216B (en) | Coffee partner containing octacosanol and manufacture method thereof | |
| CN102041204A (en) | Method for preparing tree-starch based natural biomass detergent | |
| CN105331645A (en) | Production method of diglyceride edible oil | |
| CN105238558B (en) | The method for reducing Cholesterol in Lard | |
| CN103710400A (en) | Method for preparing triglyceride containing rich conjugated linoleic acids at sn-2 site |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140528 Termination date: 20191123 |