CN102965405B - 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
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- CN102965405B CN102965405B CN201210480067.0A CN201210480067A CN102965405B CN 102965405 B CN102965405 B CN 102965405B CN 201210480067 A CN201210480067 A CN 201210480067A CN 102965405 B CN102965405 B CN 102965405B
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Abstract
本发明涉及水解酯化法制备含1,3-甘油二酯乳脂的方法，该方法包括以下步骤：（1）取新鲜牛奶，在常温条件下，离心分离，取上层金黄色清亮油状液体，即为乳脂；（2）将乳脂置于容器中，加入基于乳脂质量25%～35%的去离子水，基于乳脂质量0.4%～0.6%的脂肪水解酶，在恒温气浴中搅拌，水解反应；水解产物离心分离，取上层脂肪酸；（3）按3∶1～1.5∶1摩尔比向脂肪酸中加入甘油，混合，再按脂肪酸质量2%～4%的比例加入1,3-特异性脂肪酶，置于反应釜中，震荡反应；取反应液离心分离，弃去底层的脂肪酶和甘油，得到1,3-甘油二酯含量在39%以上的功能乳脂。The present invention relates to a method for preparing milk fat containing 1,3-diglyceride by hydrolysis and esterification. The method includes the following steps: (1) take fresh milk, and centrifuge it under normal temperature conditions, and take the upper layer of golden yellow clear oily liquid, namely (2) Put the milk fat in a container, add 25% to 35% deionized water based on the milk fat mass, and 0.4% to 0.6% lipolytic enzyme based on the milk fat mass, stir in a constant temperature air bath, and hydrolyze; Centrifuge the hydrolyzate and take the fatty acid in the upper layer; (3) add glycerol to the fatty acid at a molar ratio of 3:1 to 1.5:1, mix, and then add 1,3-specific lipase at a ratio of 2% to 4% of the fatty acid mass , placed in a reaction kettle, and shaken for reaction; the reaction solution was taken for centrifugation, and the lipase and glycerin at the bottom were discarded to obtain functional milk fat with a 1,3-diglyceride content of more than 39%.
Description
Technical field
The invention belongs to functional edible butterfat preparing technical field, be particularly first hydrolyzed the method preparation of resterification containing the method for 1,3-DAG butterfat.
Background technology
The 4th national nutrition of China and investigation of health conditions show, China approximately has 200,000,000 body weight for humans overweight, 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, suffers from obesity population and accounts 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 the diseases such as fat and type ii diabetes, cardiovascular and cerebrovascular diseases, some tumour and sleep disordered breathing have obvious correlationship, 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.Most research shows 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 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 examined by Japan medical science alliance, is classified as and has the nourishing function ester that reduces postprandial lipid metabolism and fat-reducing 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.In fresh milk, lipid content accounts for 3%～4%, 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 cow's milk fat is changed into the 1,3-DAG with nutrient health-care function, both there is the nutrition of the butterfat of improvement, there is again the meaning of development of new function butterfat.
Common triglyceride level method of modifying is all chemical method substantially, has that energy consumption is large, severe reaction conditions, and product color and weak flavor, has limited its application at field of food.Biological enzyme because gentleer, the environmental friendliness of reaction, selectivity are higher, product color and better flavor become the research emphasis of food oils modification technology.Existing patented technology " preparation of solvent-free system full-enzyme method is containing 1; method of 3-triglyceride butterfat " (number of patent application: the method using 2010105079365) is a step full-enzyme method, can obtain the butterfat of 1,3-DAG content more than 31%.
Summary of the invention
In order to improve target product content, the present invention adopts hydrolysis esterification legal system standby containing 1, the processing technology routine of 3-triglyceride butterfat, the fat in first hydrolyzed bovine Ruzhong obtains lipid acid, again lipid acid and glycerine generation esterification are generated to 1,3-triglyceride, reaches more than 39% 1,3-DAG dairy fat content in butterfat.
To achieve these goals, the present invention is by the following technical solutions:
The standby operation steps containing 1,3-DAG butterfat of hydrolysis esterification legal system is as follows:
(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 the deionized water based on butterfat quality 25%～35% and the fat hydrolase based on butterfat quality 0.4%～0.6%, in 45 ℃～55 ℃ constant temperature gas baths, stir hydrolysis reaction 12h～16h; By 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, then add based on 1 of lipid acid quality 2%～4% 3-specific lipase, concussion reaction 10h～16h under ℃ condition of temperature 50 C～60; By 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, in butterfat, the content of 1,3-DAG reaches more than 39%.
The enzymic activity of fat hydrolase described in step (2) under pH value 7.0,37 ℃ of conditions of temperature is 1200～1300 U/g.
Described in 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, first obtains lipid acid with enzymic hydrolysis butterfat, then through sn-1,3 immobilized lipases (business enzyme) esterification obtains 1,3-triglyceride butterfat, novel technique can make the content of 1,3-DAG in 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) in product of the present invention, the content of 1,3-DAG can reach more than 39%.Preparation condition gentleness of the present invention, consumes energy little, and it is golden yellow solid-state that the cream product containing 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 by the triglyceride level in cow's milk effectively, has improved the nourishing function of cow's milk, makes cow's milk be more suitable for the special population such as obesity, hyperglycemia and eats;
(3) in 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, do not have hazardous and noxious substances to produce, products therefrom comprises triglyceride level, triglyceride, Tegin 55G, lipid acid that can safe edible, has guaranteed edible safety and the environment friendly of product;
(4) cream product containing 1,3-DAG that the present invention obtains can improve 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 in medicine, makeup and chemical industry, apply.
Embodiment
Below in conjunction with concrete example, the present invention is described further.
Embodiment 1:
The standby method containing 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 the deionized water based on butterfat quality 30% and the fat hydrolase based on butterfat quality 0.5%, in 50 ℃ of constant temperature gas baths, stir hydrolysis reaction 14h; 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, then add 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; In butterfat, the content of 1,3-DAG is 40.16%.
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, then adds 2.8% based on 1 of lipid acid quality, 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; In butterfat, the content of 1,3-DAG is 39.03%.
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, then adds 3% based on 1 of lipid acid quality, 3-specific lipase; 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; In butterfat, the content of 1,3-DAG is 39.34%.
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, then adds 3.3% based on 1 of lipid acid quality, 3-specific lipase; 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; In butterfat, the content of 1,3-DAG is 41.73%.
Claims (3)
1. the standby method containing 1,3-DAG butterfat of hydrolysis esterification legal system, is characterized in that comprising following operation steps:
(1) get fresh milk, centrifugation 30min under rotating speed 5000r/min condition, gets the golden yellow limpid oily liquids in upper strata, is butterfat;
(2) in butterfat, add the deionized water based on butterfat quality 25%～35% and the fat hydrolase based on butterfat quality 0.4%～0.6%, in 45 ℃～55 ℃ constant temperature gas baths, stir hydrolysis reaction 12h～16h; By hydrolysate, centrifugation 30min under rotating speed 5000r/min condition, 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, then add based on 1 of lipid acid quality 2%～4% 3-specific lipase, concussion reaction 10h～16h under ℃ condition of temperature 50 C～60; By 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, in butterfat, the content of 1,3-DAG is more than 39%.
2. the method for claim 1, is characterized in that: the enzymic activity of fat hydrolase described in step (2) under pH value 7.0,37 ℃ of conditions of temperature is 1200～1300U/g.
3. the method for claim 1, is characterized in that: described in step (3) 1, the enzymic activity of 3-specific lipase under pH value 6.8,37 ℃ of conditions of temperature is 500～600U/g.
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| CN201210480067.0A CN102965405B (en) | 2012-11-23 | 2012-11-23 | Method for preparing 1, 3-diglyceride-containing cream through hydrolytic esterification method |
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| CN201210480067.0A CN102965405B (en) | 2012-11-23 | 2012-11-23 | Method for preparing 1, 3-diglyceride-containing cream through hydrolytic esterification method |
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| 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 microcrystalline oat bran to emulsify diglyceride instead of milk fat |
| CN116268103A (en) * | 2023-03-27 | 2023-06-23 | 厦门取福健康科技有限公司 | A kind of 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 |
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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 |
|---|
| 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;杨继国等;《中国油脂》;20090320;第34卷(第03期);摘要、2.1.2-2.1.3部分 * |
| 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》.2009,第34卷(第03期),摘要、2.1.2-2.1.3部分. |
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