CN110438175A - A kind of method that light phase rice bran oil and conjugated linoleic acid transesterification after freezing separation prepare functional grease - Google Patents

A kind of method that light phase rice bran oil and conjugated linoleic acid transesterification after freezing separation prepare functional grease Download PDF

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Publication number
CN110438175A
CN110438175A CN201910869560.3A CN201910869560A CN110438175A CN 110438175 A CN110438175 A CN 110438175A CN 201910869560 A CN201910869560 A CN 201910869560A CN 110438175 A CN110438175 A CN 110438175A
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China
Prior art keywords
rice bran
bran oil
grease
conjugated linoleic
transesterification
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Pending
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CN201910869560.3A
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Chinese (zh)
Inventor
于殿宇
唐洪琳
陈俊
李丹
王旭
王彤
张宏伟
孙立娜
王立琦
江连洲
郑冬梅
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Northeast Agricultural University
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Northeast Agricultural University
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Priority to CN201910869560.3A priority Critical patent/CN110438175A/en
Publication of CN110438175A publication Critical patent/CN110438175A/en
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    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P7/00Preparation of oxygen-containing organic compounds
    • C12P7/64Fats; Fatty oils; Ester-type waxes; Higher fatty acids, i.e. having at least seven carbon atoms in an unbroken chain bound to a carboxyl group; Oxidised oils or fats
    • C12P7/6436Fatty acid esters
    • C12P7/6445Glycerides
    • C12P7/6454Glycerides by esterification

Abstract

The method that the present invention provides the light phase rice bran oil after a kind of freezing separation and conjugated linoleic acid transesterification prepares functional grease.This method takes carclazyte as crystallizing agent, gradient freezing centrifugation keeps unsaturated fatty acid rich, and carries out transesterification using 435 lipase enzymatic conjugated linoleic acid of Novozym, is prepared for functional grease, it solves the problems, such as the recycling of organic solvent, improves the high-valued of rice bran.As the thermal stability of the raising unsaturated fatty acid complex of degree of unsaturation can gradually decrease, along with the influence of the factors such as crystallization temperature and condition, so that it may realize that different structure component is able to separation, enrichment in fatty acid mixed.Selection gradient freezing centrifugation point proposes the process conditions of rice bran oil, the result shows that preparing the optimum condition of functional grease: the additive amount 9% of lipase, 60 DEG C of reaction temperature, mixing speed 200rpm and reaction time 26h, the esterification yield of CLA is up to 35% in obtained grease.

Description

Light phase rice bran oil and conjugated linoleic acid transesterification after a kind of freezing separation prepare function The method of property grease
Technical field
The present invention relates to the light phase rice bran oils after a kind of freezing separation to prepare functional grease with conjugated linoleic acid transesterification Method, and in particular to a kind of gradient freezing centrifuge separation rice bran oil is enriched with unsaturated fatty acid, the light phase after freezing separation The method that rice bran oil and conjugated linoleic acid prepare functional grease improves the high-valued quality of rice bran oil, inhibits solvent fractionation Harm to product, reduces production cost.
Background technique
Rice bran is the Main By product during paddy processing, the rice bran oil prepared using aqueous enzymatic method, and nutriment is rich Richness has very important nutrition Development volue, market prospects containing nutritional ingredients such as tocopherol, phytosterol and oryzanol It is wide.With the development of domestic economy and the raising of living standards of the people, answer Devoting Major Efforts To Developing rice bran oil in filed of daily-use chemical industry Research dynamics, to improve rice bran value-added content of product.
Lot of documents report conjugated linoleic acid can prevent and treat atherosclerosis, breast cancer, cutaneum carcinoma, colon Cancer, the diseases such as prostate cancer, while CLA, which can reduce Body fat retention, growth promotion, improve food conversion ratio etc., important work With.But conjugated linoleic acid, as a kind of fatty acid, eating mouth feel is poor, and conjugated linoleic acid esterification is prepared functional grease, Solves this phenomenon.
It is enriched with unsaturated fatty acid the centrifugation of rice bran oil gradient freezing, the light phase rice bran oil after freezing separation and conjugation are sub- Oleate exchange system is for functional grease.
Rice bran oil often will appear oxidative rancidity in storage, lead to that the acid value of rice bran oil increases, quality deteriorates, goods The frame phase shortens.It, only need to be using acetone and ethyl alcohol as organic solvent, in organic solvent to obtain required polyvalent unsaturated fatty acid It is inside mixed into fatty acid, cooling processing then is carried out to it, so that it may divide polyvalent unsaturated fatty acid from numerous fatty acid It separates out and.The process has the advantages such as easy to operate, principle is simple, but simultaneously there is also low separation efficiency, must recycle The drawbacks such as a large amount of organic solvents.Therefore the residue problem for solving rice bran oil organic solvent is to restrict rice bran oil as new oil Crucial problem.
This method is centrifugated rice bran oil using gradient freezing, is enriched with unsaturated fatty acid, and utilizes lipase-catalyzed Conjugate linoleate exchange system removes free fatty acid using molecular distillation technique for functional grease.
Principle be it is similar by the physical property of ingredient every in fatty acid mixed, in this case, using traditional point It is difficult to realize really separate from method.But if specific crystallizing agent is added in fatty acid mixed, then different structure Fatty acid just will form the nuclei of crystallization.Wherein, since the thermal stability of unsaturated fatty acid complex is than saturated fatty acid complex Thermal stability wants low, and as the thermal stability of the raising unsaturated fatty acid complex of degree of unsaturation can gradually decrease, then In addition the influence of the factors such as crystallization temperature and condition, so that it may realize that different structure component is separated in fatty acid mixed.
Therefore, this method takes carclazyte as crystallizing agent, and gradient freezing centrifugation is enriched with unsaturated fatty acid, utilizes lipase Enzymatic conjugated linoleic acid carries out transesterification, is prepared for functional grease, solves the recycling of organic solvent, conjugated linoleic acid is difficult to Edible problem improves the higher value application of rice bran.
The process conditions of gradient freezing centrifuge separation rice bran oil are selected, with the additive amount of 435 lipase of Novozym, reaction Temperature, reaction time and stirring rate are main inspection target, determine the optimum condition for preparing functional grease.
Summary of the invention
The present invention be directed to the acid values of rice bran oil, and high, organic solvent needs a large amount of a series of problems, such as recycling, and propose A kind of method that light phase rice bran oil and conjugated linoleic acid transesterification after freezing separation prepare functional grease.
It is realized by following steps: using carclazyte as crystallizing agent, rice bran oil, addition being centrifugated using gradient freezing 0.4% carclazyte after mixing with rice bran oil, freezes 6h under the conditions of -1 DEG C, 6h is freezed under the conditions of -2 DEG C, under the conditions of -3 DEG C Freeze 6h, 6h is freezed under the conditions of -4 DEG C, then refrigerated centrifuge under the conditions of -6 DEG C, the light phase rice bran oil after taking freezing separation with Conjugated linoleic acid carries out enzymic transesterification, prepares functional grease.
Specific embodiment
Specific embodiment 1: 3,6,9,12 and 15%Novozym, 435 lipase is prepared, 50,55,60,65 and 70 Under the conditions of DEG C temperature, with after separation light phase rice bran oil and CLA (molar ratio 3:1) carry out enzymic transesterification, low whipping speed 160,180,200,220, under 240rpm, 22,24,26,28 and 30h is maintained.By the functional grease handled well in 4 DEG C of refrigerators It stores, during storage, is formed using the fatty acid in high effective liquid chromatography for measuring grease.
Specific embodiment 2: the difference of present embodiment and specific embodiment one is with 6,9 and 12% 435 lipase enzymic transesterification of Novozym.Other steps are same as the specific embodiment one.
Specific embodiment 3: the difference of present embodiment and specific embodiment one is in 55,60 and 65 DEG C of enzymes Promote transesterification.Other steps are same as the specific embodiment one.
Specific embodiment 4: the difference of present embodiment and specific embodiment one is rice bran oil mixture in enzyme Promote to handle 24,26 and 28h in reaction.Other steps are same as the specific embodiment one.
Specific embodiment 5: difference of the present embodiment from specific embodiment one is that rice bran oil mixture is stirring Mix enzymatic reaction under 180,200 and 220rpm of speed.Other steps are same as the specific embodiment one.

Claims (5)

1. a kind of method that the light phase rice bran oil and conjugated linoleic acid transesterification after freezing separation prepare functional grease, feature It is that the thermal stability of the raising unsaturated fatty acid complex with degree of unsaturation can gradually decrease, adds crystallization temperature With the influence of the factors such as condition, so that it may realize that different structure component is able to separation, enrichment in fatty acid mixed.Select gradient cold Freeze the process conditions of centrifuge separation rice bran oil, the results showed that the functional oil of preparation is realized by following steps: using carclazyte as Crystallizing agent is centrifugated rice bran oil using gradient freezing, 0.4% carclazyte is added, after mixing with rice bran oil, under the conditions of -1 DEG C 6h is freezed, 6h is freezed under the conditions of -2 DEG C, freezes 6h under the conditions of -3 DEG C, 6h is freezed under the conditions of -4 DEG C, then in -6 DEG C of items Refrigerated centrifuge is enriched with unsaturated fatty acid under part, at a certain temperature, using the enzyme of Different adding amount, carries out enzyme with CLA Promote transesterification.The functional grease that will be handled well is stored in 4 DEG C of refrigerators.During storage, using high effective liquid chromatography for measuring The fatty acid of grease forms.
2. the light phase rice bran oil and conjugated linoleic acid transesterification after a kind of freezing separation according to claim 1 prepare function The method of property grease, it is characterised in that with 6,9 and 12% lipase enzymic transesterification.
3. the light phase rice bran oil and conjugated linoleic acid transesterification after a kind of freezing separation according to claim 1 prepare function The method of property grease, it is characterised in that 55,60 and 65 DEG C of enzymic transesterifications.
4. the light phase rice bran oil and conjugated linoleic acid transesterification after a kind of freezing separation according to claim 1 prepare function The method of property grease, feature handle 24,26 and 28h in rice bran oil mixture in enzymatic reaction.
5. the light phase rice bran oil and conjugated linoleic acid transesterification after a kind of freezing separation according to claim 1 prepare function The method of property grease, it is characterised in that enzymatic reaction under 180,200 and 220rpm of rice bran oil mixture low whipping speed.
CN201910869560.3A 2019-09-16 2019-09-16 A kind of method that light phase rice bran oil and conjugated linoleic acid transesterification after freezing separation prepare functional grease Pending CN110438175A (en)

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CN201910869560.3A CN110438175A (en) 2019-09-16 2019-09-16 A kind of method that light phase rice bran oil and conjugated linoleic acid transesterification after freezing separation prepare functional grease

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100999698A (en) * 2006-12-27 2007-07-18 华南理工大学 Greasy of containing glycerin ester type conjugate linolic acid and protuction process thereof
CN102268464A (en) * 2010-06-02 2011-12-07 河南工业大学 Method for producing diglyceride with rice bran oil of high acid value
CN102311882A (en) * 2011-08-11 2012-01-11 青岛农业大学 Extraction method for unsaturated fatty acid
CN103320220A (en) * 2013-07-19 2013-09-25 河南华泰粮油机械工程有限公司 Method for distilling and refining high-grade oil by rice bran oil molecules
US20150166928A1 (en) * 2013-12-18 2015-06-18 Commonwealth Scientific And Industrial Research Organisation Lipid comprising long chain polyunsaturated fatty acids

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100999698A (en) * 2006-12-27 2007-07-18 华南理工大学 Greasy of containing glycerin ester type conjugate linolic acid and protuction process thereof
CN102268464A (en) * 2010-06-02 2011-12-07 河南工业大学 Method for producing diglyceride with rice bran oil of high acid value
CN102311882A (en) * 2011-08-11 2012-01-11 青岛农业大学 Extraction method for unsaturated fatty acid
CN103320220A (en) * 2013-07-19 2013-09-25 河南华泰粮油机械工程有限公司 Method for distilling and refining high-grade oil by rice bran oil molecules
US20150166928A1 (en) * 2013-12-18 2015-06-18 Commonwealth Scientific And Industrial Research Organisation Lipid comprising long chain polyunsaturated fatty acids

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
MAHUA GHOSH等: "米糠油加工最新进展", 《中国油脂》 *
陈俊等: "梯度冷冻离心分离法提高山茶油中不饱和脂肪酸含量的研究", 《价值工程》 *

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