CN111235190B - Horse oil rich in diglyceride and preparation method thereof - Google Patents
Horse oil rich in diglyceride and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 97
- 238000003756 stirring Methods 0.000 claims abstract description 66
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000006228 supernatant Substances 0.000 claims abstract description 45
- 102000004882 Lipase Human genes 0.000 claims abstract description 40
- 108090001060 Lipase Proteins 0.000 claims abstract description 40
- 239000004367 Lipase Substances 0.000 claims abstract description 40
- 235000019421 lipase Nutrition 0.000 claims abstract description 40
- 241000222120 Candida <Saccharomycetales> Species 0.000 claims abstract description 38
- 238000006243 chemical reaction Methods 0.000 claims abstract description 31
- 239000000376 reactant Substances 0.000 claims abstract description 31
- 102000004190 Enzymes Human genes 0.000 claims abstract description 20
- 108090000790 Enzymes Proteins 0.000 claims abstract description 20
- 239000000203 mixture Substances 0.000 claims abstract description 18
- 238000005520 cutting process Methods 0.000 claims abstract description 16
- 239000012153 distilled water Substances 0.000 claims abstract description 16
- 239000012535 impurity Substances 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 235000011187 glycerol Nutrition 0.000 claims description 36
- 238000005119 centrifugation Methods 0.000 claims description 21
- 239000012530 fluid Substances 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 15
- 238000000034 method Methods 0.000 abstract description 11
- 230000008901 benefit Effects 0.000 abstract description 8
- 239000002537 cosmetic Substances 0.000 abstract description 7
- 238000002844 melting Methods 0.000 abstract description 7
- 230000008018 melting Effects 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 7
- 238000005265 energy consumption Methods 0.000 abstract description 5
- 230000035699 permeability Effects 0.000 abstract description 4
- 235000021122 unsaturated fatty acids Nutrition 0.000 abstract description 4
- 150000004670 unsaturated fatty acids Chemical class 0.000 abstract description 4
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- 238000011161 development Methods 0.000 abstract description 3
- 238000012827 research and development Methods 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 239000003921 oil Substances 0.000 description 97
- 235000019198 oils Nutrition 0.000 description 97
- 235000019197 fats Nutrition 0.000 description 22
- 210000003491 skin Anatomy 0.000 description 7
- 230000003020 moisturizing effect Effects 0.000 description 6
- 238000005457 optimization Methods 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 239000006227 byproduct Substances 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000004519 grease Substances 0.000 description 4
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- GVJHHUAWPYXKBD-UHFFFAOYSA-N (±)-α-Tocopherol Chemical compound OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C GVJHHUAWPYXKBD-UHFFFAOYSA-N 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 230000032050 esterification Effects 0.000 description 2
- 238000005886 esterification reaction Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000011031 large-scale manufacturing process Methods 0.000 description 2
- 230000004060 metabolic process Effects 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- FPIPGXGPPPQFEQ-UHFFFAOYSA-N 13-cis retinol Natural products OCC=C(C)C=CC=C(C)C=CC1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-UHFFFAOYSA-N 0.000 description 1
- 241000272814 Anser sp. Species 0.000 description 1
- 208000010445 Chilblains Diseases 0.000 description 1
- 208000004929 Facial Paralysis Diseases 0.000 description 1
- 241000287828 Gallus gallus Species 0.000 description 1
- OYHQOLUKZRVURQ-HZJYTTRNSA-N Linoleic acid Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(O)=O OYHQOLUKZRVURQ-HZJYTTRNSA-N 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 239000004909 Moisturizer Substances 0.000 description 1
- 208000007101 Muscle Cramp Diseases 0.000 description 1
- 235000019483 Peanut oil Nutrition 0.000 description 1
- 235000019484 Rapeseed oil Nutrition 0.000 description 1
- 208000005392 Spasm Diseases 0.000 description 1
- 206010053615 Thermal burn Diseases 0.000 description 1
- 208000036826 VIIth nerve paralysis Diseases 0.000 description 1
- FPIPGXGPPPQFEQ-BOOMUCAASA-N Vitamin A Natural products OC/C=C(/C)\C=C\C=C(\C)/C=C/C1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-BOOMUCAASA-N 0.000 description 1
- 229930003427 Vitamin E Natural products 0.000 description 1
- 125000002252 acyl group Chemical group 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- FPIPGXGPPPQFEQ-OVSJKPMPSA-N all-trans-retinol Chemical compound OC\C=C(/C)\C=C\C=C(/C)\C=C\C1=C(C)CCCC1(C)C FPIPGXGPPPQFEQ-OVSJKPMPSA-N 0.000 description 1
- DTOSIQBPPRVQHS-PDBXOOCHSA-N alpha-linolenic acid Chemical compound CC\C=C/C\C=C/C\C=C/CCCCCCCC(O)=O DTOSIQBPPRVQHS-PDBXOOCHSA-N 0.000 description 1
- 235000020661 alpha-linolenic acid Nutrition 0.000 description 1
- 239000010775 animal oil Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 235000006708 antioxidants Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003833 cell viability Effects 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 235000005687 corn oil Nutrition 0.000 description 1
- 239000002285 corn oil Substances 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 239000008157 edible vegetable oil Substances 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 235000021323 fish oil Nutrition 0.000 description 1
- WIGCFUFOHFEKBI-UHFFFAOYSA-N gamma-tocopherol Natural products CC(C)CCCC(C)CCCC(C)CCCC1CCC2C(C)C(O)C(C)C(C)C2O1 WIGCFUFOHFEKBI-UHFFFAOYSA-N 0.000 description 1
- 230000003779 hair growth Effects 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 150000007529 inorganic bases Chemical class 0.000 description 1
- 230000002045 lasting effect Effects 0.000 description 1
- 235000020778 linoleic acid Nutrition 0.000 description 1
- OYHQOLUKZRVURQ-IXWMQOLASA-N linoleic acid Natural products CCCCC\C=C/C\C=C\CCCCCCCC(O)=O OYHQOLUKZRVURQ-IXWMQOLASA-N 0.000 description 1
- 229960004488 linolenic acid Drugs 0.000 description 1
- KQQKGWQCNNTQJW-UHFFFAOYSA-N linolenic acid Natural products CC=CCCC=CCC=CCCCCCCCC(O)=O KQQKGWQCNNTQJW-UHFFFAOYSA-N 0.000 description 1
- 150000004668 long chain fatty acids Chemical class 0.000 description 1
- 239000002398 materia medica Substances 0.000 description 1
- 238000010297 mechanical methods and process Methods 0.000 description 1
- 230000037353 metabolic pathway Effects 0.000 description 1
- 230000001333 moisturizer Effects 0.000 description 1
- -1 monoester Substances 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000312 peanut oil Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 235000020777 polyunsaturated fatty acids Nutrition 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000003549 soybean oil Substances 0.000 description 1
- 235000012424 soybean oil Nutrition 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 210000000434 stratum corneum Anatomy 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 150000003626 triacylglycerols Chemical class 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
- 235000019155 vitamin A Nutrition 0.000 description 1
- 239000011719 vitamin A Substances 0.000 description 1
- 235000019165 vitamin E Nutrition 0.000 description 1
- 229940046009 vitamin E Drugs 0.000 description 1
- 239000011709 vitamin E Substances 0.000 description 1
- 229940045997 vitamin a Drugs 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P7/00—Preparation of oxygen-containing organic compounds
- C12P7/64—Fats; 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
- C12P7/6436—Fatty acid esters
- C12P7/6445—Glycerides
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- Zoology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Biotechnology (AREA)
- Microbiology (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Bioinformatics & Cheminformatics (AREA)
- General Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The invention relates to the technical field of preparing diglyceride horse oil by an enzyme catalytic glycerolysis method, in particular to a diglyceride-rich horse oil and a preparation method thereof, wherein the diglyceride-rich horse oil is prepared by the following steps: removing impurities from fresh horse fat, cutting into pieces, mincing, adding distilled water, heating in water bath, stirring, standing, centrifuging supernatant, and collecting supernatant to obtain crude horse oil; uniformly mixing crude horse oil and glycerol, placing the mixture in a constant-temperature water bath, adding candida lipase, stirring, and performing enzymolysis reaction to obtain a reactant; the reaction was centrifuged to remove enzyme and glycerol to yield a diglyceride-rich horse oil. The preparation method provided by the invention has the advantages of mild reaction conditions, low energy consumption, high diglyceride yield, high unsaturated fatty acid content, low melting point, strong permeability and easiness in absorption by skin, provides a new raw material for research and development of high-grade cosmetics of the horse oil, can greatly improve the added value of the horse oil, and is a green innovative project with important development value.
Description
Technical Field
The invention relates to the technical field of preparation of diglyceride horse oil by an enzyme catalytic glycerolysis method, in particular to a diglyceride-rich horse oil and a preparation method thereof.
Background
Diglycerides (DAGs) are a naturally occurring edible trace oil component that is only 2% to 10% and is also an intermediate in oil metabolism, including the two isomers 1,3-DAG and 1,2-DAGP. DAG contains two nonpolar long chain fatty acids and one polar hydroxyl group, which reduces interfacial tension when it accumulates at the oil-water interface. Thus, DAG is mainly used as a moisturizer, emulsifier, stabilizer in the cosmetic industry. The general moisturizing agent has the advantages that the moisturizing agent is strong in hydrophilicity, can only stay on the surface layer of the skin, is difficult to permeate through the stratum corneum, has poor moisturizing effect and short acting time, and can overcome the defects of the moisturizing agent, and the moisturizing agent has good skin moisturizing performance and lasting effect. The horse oil has strong permeability to skin, is easy to absorb, can accelerate skin metabolism, resist aging and strengthen cell viability, and has recently developed in the industry of horse oil skin care products. The Xinjiang horse is rich in resources, is one of important animal husbandry bases in China, and horse fat is used as a horse byproduct, has the advantages of wide sources and easy obtainment, and is expected to develop high-grade horse oil cosmetics through intensive research.
Traditionally, the process for preparing diglycerides has been generally carried out with inorganic bases (NaOH, mgO, znO, la 2 O 3 Etc.) are catalysts. However, the method has the advantages of high energy consumption, low yield, multiple side reactions, high reaction temperature, easy damage to nutrient substances, easy environmental pollution caused by the treatment of the catalyst after the reaction, and great limitation of the application. The biological enzyme method for producing diglyceride has mild reaction condition, high selectivity and good color and smell, and accords with the production concept of green and environment protection. The method for preparing DAG by enzyme method mainly uses lipase as catalyst, and its reaction method mainly includesIncluding grease hydrolysis, direct esterification and grease glycerolysis. Although the grease hydrolysis method has wide application range, the reaction degree is difficult to control, the DAG yield is too low, and a large amount of byproducts such as monoester, glycerol and the like are generated due to excessive hydrolysis; the direct esterification method can be completed in one step, the purity of the product is high, but the reaction conditions are harsh, and the used raw materials such as grease and the like need complex pretreatment, so that the cost is too high, and the large-scale production is not easy to realize; the fat glycerolysis is a process in which triglycerides and glycerol are subjected to acyl transfer under lipase catalysis to produce DAG. The method has higher conversion rate and DAG yield, is the most studied method at present, and is suitable for large-scale production.
The application of horse fat in the history of China is long, and the application of horse fat in the Ming-Yi-Bie-Lu of the ancient ceramic and Hongdong prospect describes that the horse fat has the functions of hair growth and hair care. The plum fruit is recorded in the 'compendium of materia medica', ma Zhifang is sweet, flat and hair-growing, and can treat blackish face and rough hand and foot drying crack; has relieving effects on muscle spasm and facial paralysis; horse oil extracted from horse fat is commonly used in traditional Chinese medicine for treating chilblain and scald. Modern scientific researches show that the horse fat contains more than 60% of unsaturated fatty acid, more than 20% of polyunsaturated fatty acid, is rich in linolenic acid (13.65%) and linoleic acid (9.81%), contains fat-soluble vitamin A (7.2 mg/kg) and vitamin E (88.6 mg/kg), and is an excellent natural antioxidant. The raw materials for preparing diglycerides are mainly vegetable oil (peanut oil, rapeseed oil, corn oil, soybean oil and the like) and animal oil (fish oil, goose oil, chicken oil, lard and the like), and the purpose of the present invention is mainly to prepare edible oil based on the special metabolic pathway of the diglycerides in human bodies, and the document report of the application of the diglyceride horse oil prepared by taking horse oil as the raw material to cosmetics is not seen yet.
Disclosure of Invention
The invention provides the diglyceride-rich horse oil and the preparation method thereof, overcomes the defects of the prior art, can obtain the diglyceride-rich horse oil which has no peculiar smell, is fine and smooth and has lower melting point, and opens up a new way for comprehensively utilizing horse fat byproducts.
One of the technical schemes of the invention is realized by the following measures: the horse oil rich in diglyceride is prepared by the following steps: firstly, taking fresh horse fat, removing impurities, cutting into pieces, stirring, adding distilled water in a feed liquid ratio of 1:2, heating and stirring in a water bath at 45-55 ℃ for 3 h-3.5 h, standing, taking supernatant, centrifuging, and taking supernatant to obtain crude horse oil; step two, uniformly mixing crude horse oil and glycerin according to the weight ratio of 1:0.3-2, placing the mixture in a constant-temperature water bath, adding candida lipase, stirring at the stirring rate of 200 r/min-250 r/min, and carrying out enzymolysis reaction at the temperature of 30-65 ℃ for 4 h-10 h to obtain a reactant, wherein the weight ratio of the crude horse oil to the candida lipase is 100:1-5; and thirdly, centrifuging the reactant for 5 to 8 minutes to remove enzyme and glycerol, thus obtaining the diglyceride-rich horse oil.
The following are further optimizations and/or improvements to one of the above-described inventive solutions:
the mass ratio of the crude horse oil to the glycerol is 1:0.4 to 1.
The specific activity of the candida lipase is 20000U/g, and the weight ratio of the crude horse oil to the candida lipase is 100:2-4.
The enzymolysis reaction temperature is 35 ℃ to 40 ℃ and the time is 6h to 10 h.
In the first step, the stirring speed is 200 r/min, and the standing time is 2-5 min; or/and, the supernatant fluid centrifugal speed is 4000 r/min to 4500r/min, and the centrifugal time is 5 min to 8min; or/and, in the second step, the stirring speed is 220r/min to 250 r/min.
The second technical scheme of the invention is realized by the following measures: a preparation method of the horse oil rich in diglycerides comprises the following steps: firstly, taking fresh horse fat, removing impurities, cutting into pieces, stirring, adding distilled water in a feed liquid ratio of 1:2, heating and stirring in a water bath at 45-55 ℃ for 3 h-3.5 h, standing, taking supernatant, centrifuging, and taking supernatant to obtain crude horse oil; step two, uniformly mixing crude horse oil and glycerin according to the weight ratio of 1:0.3-2, placing the mixture in a constant-temperature water bath, adding candida lipase, stirring at the stirring rate of 200 r/min-250 r/min, and carrying out enzymolysis reaction at the temperature of 30-65 ℃ for 4 h-10 h to obtain a reactant, wherein the weight ratio of the crude horse oil to the candida lipase is 100:1-5; and thirdly, centrifuging the reactant for 5 to 8 minutes to remove enzyme and glycerol, thus obtaining the diglyceride-rich horse oil.
The following is a further optimization and/or improvement of the second technical scheme of the invention:
the mass ratio of the crude horse oil to the glycerol is 1:0.4 to 1.
The specific activity of the candida lipase is 20000U/g, and the weight ratio of the crude horse oil to the candida lipase is 100:2-4.
The enzymolysis reaction temperature is 35 ℃ to 40 ℃ and the time is 6h to 10 h.
In the first step, the stirring speed is 200 r/min, and the standing time is 2-5 min; or/and, the supernatant fluid centrifugal speed is 4000 r/min to 4500r/min, and the centrifugal time is 5 min to 8min; or/and, in the second step, the stirring speed is 220r/min to 250 r/min.
The preparation method provided by the invention has the advantages of mild reaction conditions, low energy consumption, high diglyceride yield, high unsaturated fatty acid content, low melting point, strong permeability and easiness in absorption by skin, provides a new raw material for research and development of high-grade cosmetics of the horse oil, can greatly improve the added value of the horse oil, and is a green innovative project with important development value.
Detailed Description
The present invention is not limited by the following examples, and specific embodiments can be determined according to the technical scheme and practical situations of the present invention. The various chemical reagents and chemical supplies mentioned in the invention are all commonly known and used in the prior art unless specified otherwise; the percentages in the invention are mass percentages unless specified otherwise; the solutions in the invention are aqueous solutions in which the solvent is water unless otherwise specified, for example, the hydrochloric acid solution is hydrochloric acid aqueous solution; the room temperature and the room temperature in the present invention generally refer to temperatures ranging from 15 ℃ to 25 ℃, and are generally defined as 25 ℃.
The invention is further described below with reference to examples:
example 1: the diglyceride-rich horse oil is prepared by the following steps: firstly, taking fresh horse fat, removing impurities, cutting into pieces, stirring, adding distilled water according to a feed liquid ratio of 1:2, heating in a water bath at 45-55 ℃ and stirring for 3h to 3.5 h, standing, taking supernatant, centrifuging, and taking supernatant to obtain crude horse oil; step two, uniformly mixing crude horse oil and glycerin according to the weight ratio of 1:0.3-2, placing the mixture in a constant-temperature water bath, adding candida lipase, stirring at the stirring rate of 200 r/min-250 r/min, and carrying out enzymolysis reaction for 4-10 hours at the temperature of 30-65 ℃ to obtain a reactant, wherein the weight ratio of the crude horse oil to the candida lipase is 100:1-5; and thirdly, centrifuging the reactant for 5 to 8 minutes to remove enzyme and glycerol, thus obtaining the diglyceride-rich horse oil.
The invention firstly utilizes a mechanical method to prepare crude horse oil, then mixes the crude horse oil with glycerin, utilizes candida lipase to carry out catalytic reaction, has mild reaction conditions and low energy consumption, ensures that the obtained diglyceride has high content (37 to 47 percent), can greatly improve the added value of the horse oil, is beneficial to creating economic benefit and social benefit and reducing environmental pollution, ensures that the obtained diglyceride horse oil has no peculiar smell, is finer (granularity is 20 to 33 mu m) and has lower melting point (point is 25 to 30 ℃), can be used as a new raw material of high-grade cosmetics, and opens up a new way for comprehensively utilizing the horse fat byproducts.
Example 2: the diglyceride-rich horse oil is prepared by the following steps: firstly, taking fresh horse fat, removing impurities, cutting into pieces, stirring, adding distilled water according to a feed liquid ratio of 1:2, heating and stirring in a water bath at 45 ℃ or 55 ℃ for 3 hours or 3.5 h, standing, taking supernatant, centrifuging, and taking supernatant to obtain crude horse oil; step two, uniformly mixing crude horse oil and glycerin according to the weight ratio of 1:0.3 or 2, placing the mixture in a constant-temperature water bath, adding candida lipase, stirring at the stirring rate of 200 r/min or 250 r/min, and carrying out enzymolysis reaction at 30 ℃ or 65 ℃ for 4h or 10h to obtain a reactant, wherein the weight ratio of the crude horse oil to the candida lipase is 100:1 or 5; thirdly, centrifuging the reactant for 5 min or 8min to remove enzyme and glycerol, thus obtaining the diglyceride-rich horse oil.
Example 3: as an optimization of the above examples, the mass ratio of crude horse oil to glycerin was 1:0.4 to 1.
Example 4: as an optimization of the above examples, the specific activity of candida lipase was 20000U/g, and the weight ratio of crude horse oil to candida lipase was 100:2 to 4.
Example 5: as optimization of the above examples, the enzymolysis reaction temperature is 35 ℃ to 40 ℃ and the time is 6h to 10 h.
Example 6: as an optimization of the above embodiment, in the first step, the stirring rate was 200 r/min and the standing time was 2 min to 5 min; or/and, the supernatant fluid centrifugal speed is 4000 r/min to 4500r/min, and the centrifugal time is 5 min to 8min; or/and, in the second step, the stirring speed is 220r/min to 250 r/min.
Example 7: the preparation method of the diglyceride-rich horse oil comprises the following steps: firstly, taking fresh horse fat, removing impurities, cutting into pieces, stirring, adding distilled water in a feed liquid ratio of 1:2, heating and stirring in a water bath at 45-55 ℃ for 3 h-3.5 h, standing, taking supernatant, centrifuging, and taking supernatant to obtain crude horse oil; step two, uniformly mixing crude horse oil and glycerin according to the weight ratio of 1:0.3-2, placing the mixture in a constant-temperature water bath, adding candida lipase, stirring at the stirring rate of 200 r/min-250 r/min, and carrying out enzymolysis reaction at the temperature of 30-65 ℃ for 4 h-10 h to obtain a reactant, wherein the weight ratio of the crude horse oil to the candida lipase is 100:1-5; and thirdly, centrifuging the reactant for 5 to 8 minutes to remove enzyme and glycerol, thus obtaining the diglyceride-rich horse oil.
Example 8: the diglyceride-rich horse oil is prepared by the following steps: firstly, taking fresh horse fat, removing impurities, cutting into pieces, stirring, adding distilled water in a feed liquid ratio of 1:2, heating in a water bath at 45 ℃ and stirring for 3h, standing, taking supernatant, centrifuging, and taking supernatant to obtain crude horse oil; step two, uniformly mixing crude horse oil and glycerin according to the weight ratio of 1:0.5, placing the mixture in a constant-temperature water bath, adding candida lipase, stirring at the stirring rate of 220r/min, and carrying out enzymolysis reaction at 40 ℃ for 6h to obtain a reactant, wherein the weight ratio of the crude horse oil to the candida lipase is 100:4, the centrifugation rate of supernatant fluid is 4500r/min, and the centrifugation time is 8min; and thirdly, centrifuging the reactant for 8min to remove enzyme and glycerol, thus obtaining the diglyceride-rich horse oil.
Example 9: the diglyceride-rich horse oil is prepared by the following steps: firstly, taking fresh horse fat, removing impurities, cutting into pieces, stirring, adding distilled water in a feed liquid ratio of 1:2, heating in a water bath at 40 ℃ and stirring for 3h, standing, taking supernatant, centrifuging, and taking supernatant to obtain crude horse oil; step two, uniformly mixing crude horse oil and glycerin according to the weight ratio of 1:0.5, placing the mixture in a constant-temperature water bath, adding candida lipase, stirring at the stirring rate of 220r/min, and carrying out enzymolysis reaction at 40 ℃ for 6h to obtain a reactant, wherein the weight ratio of the crude horse oil to the candida lipase is 100:3, the centrifugation rate of supernatant fluid is 4500r/min, and the centrifugation time is 8min; and thirdly, centrifuging the reactant for 8min to remove enzyme and glycerol, thus obtaining the diglyceride-rich horse oil.
Example 10: the diglyceride-rich horse oil is prepared by the following steps: firstly, taking fresh horse fat, removing impurities, cutting into pieces, stirring, adding distilled water in a feed liquid ratio of 1:2, heating in a water bath at 40 ℃ and stirring for 3h, standing, taking supernatant, centrifuging, and taking supernatant to obtain crude horse oil; step two, uniformly mixing crude horse oil and glycerin according to the weight ratio of 1:1, placing the mixture in a constant-temperature water bath, adding candida lipase, stirring at the stirring rate of 220r/min, and carrying out enzymolysis reaction at 40 ℃ for 6h to obtain a reactant, wherein the weight ratio of the crude horse oil to the candida lipase is 100:4, the centrifugation rate of supernatant fluid is 4500r/min, and the centrifugation time is 8min; and thirdly, centrifuging the reactant for 8min to remove enzyme and glycerol, thus obtaining the diglyceride-rich horse oil.
Example 11: the diglyceride-rich horse oil is prepared by the following steps: firstly, taking fresh horse fat, removing impurities, cutting into pieces, stirring, adding distilled water in a feed liquid ratio of 1:2, heating in a water bath at 40 ℃ and stirring for 3h, standing, taking supernatant, centrifuging, and taking supernatant to obtain crude horse oil; step two, uniformly mixing crude horse oil and glycerin according to the weight ratio of 1:1, placing the mixture in a constant-temperature water bath, adding candida lipase, stirring at the stirring rate of 250 r/min, and carrying out enzymolysis reaction at 40 ℃ for 6h to obtain a reactant, wherein the weight ratio of the crude horse oil to the candida lipase is 100:2, the centrifugation rate of supernatant fluid is 4500r/min, and the centrifugation time is 8min; and thirdly, centrifuging the reactant for 8min to remove enzyme and glycerol, thus obtaining the diglyceride-rich horse oil.
Example 12: the diglyceride horse oil is prepared by the following steps: firstly, taking fresh horse fat, removing impurities, cutting into pieces, stirring, adding distilled water in a feed liquid ratio of 1:2, heating in a water bath at 40 ℃ and stirring for 3h, standing, taking supernatant, centrifuging, and taking supernatant to obtain crude horse oil; step two, uniformly mixing crude horse oil and glycerin according to the weight ratio of 1:0.5, placing the mixture in a constant-temperature water bath, adding candida lipase, stirring at the stirring rate of 220r/min, and carrying out enzymolysis reaction at 40 ℃ for 6h to obtain a reactant, wherein the weight ratio of the crude horse oil to the candida lipase is 100:4, the centrifugation rate of supernatant fluid is 4500r/min, and the centrifugation time is 8min; and thirdly, centrifuging the reactant for 8min to remove enzyme and glycerol, thus obtaining the diglyceride-rich horse oil.
Example 13: the diglyceride-rich horse oil is prepared by the following steps: firstly, taking fresh horse fat, removing impurities, cutting into pieces, stirring, adding distilled water in a feed liquid ratio of 1:2, heating in a water bath at 45 ℃ and stirring for 3h, standing, taking supernatant, centrifuging, and taking supernatant to obtain crude horse oil; step two, uniformly mixing crude horse oil and glycerin according to the weight ratio of 1:0.4, placing the mixture in a constant-temperature water bath, adding candida lipase, stirring at the stirring rate of 220r/min, and carrying out enzymolysis reaction at 40 ℃ for 6h to obtain a reactant, wherein the weight ratio of the crude horse oil to the candida lipase is 100:4, the centrifugation rate of supernatant fluid is 4500r/min, and the centrifugation time is 8min; and thirdly, centrifuging the reactant for 8min to remove enzyme and glycerol, thus obtaining the diglyceride-rich horse oil.
Example 14: the diglyceride-rich horse oil is prepared by the following steps: firstly, taking fresh horse fat, removing impurities, cutting into pieces, stirring, adding distilled water in a feed liquid ratio of 1:2, heating in a water bath at 45 ℃ and stirring for 3h, standing, taking supernatant, centrifuging, and taking supernatant to obtain crude horse oil; step two, uniformly mixing crude horse oil and glycerin according to the weight ratio of 1:0.4, placing the mixture in a constant-temperature water bath, adding candida lipase, stirring at the stirring rate of 220r/min, and carrying out enzymolysis reaction at 40 ℃ for 8 h to obtain a reactant, wherein the weight ratio of the crude horse oil to the candida lipase is 100:2, the centrifugation rate of supernatant fluid is 4500r/min, and the centrifugation time is 8min; and thirdly, centrifuging the reactant for 8min to remove enzyme and glycerol, thus obtaining the diglyceride-rich horse oil.
Example 15: the diglyceride-rich horse oil is prepared by the following steps: firstly, taking fresh horse fat, removing impurities, cutting into pieces, stirring, adding distilled water in a feed liquid ratio of 1:2, heating in a water bath at 45 ℃ and stirring for 3h, standing, taking supernatant, centrifuging, and taking supernatant to obtain crude horse oil; step two, uniformly mixing crude horse oil and glycerin according to the weight ratio of 1:0.5, placing the mixture in a constant-temperature water bath, adding candida lipase, stirring at the stirring rate of 220r/min, and carrying out enzymolysis reaction at 40 ℃ for 6h to obtain a reactant, wherein the weight ratio of the crude horse oil to the candida lipase is 100:2, the centrifugation rate of supernatant fluid is 4500r/min, and the centrifugation time is 8min; and thirdly, centrifuging the reactant for 8min to remove enzyme and glycerol, thus obtaining the diglyceride-rich horse oil.
The content of diglyceride in the diglyceride horse oil obtained according to examples 8 to 15 of the present invention was 42.93%, 43.85%, 41.91%, 37.82%, 42.93%, 43.09%, 42.02%, 46.69%, respectively; melting points are 28 ℃, 27 ℃, 28 ℃, 30 ℃, 27 ℃, 26 ℃, 27 ℃ and 25 ℃ respectively in sequence; the particle sizes were 26 μm, 30 μm, 27 μm, 26 μm, 30 μm, 24 μm, 31 μm, 23 μm, respectively, in this order. Therefore, compared with crude horse oil, the diglyceride horse oil obtained by the invention has high content of diglyceride, no peculiar smell, finer fineness and lower melting point.
In conclusion, the preparation method provided by the invention has the advantages of mild reaction conditions, low energy consumption, high diglyceride yield, high unsaturated fatty acid content, low melting point, strong permeability and easiness in absorption by skin, provides a new raw material for research and development of high-grade cosmetics of the horse oil, can greatly improve the additional value of the horse oil, and is a green innovative project with important development value.
The technical characteristics form the embodiment of the invention, have stronger adaptability and implementation effect, and can increase or decrease unnecessary technical characteristics according to actual needs so as to meet the requirements of different situations.
Claims (2)
1. The diglyceride-rich horse oil is characterized by being prepared by the following steps: firstly, taking fresh horse fat, removing impurities, cutting into pieces, stirring, adding distilled water in a feed liquid ratio of 1:2, heating in a water bath at 45 ℃ and stirring for 3 hours, standing, taking supernatant, centrifuging, and taking supernatant to obtain crude horse oil; step two, uniformly mixing crude horse oil and glycerin according to the weight ratio of 1:0.5, placing the mixture in a constant-temperature water bath, adding candida lipase, stirring at the stirring rate of 220r/min, and carrying out enzymolysis reaction for 6 hours at the temperature of 40 ℃ to obtain a reactant, wherein the weight ratio of the crude horse oil to the candida lipase is 100:2, the centrifugation rate of supernatant fluid is 4500r/min, and the centrifugation time is 8min; and thirdly, centrifuging the reactant for 8min to remove enzyme and glycerol, thus obtaining the diglyceride-rich horse oil.
2. A preparation method of horse oil rich in diglyceride is characterized in that firstly, fresh horse oil is taken for removing impurities, cutting into pieces and mincing, distilled water is added according to the feed liquid ratio of 1:2, the mixture is heated and stirred in a water bath at 45 ℃ for 3 hours, then the mixture is stood, supernatant fluid is taken for centrifugation, and supernatant fluid is taken to obtain crude horse oil; step two, uniformly mixing crude horse oil and glycerin according to the weight ratio of 1:0.5, placing the mixture in a constant-temperature water bath, adding candida lipase, stirring at the stirring rate of 220r/min, and carrying out enzymolysis reaction for 6 hours at the temperature of 40 ℃ to obtain a reactant, wherein the weight ratio of the crude horse oil to the candida lipase is 100:2, the centrifugation rate of supernatant fluid is 4500r/min, and the centrifugation time is 8min; and thirdly, centrifuging the reactant for 8min to remove enzyme and glycerol, thus obtaining the diglyceride-rich horse oil.
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