CN116672336A - Fat-reducing and weight-losing diglyceride composition and preparation method thereof - Google Patents
Fat-reducing and weight-losing diglyceride composition and preparation method thereof Download PDFInfo
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- CN116672336A CN116672336A CN202310972403.1A CN202310972403A CN116672336A CN 116672336 A CN116672336 A CN 116672336A CN 202310972403 A CN202310972403 A CN 202310972403A CN 116672336 A CN116672336 A CN 116672336A
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- 239000000203 mixture Substances 0.000 title claims abstract description 104
- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 79
- 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 claims abstract description 60
- 239000004005 microsphere Substances 0.000 claims abstract description 59
- 229930003427 Vitamin E Natural products 0.000 claims abstract description 30
- 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 claims abstract description 30
- 229940046009 vitamin E Drugs 0.000 claims abstract description 30
- 235000019165 vitamin E Nutrition 0.000 claims abstract description 30
- 239000011709 vitamin E Substances 0.000 claims abstract description 30
- 235000015112 vegetable and seed oil Nutrition 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000008158 vegetable oil Substances 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims description 65
- 238000006243 chemical reaction Methods 0.000 claims description 64
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 claims description 64
- 239000011248 coating agent Substances 0.000 claims description 47
- 238000000576 coating method Methods 0.000 claims description 47
- 239000007788 liquid Substances 0.000 claims description 47
- 238000002156 mixing Methods 0.000 claims description 37
- 238000003756 stirring Methods 0.000 claims description 35
- 235000021314 Palmitic acid Nutrition 0.000 claims description 32
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 claims description 32
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 30
- 235000011187 glycerol Nutrition 0.000 claims description 27
- 239000002904 solvent Substances 0.000 claims description 25
- 239000000839 emulsion Substances 0.000 claims description 23
- CIWBSHSKHKDKBQ-DUZGATOHSA-N D-isoascorbic acid Chemical compound OC[C@@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-DUZGATOHSA-N 0.000 claims description 22
- 239000012043 crude product Substances 0.000 claims description 21
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 20
- 239000012153 distilled water Substances 0.000 claims description 20
- 239000000047 product Substances 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- IPCSVZSSVZVIGE-UHFFFAOYSA-M hexadecanoate Chemical compound CCCCCCCCCCCCCCCC([O-])=O IPCSVZSSVZVIGE-UHFFFAOYSA-M 0.000 claims description 17
- 238000000605 extraction Methods 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 15
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- 108010039918 Polylysine Proteins 0.000 claims description 14
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- 239000004320 sodium erythorbate Substances 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 13
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- 101710093543 Probable non-specific lipid-transfer protein Proteins 0.000 claims description 11
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- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 5
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- 239000008280 blood Substances 0.000 abstract description 4
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- 201000001431 Hyperuricemia Diseases 0.000 abstract description 2
- 230000009471 action Effects 0.000 abstract description 2
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- 239000008194 pharmaceutical composition Substances 0.000 abstract description 2
- 235000019483 Peanut oil Nutrition 0.000 description 9
- 239000000312 peanut oil Substances 0.000 description 9
- 230000000694 effects Effects 0.000 description 6
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- 235000019484 Rapeseed oil Nutrition 0.000 description 4
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- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 description 3
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- 206010003210 Arteriosclerosis Diseases 0.000 description 1
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 1
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- 241001465754 Metazoa Species 0.000 description 1
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- ZSLZBFCDCINBPY-ZSJPKINUSA-N acetyl-CoA Chemical compound O[C@@H]1[C@H](OP(O)(O)=O)[C@@H](COP(O)(=O)OP(O)(=O)OCC(C)(C)[C@@H](O)C(=O)NCCC(=O)NCCSC(=O)C)O[C@H]1N1C2=NC=NC(N)=C2N=C1 ZSLZBFCDCINBPY-ZSJPKINUSA-N 0.000 description 1
- 208000011775 arteriosclerosis disease Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910001424 calcium ion Inorganic materials 0.000 description 1
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- 208000029078 coronary artery disease Diseases 0.000 description 1
- 230000002526 effect on cardiovascular system Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
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- 150000002576 ketones Chemical class 0.000 description 1
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- 231100000252 nontoxic Toxicity 0.000 description 1
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- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/33—Heterocyclic compounds
- A61K31/335—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin
- A61K31/35—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom
- A61K31/352—Heterocyclic compounds having oxygen as the only ring hetero atom, e.g. fungichromin having six-membered rings with one oxygen as the only ring hetero atom condensed with carbocyclic rings, e.g. methantheline
- A61K31/353—3,4-Dihydrobenzopyrans, e.g. chroman, catechin
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- A61K31/197—Carboxylic acids, e.g. valproic acid having an amino group the amino and the carboxyl groups being attached to the same acyclic carbon chain, e.g. gamma-aminobutyric acid [GABA], beta-alanine, epsilon-aminocaproic acid or pantothenic acid
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- 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
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- C12P7/6445—Glycerides
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Abstract
The invention relates to the field of pharmaceutical compositions, in particular to a fat-reducing and weight-losing diglyceride composition and a preparation method thereof, wherein the mass ratio of diglyceride to diglyceride slow-release microspheres to vitamin E in the components of the fat-reducing and weight-losing diglyceride composition is 78-90:10-15:0.1-0.5. The invention prepares diglyceride by using glycerol and vegetable oil under the action of an enzymolysis method, and the prepared diglyceride, the slow-release microsphere of the diglyceride and a small amount of vitamin E are compounded to obtain the fat-reducing and weight-losing diglyceride composition. The diglyceride composition prepared by the invention has important functions in reducing blood fat, reducing visceral fat, inhibiting weight gain and the like, and can be used as a product or an auxiliary drug for preventing and treating hyperuricemia or used in combination with a proper drug.
Description
Technical Field
The invention relates to the field of pharmaceutical compositions, in particular to a fat-reducing and weight-losing diglyceride composition and a preparation method thereof.
Background
The diglyceride is an ester formed by combining one glycerin molecule and two fatty acid molecules, and recent researches show that the diglyceride can reduce serum triglyceride of human and mice, can be used for preventing and treating hyperlipidemia and cardiovascular and cerebrovascular diseases closely related to the hyperlipidemia, such as arteriosclerosis, coronary heart disease, apoplexy, cerebral thrombosis and the like, has the effect of preventing obesity, and can prevent weight gain. At present, a plurality of safety evaluations show that the diglyceride is nontoxic and harmless to human bodies. Although diglycerides and triglycerides are substantially identical in energy and absorption, they have large differences in metabolism in the body, and short-term and long-term animal and human tests have shown that 1, 3-diglycerides have the effect of controlling and treating hypertriglyceridemia, obesity and complications thereof, as compared with triglycerides containing the same or similar fatty acid composition. Therefore, the edible oil rich in 1, 3-diglyceride can be used as health-care oil for healthy people instead of triglyceride edible oil, and can also be used for nutrition treatment of obese people and related complication people.
Diglycerides (DAGs) have the effect of inhibiting fat accumulation, mainly by increasing the rate of beta-oxidation in the liver. Beta-oxidation is a key metabolic process that reduces fat accumulation in the body. By conversion of beta-oxidized fatty acids to ketone bodies, followed by conversion to acetyl-coa, serves as a rapid energy source rather than resynthesis of new Triglyceride (TAG) molecules. It has been found that Diglycerides (DAG) enhance oxidation of fatty acids in the liver and reduce fatty acid synthesis. Moreover, the effect of Diglycerides (DAG) on increasing energy expenditure, fat oxidation and respiratory quotient is more pronounced in overweight people than in healthy people. However, the effect of the present diglyceride composition on weight loss cannot be expected.
Disclosure of Invention
Aiming at the problems existing in the prior art, the invention aims to provide a fat-reducing and weight-losing diglyceride composition and a preparation method thereof.
The aim of the invention is realized by adopting the following technical scheme:
the first object of the invention is to provide a preparation method of a fat-reducing and weight-losing diglyceride composition, which comprises the following steps:
firstly, mixing glycerol and vegetable oil in a reaction tank provided with heating equipment, adding an extraction solvent into the reaction tank, and continuously stirring until the mixture is uniform to form a first mixed reaction system;
secondly, adding lipase into the first mixed reaction system, starting heating equipment, heating to 45-65 ℃, uniformly mixing by ultrasound, and reacting for 5-10h under heat preservation and stirring to form a second mixed reaction system;
thirdly, continuously heating to 70-80 ℃, filtering the second mixed reaction system after enzyme deactivation, collecting supernatant, and then decompressing to remove solvent to obtain a crude diglyceride product;
fourthly, purifying the crude diglyceride product through molecular distillation and drying in vacuum to obtain diglyceride;
and fifthly, adding the diglyceride slow-release microspheres and the vitamin E into the diglyceride, and uniformly mixing to form the diglyceride composition.
Preferably, in the first step, the mass volume ratio of the glycerol, the vegetable oil and the extraction solvent is 1g (4-6): 0.8-1.2 mL; wherein the extraction solvent is No. 6 solvent oil.
Preferably, in the first step, the vegetable oil comprises any one of peanut oil, rapeseed oil, linseed oil, corn oil, soybean oil, olive oil, camellia seed oil and coconut oil.
Preferably, in the second step, the lipase is lipase TL100L and the input amount is 2% -6% of the sum of the mass of the glycerol and the mass of the vegetable oil.
Preferably, in the fourth step, the molecular distillation purification condition is that the evaporation surface temperature is 180-200 ℃, the feeding speed is 2-4mL/min, and the scraper rotating speed is 200-400r/min; the vacuum drying is performed in a vacuum box at 30-50deg.C.
Preferably, in the fourth step, the diglyceride slow-release microsphere is formed by preparing a palmitic acid diglyceride product, preparing a coating material into a coating liquid, homogenizing the palmitic acid diglyceride product, the mixed emulsion and the coating liquid to form a microsphere mixed liquid, and forming the microsphere by a spray drying mode.
Preferably, the preparation method of the diglyceride slow-release microsphere comprises the following steps:
(1) Preparing a palmitic acid diglyceride product, including preparing a crude product and purifying the crude product;
(2) Preparing coating liquid by taking resistant starch, polylysine and D-sodium erythorbate as coating materials;
(3) And mixing the coating liquid, the palmitic acid diglyceride product and the mixed emulsion, homogenizing and drying to form the diglyceride slow-release microsphere.
Preferably, the preparation process of the crude product of the palmitic acid diglyceride comprises the following steps:
s1, weighing palmitic acid and glycerol, mixing into a reaction bottle, placing the reaction bottle into a heating sleeve, heating to 80-100 ℃, and stirring until homogenization to obtain a mixture A; wherein the mass ratio of the palmitic acid to the glycerol is 1.12-1.14:1;
s2, heating the mixture A to 180-200 ℃, slowly adding sodium hydroxide powder, wherein the addition amount of the sodium hydroxide powder is 0.1-0.5% of the weight of the mixture A, and continuously stirring until homogenization is carried out to obtain a mixture B;
s3, introducing the reaction bottle containing the mixture B into a vacuum pump, pumping the reaction bottle to a vacuum degree of 20-50Pa, then continuing to perform heat preservation and stirring reaction for 1-3h, removing the heating sleeve and the vacuum pump, and naturally cooling to room temperature to obtain a mixture C;
s4, adding tartaric acid into the mixture C to adjust the pH of the reaction solution to 7.0-7.5, centrifuging in a centrifuge, and collecting an organic layer after centrifuging to obtain a crude product of the diglyceride palmitate;
preferably, the purification process of the crude product of palmitic acid diglyceride comprises:
and (3) additionally taking the flask and the heating sleeve, placing the liquid diglyceride crude product into the flask, heating to 175-185 ℃, vacuumizing, continuously introducing nitrogen into the liquid, continuously vacuumizing, removing the heating sleeve after the vacuum is continuously performed for 1.5-2h, stopping heating, and stopping vacuumizing and introducing nitrogen after the liquid is cooled to room temperature to obtain the diglyceride palmitate.
Preferably, the process for preparing the coating material into the coating liquid comprises the following steps:
mixing resistant starch, polylysine and D-sodium erythorbate into distilled water, heating to 55-60deg.C, and stirring to obtain uniform coating solution; wherein the mass ratio of the resistant starch, the polylysine, the D-sodium erythorbate and the distilled water is 1.2-2.6:1.5-2.8:0.3-0.8:15-20.
Preferably, the preparation process of the mixed emulsion comprises the following steps:
mixing milk basic protein and D-isoascorbic acid in distilled water, stirring at room temperature, pouring into a super-high speed shearing and dispersing machine, and high-speed shearing and dispersing for 3-5min to obtain mixed emulsion; wherein the mass ratio of the milk basic protein, the D-isoascorbic acid and the distilled water is 1:1:30-50.
Preferably, the preparation process of the microsphere mixed solution comprises the following steps:
mixing the diglyceride palmitate with the mixed emulsion, adding the mixture into the coating liquid, and dispersing the mixture in a homogenizing mixer to form uniform mixed liquid, namely the coating mixed liquid; the mass ratio of the palmitic acid diglyceride, the mixed emulsion and the coating liquid is 1:0.1-0.3:4-6.
Preferably, the drying process of the diglyceride slow-release microspheres comprises the following steps:
and (3) placing the coating mixed solution in a spray dryer, performing spray treatment, wherein the air inlet temperature of the spray dryer is 160-170 ℃, the feeding speed is 15-30mL/min, and collecting the obtained powder, namely the diglyceride slow-release microspheres.
The second object of the invention is to provide a fat-reducing and weight-losing diglyceride composition prepared by the preparation method.
Preferably, in the components of the fat-reducing and weight-losing diglyceride composition, the mass ratio of the diglyceride to the diglyceride slow-release microsphere to the vitamin E is 78-90:10-15:0.1-0.5.
The beneficial effects of the invention are as follows:
1. the invention prepares diglyceride by using glycerol and vegetable oil under the action of an enzymolysis method, and the prepared diglyceride, the slow-release microsphere of the diglyceride and a small amount of vitamin E are compounded to obtain the fat-reducing and weight-losing diglyceride composition.
2. The diglyceride composition prepared by the invention has important functions in reducing blood fat, reducing visceral fat, inhibiting weight gain and the like, and can be used as a product or an auxiliary drug for preventing and treating hyperuricemia or used in combination with a proper drug.
3. The diglyceride composition prepared by the invention also comprises diglyceride slow-release microspheres, and the microspheres are prepared by taking a mixture of resistant starch, polylysine and D-sodium erythorbate as a coating material and homemade diglyceride palmitate as a coating material. The microsphere product can gradually release the diglyceride of palmitic acid, thereby playing a role in continuous fat elimination, and meanwhile, the diglyceride of palmitic acid prepared by the invention can promote the absorption of calcium ions, and can enhance the immunity and regulate intestinal flora. The three products of resistant starch, polylysine and D-sodium erythorbate are low-calorie edible products, have the functions of reducing blood sugar and blood fat,
4. in the preparation process of the diglyceride slow-release microsphere, milk basic protein and D-isoascorbic acid are also used as an emulsifier, the emulsifier has good compatibility, the embedding rate of the diglyceride can reach more than 90% by matching with the coating material, and the embedding amount of the diglyceride is more than 30%, so that the effective content of the microsphere is high and the slow-release effect is better.
Detailed Description
The technical features, objects and advantages of the present invention will be more clearly understood from the following detailed description of the technical aspects of the present invention, but should not be construed as limiting the scope of the invention.
The invention is further described with reference to the following examples.
Example 1
A fat-reducing and weight-losing diglyceride composition comprises diglyceride, diglyceride slow-release microspheres and vitamin E; the mass ratio of the diglyceride to the diglyceride slow-release microsphere to the vitamin E is 78-90:10-15:0.1-0.5.
The preparation method of the fat-reducing and weight-losing diglyceride composition comprises the following steps:
firstly, mixing glycerol and peanut oil in a reaction tank provided with heating equipment, adding an extraction solvent into the reaction tank, and continuously stirring until the mixture is uniform to form a first mixed reaction system; the mass volume ratio of the glycerol to the peanut oil to the extraction solvent is 1g (4-6): 0.8-1.2 mL; wherein the extraction solvent is No. 6 solvent oil;
secondly, adding lipase TL100L with the total mass of glycerin and peanut oil into the first mixed reaction system, starting a heating device, heating to 45-65 ℃, uniformly mixing by ultrasonic, and carrying out heat preservation and stirring for 5-10h to form a second mixed reaction system;
thirdly, continuously heating to 70-80 ℃, filtering the second mixed reaction system after enzyme deactivation, collecting supernatant, and then decompressing to remove solvent to obtain a crude diglyceride product;
fourthly, purifying the crude diglyceride product through molecular distillation and drying in vacuum to obtain diglyceride; the molecular distillation purification condition is that the temperature of the evaporation surface is 180-200 ℃, the feeding speed is 2-4mL/min, and the scraper rotating speed is 200-400r/min; vacuum drying is drying in a vacuum box at 30-50deg.C;
and fifthly, adding the diglyceride slow-release microspheres and the vitamin E into the diglyceride, and uniformly mixing to form the diglyceride composition.
The preparation method of the diglyceride slow-release microsphere comprises the following steps:
(1) Preparation of crude product of palmitic acid diglyceride:
s1, weighing palmitic acid and glycerol, mixing into a reaction bottle, placing the reaction bottle into a heating sleeve, heating to 80-100 ℃, and stirring until homogenization to obtain a mixture A; wherein the mass ratio of the palmitic acid to the glycerol is 1.12-1.14:1;
s2, heating the mixture A to 180-200 ℃, slowly adding sodium hydroxide powder, wherein the addition amount of the sodium hydroxide powder is 0.1-0.5% of the weight of the mixture A, and continuously stirring until homogenization is carried out to obtain a mixture B;
s3, introducing the reaction bottle containing the mixture B into a vacuum pump, pumping the reaction bottle to a vacuum degree of 20-50Pa, then continuing to perform heat preservation and stirring reaction for 1-3h, removing the heating sleeve and the vacuum pump, and naturally cooling to room temperature to obtain a mixture C;
s4, adding tartaric acid into the mixture C to adjust the pH of the reaction solution to 7.0-7.5, centrifuging in a centrifuge, and collecting an organic layer after centrifuging to obtain a crude product of the diglyceride palmitate;
(2) Purification of crude palmitic acid diglyceride:
and (3) additionally taking the flask and the heating sleeve, placing the liquid diglyceride crude product into the flask, heating to 175-185 ℃, vacuumizing, continuously introducing nitrogen into the liquid, continuously vacuumizing, removing the heating sleeve after the vacuum is continuously performed for 1.5-2h, stopping heating, and stopping vacuumizing and introducing nitrogen after the liquid is cooled to room temperature to obtain the diglyceride palmitate.
(3) The coating material is prepared into coating liquid:
mixing resistant starch, polylysine and D-sodium erythorbate into distilled water, heating to 55-60deg.C, and stirring to obtain uniform coating solution; wherein the mass ratio of the resistant starch, the polylysine, the D-sodium erythorbate and the distilled water is 1.2-2.6:1.5-2.8:0.3-0.8:15-20.
(4) Preparation of the mixed emulsion:
mixing milk basic protein and D-isoascorbic acid in distilled water, stirring at room temperature, pouring into a super-high speed shearing and dispersing machine, and high-speed shearing and dispersing for 3-5min to obtain mixed emulsion; wherein the mass ratio of the milk basic protein, the D-isoascorbic acid and the distilled water is 1:1:30-50.
(5) Preparing microspheres:
mixing the diglyceride palmitate with the mixed emulsion, adding the mixture into the coating liquid, and dispersing the mixture in a homogenizing mixer to form uniform mixed liquid, namely the coating mixed liquid; the mass ratio of the palmitic acid diglyceride, the mixed emulsion and the coating liquid is 1:0.1-0.3:4-6;
and (3) placing the coating mixed solution in a spray dryer, performing spray treatment, wherein the air inlet temperature of the spray dryer is 160-170 ℃, the feeding speed is 15-30mL/min, and collecting the obtained powder, namely the diglyceride slow-release microspheres.
Example 2
A fat-reducing and weight-losing diglyceride composition comprises diglyceride, diglyceride slow-release microspheres and vitamin E; the mass ratio of the diglyceride to the diglyceride slow-release microsphere to the vitamin E is 78-90:10-15:0.1-0.5.
The preparation method of the fat-reducing and weight-losing diglyceride composition comprises the following steps:
firstly, mixing glycerol and rapeseed oil in a reaction tank provided with heating equipment, adding an extraction solvent into the reaction tank, and continuously stirring until the mixture is uniform to form a first mixed reaction system; the mass volume ratio of the glycerol to the rapeseed oil to the extraction solvent is 1g (4-6): 0.8-1.2 mL; wherein the extraction solvent is No. 6 solvent oil;
secondly, adding lipase TL100L with the total mass of glycerin and rapeseed oil into the first mixed reaction system, starting a heating device, heating to 45-65 ℃, uniformly mixing by ultrasonic, and performing heat preservation and stirring reaction for 5-10h to form a second mixed reaction system;
thirdly, continuously heating to 70-80 ℃, filtering the second mixed reaction system after enzyme deactivation, collecting supernatant, and then decompressing to remove solvent to obtain a crude diglyceride product;
fourthly, purifying the crude diglyceride product through molecular distillation and drying in vacuum to obtain diglyceride; the molecular distillation purification condition is that the temperature of the evaporation surface is 180-200 ℃, the feeding speed is 2-4mL/min, and the scraper rotating speed is 200-400r/min; vacuum drying is drying in a vacuum box at 30-50deg.C;
and fifthly, adding the diglyceride slow-release microspheres and the vitamin E into the diglyceride, and uniformly mixing to form the diglyceride composition.
Wherein, the preparation method of the diglyceride slow-release microsphere is the same as that of the example 1.
Example 3
A fat-reducing and weight-losing diglyceride composition comprises diglyceride, diglyceride slow-release microspheres and vitamin E; the mass ratio of the diglyceride to the diglyceride slow-release microsphere to the vitamin E is 78-90:10-15:0.1-0.5.
The preparation method of the fat-reducing and weight-losing diglyceride composition comprises the following steps:
firstly, mixing glycerol and linseed oil in a reaction tank provided with heating equipment, adding an extraction solvent into the reaction tank, and continuously stirring until the mixture is uniform to form a first mixed reaction system; the mass volume ratio of the glycerol to the linseed oil to the extraction solvent is 1g (4-6) of (0.8-1.2) mL; wherein the extraction solvent is No. 6 solvent oil;
secondly, adding lipase TL100L with the total mass of glycerol and linseed oil to the first mixed reaction system, starting heating equipment, heating to 45-65 ℃, uniformly mixing by ultrasound, and performing heat preservation and stirring for reaction for 5-10h to form a second mixed reaction system;
thirdly, continuously heating to 70-80 ℃, filtering the second mixed reaction system after enzyme deactivation, collecting supernatant, and then decompressing to remove solvent to obtain a crude diglyceride product;
fourthly, purifying the crude diglyceride product through molecular distillation and drying in vacuum to obtain diglyceride; the molecular distillation purification condition is that the temperature of the evaporation surface is 180-200 ℃, the feeding speed is 2-4mL/min, and the scraper rotating speed is 200-400r/min; vacuum drying is drying in a vacuum box at 30-50deg.C;
and fifthly, adding the diglyceride slow-release microspheres and the vitamin E into the diglyceride, and uniformly mixing to form the diglyceride composition.
Wherein, the preparation method of the diglyceride slow-release microsphere is the same as that of the example 1.
Example 4
A fat-reducing and weight-losing diglyceride composition comprises diglyceride, diglyceride slow-release microspheres and vitamin E; the mass ratio of the diglyceride to the diglyceride slow-release microsphere to the vitamin E is 78-90:10-15:0.1-0.5.
The preparation method of the fat-reducing and weight-losing diglyceride composition is the same as that of example 1, except that the preparation method of the diglyceride slow-release microspheres is slightly different. The preparation method of the diglyceride slow-release microsphere comprises the following steps:
(1) Preparation of crude product of palmitic acid diglyceride:
s1, weighing palmitic acid and glycerol, mixing into a reaction bottle, placing the reaction bottle into a heating sleeve, heating to 80-100 ℃, and stirring until homogenization to obtain a mixture A; wherein the mass ratio of the palmitic acid to the glycerol is 1.12-1.14:1;
s2, heating the mixture A to 180-200 ℃, slowly adding sodium hydroxide powder, wherein the addition amount of the sodium hydroxide powder is 0.1-0.5% of the weight of the mixture A, and continuously stirring until homogenization is carried out to obtain a mixture B;
s3, introducing the reaction bottle containing the mixture B into a vacuum pump, pumping the reaction bottle to a vacuum degree of 20-50Pa, then continuing to perform heat preservation and stirring reaction for 1-3h, removing the heating sleeve and the vacuum pump, and naturally cooling to room temperature to obtain a mixture C;
s4, adding tartaric acid into the mixture C to adjust the pH of the reaction solution to 7.0-7.5, centrifuging in a centrifuge, and collecting an organic layer after centrifuging to obtain a crude product of the diglyceride palmitate;
(2) Purification of crude palmitic acid diglyceride:
and (3) additionally taking the flask and the heating sleeve, placing the liquid diglyceride crude product into the flask, heating to 175-185 ℃, vacuumizing, continuously introducing nitrogen into the liquid, continuously vacuumizing, removing the heating sleeve after the vacuum is continuously performed for 1.5-2h, stopping heating, and stopping vacuumizing and introducing nitrogen after the liquid is cooled to room temperature to obtain the diglyceride palmitate.
(3) The coating material is prepared into coating liquid:
mixing resistant starch, polylysine and D-sodium erythorbate into distilled water, heating to 55-60deg.C, and stirring to obtain uniform coating solution; wherein the mass ratio of the resistant starch, the polylysine, the D-sodium erythorbate and the distilled water is 1.2-2.6:1.5-2.8:0.3-0.8:15-20.
(4) Preparation of the mixed emulsion:
mixing milk basic protein and D-isoascorbic acid in distilled water, stirring at room temperature, pouring into a super-high speed shearing and dispersing machine, and high-speed shearing and dispersing for 3-5min to obtain mixed emulsion; wherein the mass ratio of the milk basic protein, the D-isoascorbic acid and the distilled water is 1:1:30-50.
(5) Preparing microspheres:
mixing the diglyceride palmitate with the mixed emulsion, adding the mixture into the coating liquid, and dispersing the mixture in a homogenizing mixer to form uniform mixed liquid, namely the coating mixed liquid; the mass ratio of the palmitic acid diglyceride, the mixed emulsion and the coating liquid is 1:0.1-0.3:4-6;
and (3) placing the coating mixed solution in a spray dryer, performing spray treatment, wherein the air inlet temperature of the spray dryer is 160-170 ℃, the feeding speed is 15-30mL/min, and collecting the obtained powder, namely the diglyceride slow-release microspheres.
Example 5
A fat-reducing and weight-losing diglyceride composition comprises diglyceride, diglyceride slow-release microspheres and vitamin E; the mass ratio of the diglyceride to the diglyceride slow-release microsphere to the vitamin E is 78-90:10-15:0.1-0.5.
The preparation method of the fat-reducing and weight-losing diglyceride composition is the same as that of example 1, except that the preparation method of the diglyceride slow-release microspheres is slightly different. The preparation method of the diglyceride slow-release microsphere comprises the following steps:
(1) Preparation of crude product of palmitic acid diglyceride:
s1, weighing palmitic acid and glycerol, mixing into a reaction bottle, placing the reaction bottle into a heating sleeve, heating to 80-100 ℃, and stirring until homogenization to obtain a mixture A; wherein the mass ratio of the palmitic acid to the glycerol is 1.12-1.14:1;
s2, heating the mixture A to 180-200 ℃, slowly adding sodium hydroxide powder, wherein the addition amount of the sodium hydroxide powder is 0.1-0.5% of the weight of the mixture A, and continuously stirring until homogenization is carried out to obtain a mixture B;
s3, introducing the reaction bottle containing the mixture B into a vacuum pump, pumping the reaction bottle to a vacuum degree of 20-50Pa, then continuing to perform heat preservation and stirring reaction for 1-3h, removing the heating sleeve and the vacuum pump, and naturally cooling to room temperature to obtain a mixture C;
s4, adding tartaric acid into the mixture C to adjust the pH of the reaction solution to 7.0-7.5, centrifuging in a centrifuge, and collecting an organic layer after centrifuging to obtain a crude product of the diglyceride palmitate;
(2) Purification of crude palmitic acid diglyceride:
and (3) additionally taking the flask and the heating sleeve, placing the liquid diglyceride crude product into the flask, heating to 175-185 ℃, vacuumizing, continuously introducing nitrogen into the liquid, continuously vacuumizing, removing the heating sleeve after the vacuum is continuously performed for 1.5-2h, stopping heating, and stopping vacuumizing and introducing nitrogen after the liquid is cooled to room temperature to obtain the diglyceride palmitate.
(3) The coating material is prepared into coating liquid:
mixing resistant starch, polylysine and D-sodium erythorbate into distilled water, heating to 55-60deg.C, and stirring to obtain uniform coating solution; wherein the mass ratio of the resistant starch, the polylysine, the D-sodium erythorbate and the distilled water is 1.2-2.6:1.5-2.8:0.3-0.8:15-20.
(4) Preparation of the mixed emulsion:
mixing milk basic protein and D-isoascorbic acid in distilled water, stirring at room temperature, pouring into a super-high speed shearing and dispersing machine, and high-speed shearing and dispersing for 3-5min to obtain mixed emulsion; wherein the mass ratio of the milk basic protein, the D-isoascorbic acid and the distilled water is 1:1:30-50.
(5) Preparing microspheres:
mixing the diglyceride palmitate with the mixed emulsion, adding the mixture into the coating liquid, and dispersing the mixture in a homogenizing mixer to form uniform mixed liquid, namely the coating mixed liquid; the mass ratio of the palmitic acid diglyceride, the mixed emulsion and the coating liquid is 1:0.1-0.3:4-6;
and (3) placing the coating mixed solution in a spray dryer, performing spray treatment, wherein the air inlet temperature of the spray dryer is 160-170 ℃, the feeding speed is 15-30mL/min, and collecting the obtained powder, namely the diglyceride slow-release microspheres.
Example 6
A fat-reducing and weight-losing diglyceride composition comprises diglyceride, diglyceride slow-release microspheres and vitamin E; the mass ratio of the diglyceride to the diglyceride slow-release microsphere to the vitamin E is 78-90:10-15:0.1-0.5.
The preparation method of the fat-reducing diglyceride composition is the same as that of example 1, except that peanut oil is replaced with corn oil.
Example 7
A fat-reducing and weight-losing diglyceride composition comprises diglyceride, diglyceride slow-release microspheres and vitamin E; the mass ratio of the diglyceride to the diglyceride slow-release microsphere to the vitamin E is 78-90:10-15:0.1-0.5.
The preparation method of the fat-reducing diglyceride composition is the same as that of example 1, except that peanut oil is replaced with soybean oil.
Example 8
A fat-reducing and weight-losing diglyceride composition comprises diglyceride, diglyceride slow-release microspheres and vitamin E; the mass ratio of the diglyceride to the diglyceride slow-release microsphere to the vitamin E is 78-90:10-15:0.1-0.5.
The preparation method of the fat-reducing diglyceride composition is the same as that of example 1, except that peanut oil is replaced with olive oil.
Example 9
A fat-reducing and weight-losing diglyceride composition comprises diglyceride, diglyceride slow-release microspheres and vitamin E; the mass ratio of the diglyceride to the diglyceride slow-release microsphere to the vitamin E is 78-90:10-15:0.1-0.5.
The preparation method of the fat-reducing diglyceride composition is the same as that of example 1, except that peanut oil is replaced with camellia seed oil.
Example 10
A fat-reducing and weight-losing diglyceride composition comprises diglyceride, diglyceride slow-release microspheres and vitamin E; the mass ratio of the diglyceride to the diglyceride slow-release microsphere to the vitamin E is 78-90:10-15:0.1-0.5.
The preparation method of the fat-reducing diglyceride composition is the same as that of example 1, except that peanut oil is replaced with coconut oil.
Finally, it should be noted that the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the scope of the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made to the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention.
Claims (10)
1. The preparation method of the fat-reducing and weight-losing diglyceride composition is characterized by comprising the following steps of:
firstly, mixing glycerol and vegetable oil in a reaction tank provided with heating equipment, adding an extraction solvent into the reaction tank, and continuously stirring until the mixture is uniform to form a first mixed reaction system;
secondly, adding lipase into the first mixed reaction system, starting heating equipment, heating to 45-65 ℃, uniformly mixing by ultrasound, and reacting for 5-10h under heat preservation and stirring to form a second mixed reaction system;
thirdly, continuously heating to 70-80 ℃, filtering the second mixed reaction system after enzyme deactivation, collecting supernatant, and then decompressing to remove solvent to obtain a crude diglyceride product;
fourthly, purifying the crude diglyceride product through molecular distillation and drying in vacuum to obtain diglyceride;
and fifthly, adding the diglyceride slow-release microspheres and the vitamin E into the diglyceride, and uniformly mixing to form the diglyceride composition.
2. The method for preparing a fat-reducing diglyceride composition according to claim 1, wherein in the first step, the mass-to-volume ratio of glycerin, vegetable oil and extraction solvent is 1g (4-6): 0.8-1.2 mL; wherein the extraction solvent is No. 6 solvent oil.
3. The method for producing a fat-reducing diglyceride composition according to claim 1, wherein in the second step, the lipase is lipase TL100L in an amount of 2% -6% of the sum of the mass of glycerin and vegetable oil.
4. The method for preparing a fat-reducing diglyceride composition according to claim 1, wherein in the fourth step, the conditions for molecular distillation purification are that the evaporation surface temperature is 180-200 ℃, the feeding speed is 2-4mL/min, and the scraper rotation speed is 200-400r/min; the vacuum drying is performed in a vacuum box at 30-50deg.C.
5. The method for preparing the fat-reducing and weight-losing diglyceride composition according to claim 1, wherein the method for preparing the diglyceride slow-release microsphere comprises the following steps:
(1) Preparing a palmitic acid diglyceride product, including preparing a crude product and purifying the crude product;
(2) Preparing coating liquid by taking resistant starch, polylysine and D-sodium erythorbate as coating materials;
(3) And mixing the coating liquid, the palmitic acid diglyceride product and the mixed emulsion, homogenizing and drying to form the diglyceride slow-release microsphere.
6. The method for producing a fat-reducing diglyceride composition according to claim 5, wherein in step (1), the crude product of diglyceride palmitate is produced by the steps of:
s1, weighing palmitic acid and glycerol, mixing into a reaction bottle, placing the reaction bottle into a heating sleeve, heating to 80-100 ℃, and stirring until homogenization to obtain a mixture A; wherein the mass ratio of the palmitic acid to the glycerol is 1.12-1.14:1;
s2, heating the mixture A to 180-200 ℃, slowly adding sodium hydroxide powder, wherein the addition amount of the sodium hydroxide powder is 0.1-0.5% of the weight of the mixture A, and continuously stirring until homogenization is carried out to obtain a mixture B;
s3, introducing the reaction bottle containing the mixture B into a vacuum pump, pumping the reaction bottle to a vacuum degree of 20-50Pa, then continuing to perform heat preservation and stirring reaction for 1-3h, removing the heating sleeve and the vacuum pump, and naturally cooling to room temperature to obtain a mixture C;
s4, adding tartaric acid into the mixture C to adjust the pH of the reaction solution to 7.0-7.5, centrifuging in a centrifuge, and collecting an organic layer after centrifuging to obtain a crude product of the diglyceride palmitate;
the purification process of the crude product of the palmitic acid diglyceride comprises the following steps:
and (3) additionally taking the flask and the heating sleeve, placing the liquid diglyceride crude product into the flask, heating to 175-185 ℃, vacuumizing, continuously introducing nitrogen into the liquid, continuously vacuumizing, removing the heating sleeve after the vacuum is continuously performed for 1.5-2h, stopping heating, and stopping vacuumizing and introducing nitrogen after the liquid is cooled to room temperature to obtain the diglyceride palmitate.
7. The method for preparing the fat-reducing diglyceride composition according to claim 5, wherein in step (2), the process for preparing the coating material into the coating liquid comprises the following steps:
mixing resistant starch, polylysine and D-sodium erythorbate into distilled water, heating to 55-60deg.C, and stirring to obtain uniform coating solution; wherein the mass ratio of the resistant starch, the polylysine, the D-sodium erythorbate and the distilled water is 1.2-2.6:1.5-2.8:0.3-0.8:15-20.
8. The method for preparing a fat-reducing diglyceride composition according to claim 5, wherein in step (3), the process for preparing the mixed emulsion comprises:
mixing milk basic protein and D-isoascorbic acid in distilled water, stirring at room temperature, pouring into a super-high speed shearing and dispersing machine, and high-speed shearing and dispersing for 3-5min to obtain mixed emulsion; wherein the mass ratio of the milk basic protein, the D-isoascorbic acid and the distilled water is 1:1:30-50.
9. The method for preparing a fat-reducing diglyceride composition according to claim 5, wherein in step (3), the homogenizing process comprises:
mixing the diglyceride palmitate with the mixed emulsion, adding the mixture into the coating liquid, and dispersing the mixture in a homogenizing mixer to form uniform mixed liquid, namely the coating mixed liquid; the mass ratio of the palmitic acid diglyceride, the mixed emulsion and the coating liquid is 1:0.1-0.3:4-6;
the drying process includes:
and (3) placing the coating mixed solution in a spray dryer, performing spray treatment, wherein the air inlet temperature of the spray dryer is 160-170 ℃, the feeding speed is 15-30mL/min, and collecting the obtained powder, namely the diglyceride slow-release microspheres.
10. The fat-reducing and weight-losing diglyceride composition is characterized by being prepared by the preparation method of the fat-reducing and weight-losing diglyceride composition according to claim 1, wherein the mass ratio of diglyceride to diglyceride slow-release microspheres to vitamin E in the components of the fat-reducing and weight-losing diglyceride composition is 78-90:10-15:0.1-0.5.
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| 华娣;温琦;裘爱泳;蒋蕴珍;: "酶法甘油解连续制备甘油二酯的研究", 中国油脂, no. 05, pages 391 - 392 * |
| 温琦;姚专;蒋蕴珍;: "甘油二酯的工业化生产研究进展", 中国油脂, no. 09, pages 10 - 12 * |
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