CN112189846B - High-oil-loading pressure-resistant particle preparation and preparation method thereof - Google Patents
High-oil-loading pressure-resistant particle preparation and preparation method thereof Download PDFInfo
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- CN112189846B CN112189846B CN202011198275.2A CN202011198275A CN112189846B CN 112189846 B CN112189846 B CN 112189846B CN 202011198275 A CN202011198275 A CN 202011198275A CN 112189846 B CN112189846 B CN 112189846B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 37
- 239000002245 particle Substances 0.000 title claims abstract description 27
- 238000011068 loading method Methods 0.000 title claims abstract description 26
- 239000000463 material Substances 0.000 claims abstract description 33
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000002270 dispersing agent Substances 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 8
- 239000002775 capsule Substances 0.000 claims abstract description 3
- 239000003921 oil Substances 0.000 claims description 61
- 108010010803 Gelatin Proteins 0.000 claims description 38
- 239000008273 gelatin Substances 0.000 claims description 38
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- 235000011852 gelatine desserts Nutrition 0.000 claims description 38
- 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 description 32
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 22
- 239000000203 mixture Substances 0.000 claims description 20
- 229930003427 Vitamin E Natural products 0.000 claims description 16
- 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 description 16
- 229940046009 vitamin E Drugs 0.000 claims description 16
- 235000019165 vitamin E Nutrition 0.000 claims description 16
- 239000011709 vitamin E Substances 0.000 claims description 16
- 230000008014 freezing Effects 0.000 claims description 14
- 238000007710 freezing Methods 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 13
- ZAKOWWREFLAJOT-CEFNRUSXSA-N D-alpha-tocopherylacetate Chemical compound CC(=O)OC1=C(C)C(C)=C2O[C@@](CCC[C@H](C)CCC[C@H](C)CCCC(C)C)(C)CCC2=C1C ZAKOWWREFLAJOT-CEFNRUSXSA-N 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- ZAKOWWREFLAJOT-UHFFFAOYSA-N d-alpha-Tocopheryl acetate Natural products CC(=O)OC1=C(C)C(C)=C2OC(CCCC(C)CCCC(C)CCCC(C)C)(C)CCC2=C1C ZAKOWWREFLAJOT-UHFFFAOYSA-N 0.000 claims description 12
- 239000011859 microparticle Substances 0.000 claims description 12
- 229940042585 tocopherol acetate Drugs 0.000 claims description 12
- 239000000377 silicon dioxide Substances 0.000 claims description 11
- 239000001506 calcium phosphate Substances 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 9
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 0.000 claims description 9
- 229940078499 tricalcium phosphate Drugs 0.000 claims description 9
- 229910000391 tricalcium phosphate Inorganic materials 0.000 claims description 9
- 235000019731 tricalcium phosphate Nutrition 0.000 claims description 9
- 238000004132 cross linking Methods 0.000 claims description 8
- 238000009472 formulation Methods 0.000 claims description 8
- 108010010779 glutamine-pyruvate aminotransferase Proteins 0.000 claims description 8
- 239000000378 calcium silicate Substances 0.000 claims description 7
- 229910052918 calcium silicate Inorganic materials 0.000 claims description 7
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 claims description 7
- 230000003301 hydrolyzing effect Effects 0.000 claims description 7
- 230000007935 neutral effect Effects 0.000 claims description 7
- 235000012239 silicon dioxide Nutrition 0.000 claims description 6
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- VYGQUTWHTHXGQB-FFHKNEKCSA-N Retinol Palmitate Chemical compound CCCCCCCCCCCCCCCC(=O)OC\C=C(/C)\C=C\C=C(/C)\C=C\C1=C(C)CCCC1(C)C VYGQUTWHTHXGQB-FFHKNEKCSA-N 0.000 claims description 4
- JEBFVOLFMLUKLF-IFPLVEIFSA-N Astaxanthin Natural products CC(=C/C=C/C(=C/C=C/C1=C(C)C(=O)C(O)CC1(C)C)/C)C=CC=C(/C)C=CC=C(/C)C=CC2=C(C)C(=O)C(O)CC2(C)C JEBFVOLFMLUKLF-IFPLVEIFSA-N 0.000 claims description 3
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- 235000013793 astaxanthin Nutrition 0.000 claims description 3
- 229940022405 astaxanthin Drugs 0.000 claims description 3
- MQZIGYBFDRPAKN-ZWAPEEGVSA-N astaxanthin Chemical compound C([C@H](O)C(=O)C=1C)C(C)(C)C=1/C=C/C(/C)=C/C=C/C(/C)=C/C=C/C=C(C)C=CC=C(C)C=CC1=C(C)C(=O)[C@@H](O)CC1(C)C MQZIGYBFDRPAKN-ZWAPEEGVSA-N 0.000 claims description 3
- 239000001168 astaxanthin Substances 0.000 claims description 3
- 229960000342 retinol acetate Drugs 0.000 claims description 3
- 235000019173 retinyl acetate Nutrition 0.000 claims description 3
- 239000011770 retinyl acetate Substances 0.000 claims description 3
- QGNJRVVDBSJHIZ-QHLGVNSISA-N retinyl acetate Chemical compound CC(=O)OC\C=C(/C)\C=C\C=C(/C)\C=C\C1=C(C)CCCC1(C)C QGNJRVVDBSJHIZ-QHLGVNSISA-N 0.000 claims description 3
- 241000251468 Actinopterygii Species 0.000 claims description 2
- VYGQUTWHTHXGQB-UHFFFAOYSA-N Retinol hexadecanoate Natural products CCCCCCCCCCCCCCCC(=O)OCC=C(C)C=CC=C(C)C=CC1=C(C)CCCC1(C)C VYGQUTWHTHXGQB-UHFFFAOYSA-N 0.000 claims description 2
- 210000000988 bone and bone Anatomy 0.000 claims description 2
- 229940108325 retinyl palmitate Drugs 0.000 claims description 2
- 235000019172 retinyl palmitate Nutrition 0.000 claims description 2
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- 230000008569 process Effects 0.000 abstract description 7
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 8
- 235000021466 carotenoid Nutrition 0.000 description 7
- 150000001747 carotenoids Chemical class 0.000 description 7
- 229940088594 vitamin Drugs 0.000 description 7
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- 239000011782 vitamin Substances 0.000 description 7
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 150000003722 vitamin derivatives Chemical class 0.000 description 6
- 239000004615 ingredient Substances 0.000 description 5
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- JBYXPOFIGCOSSB-GOJKSUSPSA-N 9-cis,11-trans-octadecadienoic acid Chemical compound CCCCCC\C=C\C=C/CCCCCCCC(O)=O JBYXPOFIGCOSSB-GOJKSUSPSA-N 0.000 description 3
- 229940108924 conjugated linoleic acid Drugs 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 208000002173 dizziness Diseases 0.000 description 3
- OYHQOLUKZRVURQ-IXWMQOLASA-N linoleic acid Natural products CCCCC\C=C/C\C=C\CCCCCCCC(O)=O OYHQOLUKZRVURQ-IXWMQOLASA-N 0.000 description 3
- 239000003963 antioxidant agent Substances 0.000 description 2
- 230000003078 antioxidant effect Effects 0.000 description 2
- 235000006708 antioxidants Nutrition 0.000 description 2
- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
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- 239000011261 inert gas Substances 0.000 description 2
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
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- 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
- GUOCOOQWZHQBJI-UHFFFAOYSA-N 4-oct-7-enoxy-4-oxobutanoic acid Chemical compound OC(=O)CCC(=O)OCCCCCCC=C GUOCOOQWZHQBJI-UHFFFAOYSA-N 0.000 description 1
- 241000283690 Bos taurus Species 0.000 description 1
- FBPFZTCFMRRESA-KVTDHHQDSA-N D-Mannitol Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-KVTDHHQDSA-N 0.000 description 1
- 206010020772 Hypertension Diseases 0.000 description 1
- 108060003951 Immunoglobulin Proteins 0.000 description 1
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 description 1
- 229930195725 Mannitol Natural products 0.000 description 1
- 229920000168 Microcrystalline cellulose Polymers 0.000 description 1
- 229920002472 Starch Polymers 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
- 239000004480 active ingredient Substances 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
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
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- 230000017531 blood circulation Effects 0.000 description 1
- 238000010382 chemical cross-linking Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 235000012000 cholesterol Nutrition 0.000 description 1
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- 238000004925 denaturation Methods 0.000 description 1
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- 235000015872 dietary supplement Nutrition 0.000 description 1
- 238000007907 direct compression Methods 0.000 description 1
- 210000000981 epithelium Anatomy 0.000 description 1
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- 239000003925 fat Substances 0.000 description 1
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- 235000004280 healthy diet Nutrition 0.000 description 1
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- 230000006872 improvement Effects 0.000 description 1
- 239000008101 lactose Substances 0.000 description 1
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- 235000019359 magnesium stearate Nutrition 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 239000000594 mannitol Substances 0.000 description 1
- 235000010355 mannitol Nutrition 0.000 description 1
- 229940016286 microcrystalline cellulose Drugs 0.000 description 1
- 235000019813 microcrystalline cellulose Nutrition 0.000 description 1
- 239000008108 microcrystalline cellulose Substances 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000000546 pharmaceutical excipient Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
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- 230000001737 promoting effect Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
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- 238000003786 synthesis reaction Methods 0.000 description 1
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- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
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- 239000011719 vitamin A Substances 0.000 description 1
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Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23P—SHAPING OR WORKING OF FOODSTUFFS, NOT FULLY COVERED BY A SINGLE OTHER SUBCLASS
- A23P10/00—Shaping or working of foodstuffs characterised by the products
- A23P10/30—Encapsulation of particles, e.g. foodstuff additives
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Mycology (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Medicinal Preparation (AREA)
- Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
Abstract
The invention discloses a high oil-loading pressure-resistant particle preparation and a preparation method thereof, wherein the high oil-loading pressure-resistant particle preparation comprises an oil phase with the addition amount of 65-88% of the weight of the particle preparation, a specific embedding material and a dispersing agent. The inherent defects of the oil and fat-soluble functional component raw materials in the application are overcome by the microencapsulation technology through the selection of different embedding wall materials and the combined use and synergistic effect of the dispersing agent, and the problems of oil leakage, unstable exudation and the like of the fat-soluble functional components in the tabletting process are solved; the mechanical strength and stability of the high oil-loading particles are improved under high oil loading, and the particles are pressure-resistant and oil-tight, so that the particles have good application prospects in preparation of tablet or capsule products, particularly in preparation of foods, medicines, health-care products and functional foods.
Description
Technical Field
The invention belongs to the technical field of functional food preparations, and particularly relates to a high-oil-loading pressure-resistant particle preparation and a preparation method thereof.
Background
Many foods and functional foods contain functional fats and oils or fat-soluble functional ingredients, such as vitamins, carotenoids, unsaturated fatty acids, etc., and these functional ingredients play an important role in the healthy diet, dietary supplement, and nutrition fortification of people. For example, vitamin E and its esters have antioxidant, blood circulation improving, tissue protecting, cholesterol reducing, and hypertension preventing effects; vitamin A and its ester have effects of maintaining normal visual function, maintaining epithelial tissue cell health and promoting immunoglobulin synthesis; the carotenoid, especially astaxanthin, has remarkable effects in resisting oxidation and aging. However, the fat-soluble functional ingredients have many problems in the application process, such as oxidative denaturation, difficulty in storage, sensitivity to light, oxygen, heat, and the like.
The microcapsule technology utilizes a special embedding means to wrap fat-soluble functional components in a macromolecular colloid wall material to form a surface barrier, thereby greatly improving the stability and bioavailability of food raw materials and having a certain improvement effect on the taste and smell of the food raw materials. However, with the continuous knowledge of the microencapsulation technology and the demand for the intake of functional ingredients, more and more people are beginning to pay attention to the preparation method of microencapsulation of highly oil-loaded active ingredients. However, in the current technical level, when the oil loading reaches 60% or more of the total mass of the product, the embedding of the product has a plurality of problems, which can not completely solve the application requirements of oil and fat-soluble functional components, especially when the high-oil loading product is used in tablets: since the granules and tablet excipients are subjected to great pressure during the tabletting process, this places higher demands on the compression resistance of the embedded product. In recent years, many patents are dedicated to find a suitable embedding mode to optimize the process and the formula of a product with high oil loading.
For example, patent CN 109418541 a discloses a method for preparing a novel water-repellent fat-soluble vitamin microcapsule, in which under the protection of inert gas, sodium starch octenyl succinate and reducing sugar are used for embedding, and a chemical cross-linking agent is used to obtain a vitamin E product with a oil-carrying amount of 5-60%. The preparation process is complex, the use of inert gas is high, and the oil carrying capacity is low.
WO2017114120A1 discloses a vitamin and carotenoid powder and a preparation method thereof, wherein gel and antioxidant are used for forming a supermolecular solution, and the supermolecular solution is sprayed on the surfaces of suspended vitamin and carotenoid to form a gel protective film, so that the vitamin and carotenoid powder is obtained. The temperature for preparing the supermolecule solution is 70-100 ℃, the content of carotenoid or vitamin is degraded when the carotenoid or vitamin is sprayed and suspended in the air, the problem that the production is not easy to amplify is solved, and the carrying amount of fat-soluble functional components contained in the supermolecule solution is 10.9-36.5%. In the same way, the problem of low loading capacity also exists in the patent CN 106256346A, the loading capacity of the obtained vitamin E acetate is 1-20%, and meanwhile, magnesium stearate and silicon dioxide are added to serve as an anticaking agent, so that the flowability of the powder is improved.
In addition, patent 109718206 a, a method for producing vitamin E powder, provides a method for adsorbing vitamin E acetate with oil-loaded silica, the oil loading is 90-99%, but this method cannot utilize the adsorption performance of silica, only simple physical adsorption, does not have embedding effect, cannot improve the stability of vitamin E, and the obtained powder product cannot be applied to high-pressure tablet products because the silica is soft.
The patent CN109090613A discloses conjugated linoleic acid glyceride microcapsule powder and a preparation method thereof, wherein 3-35 parts of starch or colloid are used for preparing the conjugated linoleic acid microcapsule powder, the addition amount of an oil phase can reach 60-85 parts, the embedding rate can also reach more than 98%, and silicon dioxide, calcium silicate and the like are used as flow aids, so that the fluidity of the product is improved, and the adhesion of high-oil-loading powder is prevented. As is well known in the art, microencapsulated powders have an embedding property, but are not pressure-resistant, break when compressed, and leak oil.
In order to solve the application problem of the existing high-loading fat-soluble functional ingredients, a new granular preparation product with high oil loading, good stability and strong pressure resistance needs to be developed urgently.
Disclosure of Invention
The invention overcomes the inherent defects of the raw materials of the grease and the fat-soluble functional components in the application by the microencapsulation technology, and solves the problems of oil leakage, unstable exudation and the like of the fat-soluble functional components in the tabletting process; and the mechanical strength and stability of the high oil-loading particles are greatly improved by the combined use of the embedding wall material 1, the embedding wall material 2 and the dispersing agent.
First, the first aspect of the present invention is to protect a high oil-loading pressure-resistant microparticle preparation, which includes an oil phase, an embedding material 1, an embedding material 2, and a dispersant, wherein the addition amount of the oil phase is 65 to 88% of the weight of the microparticle preparation.
In the above technical solution, preferably, the oil phase is at least one selected from the group consisting of vitamin E, vitamin E acetate, vitamin a palmitate, vitamin a acetate and astaxanthin.
In the above-mentioned technical solution, preferably, the oil phase is added in an amount of 69 to 87% by weight of the final microparticle preparation. All percentages are based on the dry weight of the microparticle formulation.
In the above technical solution, preferably, the addition amount of the embedding wall material 1 is 1-2% of the weight of the granule preparation; the embedding material 1 is selected from calcium silicate and/or tricalcium phosphate. More preferably, the weight ratio of the calcium silicate to the tricalcium phosphate is (5-20): 0.5-2); most preferably, the weight ratio of the calcium silicate to the tricalcium phosphate is (8-12): 1.
In the above technical solution, preferably, the embedding material 2 is gelatin with a freezing force of 50 to 180Bloom g; the gelatin comprises pig gelatin, bovine bone gelatin and fish gelatin.
In the above technical solution, preferably, the gelatin preparation step comprises: dissolving gelatin in water, adding acid to adjust the pH value to 2.5-3.5, hydrolyzing, adjusting the pH value to be neutral, and adding glutamine transaminase for crosslinking. The embedding wall material 2 is gelatin which is used as a high molecular material with a three-dimensional structure and is a macromolecule material in a common microencapsulation product, but the common gelatin sold in the market can not meet the embedding requirement of high oil-loading particles. According to the invention, 0.1M hydrochloric acid is used for carrying out hydrolysis treatment on gelatin, and then glutamine transaminase is added for crosslinking to obtain the gelatin with the freezing force of 50-180 Bloom g, so that the gelatin has a good effect on the preparation of high oil-carrying particles, not only is an embedding effect achieved, but also a supporting effect is achieved by combining the gelatin with an embedding wall material 1, and the compression resistance degree of the combined particles is greatly improved.
In the above technical solution, preferably, the hydrolysis is performed by adding 0.05 to 0.3M hydrochloric acid to adjust the pH, and the hydrolysis time is at least 0.3 h.
In the above technical solution, preferably, the dispersant is silica. The silicon dioxide used as a dispersing agent can flow and disperse, and simultaneously, the silicon dioxide and the embedding wall material 1 and the embedding wall material 2 act synergistically to fill the cavity of the macromolecular material, so that the effect of three-layer embedding is achieved, and the technical effects of pressure resistance and oil leakage under high oil loading are achieved.
In the above technical solution, preferably, the amount of the dispersant added is 5 to 8% of the weight of the final granule formulation.
Another aspect of the present invention is to provide a method for preparing the oil-high pressure resistant microparticle preparation described above, comprising the steps of:
a) mixing the embedding wall material 1 with an oil phase, and stirring at 75-85 ℃ for 15-30 min to obtain an oil phase composition;
b) dissolving gelatin in water, adding acid to adjust the pH value to 2.5-3.5, hydrolyzing, adjusting the pH value to be neutral, and adding glutamine transaminase for crosslinking to obtain gelatin with the freezing force of 50-180 Bloom g;
c) adding the oil phase composition obtained in the step a) into the gelatin obtained in the step b), stirring, homogenizing and dispersing;
d) and adding a dispersing agent in the drying process to obtain the high oil-loading particles.
In the above-described embodiment, it is preferable that the embedding wall material 1 and the oil phase are mixed to form an oil phase composition, which is equivalent to the oil phase being embedded once and has an effect of adsorbing the oil phase and changing the inherent physical properties of the oil phase.
Another aspect of the present invention is to protect the application of the oil-high pressure resistant particle preparation described above in the preparation of tablet or capsule products, and the oil-high pressure resistant particle preparation of the present invention can be used as a raw material for further processing into functional foods such as tablets. Has the advantages of no blushing and high stability. In particular to the application in preparing food, medicine, health products and functional food.
Detailed Description
The following non-limiting examples further illustrate the invention but should not be construed as limiting the invention in any way, as the following methods are employed in the present application to measure and evaluate the product, unless otherwise specified.
The freezing force of the gelatin is determined by referring to appendix A.4 in national standard GB 6783-2013 food safety national standard food additive gelatin. And (4) calculating a result: the measured freezing strength values were read directly from the freezing force apparatus and expressed in Bloom g. The results are integers, and the arithmetic mean of the parallel measurements is taken as the measurement result. The absolute difference between two independent results obtained under repetitive conditions must not exceed 10Bloom g.
In the invention, surface oil is adopted to express microencapsulation efficiency, and the more the surface oil is, the lower the microencapsulation efficiency is, the more the non-embedded grease is, and the lower the stability is. The method for measuring the surface oil comprises the following steps: adding 5g of microcapsule product to be detected into an eggplant-shaped bottle, adding 20ml of petroleum ether (30-60 ℃), shaking for 20s, filtering, repeatedly washing twice, combining filtrates, removing the petroleum ether by rotary evaporation, drying at 105 ℃ to constant weight, and obtaining the mass ratio of the dry weight of the residual solid to the microcapsule product to be detected as the content of surface oil, wherein the content is expressed by percentage.
In the present invention, the oil leakage rate is used to indicate that the more grease oozes out after flaking, the worse the pressure resistance and the worse the stability. Weighing 6 tablets, adding 50ml of petroleum ether, soaking for 10 minutes, repeatedly soaking once, combining filtrates, removing the petroleum ether by rotary evaporation, drying at 105 ℃ to constant weight, and taking the mass ratio of the dry weight of the residual solid to the microcapsule product to be detected as the dizziness rate, which is expressed by percentage.
The product accelerated stability evaluation method provided by the invention is a method provided by Chinese pharmacopoeia: and (3) measuring the ratio of the product content to the initial content at different times at 40 ℃ and 75% RH for 3 months, namely determining the retention rate of the product so as to determine the quality of the product.
Example 1
Selection of embedding wall material 1:
mixing 1g of different materials with 70g of vitamin E, and stirring at a high temperature of 75-85 ℃ for 15-30 min to obtain an oil phase composition, wherein the influence of the different materials on the oil is shown in the following table 1:
TABLE 1 Effect of different materials on grease see below
Calcium silicate and tricalcium phosphate are used as embedding wall materials 1 to treat the oil phase, and the physical state of the oil phase composition is changed after treatment, so that later-period embedding is facilitated.
Example 2
Influence of the treatment of the embedding wall material 2 on the embedding effect:
(1) mixing 1g of tricalcium phosphate and 70g of vitamin E by stirring, and stirring at the high temperature of 75-85 ℃ for 15min to obtain an oil phase composition A; dissolving commercially available pig gelatin 16g and freezing power 100bloom g in water, stirring with the oil phase composition for dispersion, and drying to obtain vitamin E granule 1 with surface oil of 50%.
(2) 1g of tricalcium phosphate and 70g of vitamin E are stirred and mixed, and stirred for 15min at a high temperature of 75-85 ℃; adding 0.1M hydrochloric acid into 16g of commercially available porcine gelatin to adjust pH to 3, hydrolyzing for 0.5h, adjusting the dissolution after hydrolysis to be neutral, adding glutamine transaminase, crosslinking for 1h, measuring the gelatin freezing force to be 105bloom g, stirring and dispersing with the oil phase composition A, and drying to obtain vitamin E granules 2 with surface oil of 38.2%.
(3) Stirring and mixing 1g of tricalcium phosphate and 70g of vitamin E, and stirring at the high temperature of 75-85 ℃ for 15 min; adding commercially available porcine gelatin 16g, adding 0.1M citric acid to adjust pH to 3, hydrolyzing for 0.5 hr, adjusting dissolution after hydrolysis to neutral, adding glutamine transaminase, crosslinking for 1 hr, measuring gelatin freezing force to be 190bloom g, stirring with oil phase composition A, dispersing, and drying to obtain vitamin E granule 3 with surface oil of 44%.
And (4) conclusion: although the freezing force of the specially processed gelatin is not changed greatly, the embedding performance of the gelatin is obviously improved, hydrochloric acid is replaced by citric acid for hydrolysis under the same hydrolysis condition, the freezing force of the gelatin after hydrolysis and crosslinking is not as good as the optimal value, and the surface oil of the obtained particles is larger.
Example 3
The selection of the dispersant is that vitamin A acetate is prepared according to the preparation method of preparing vitamin E particles 2, and 13g of dispersant is added in the drying process, and the influence of different dispersants on the surface oil of the product is shown in the following table 2:
table 2. effect of different dispersants on product surface oil:
and (4) conclusion: the dispersing agent silicon dioxide has good filling effect, can fill the holes of the macromolecular embedding wall material 2, and achieves the purposes of reducing surface oil and improving stability.
Comparative example 1
(1) Using a method of producing vitamin E powder of patent 109718206 a, vitamin E acetate-silica particles were prepared with a vitamin E acetate content of 90% to give vitamin E acetate particles 1.
(2) The vitamin E acetate microcapsule powder 1 is prepared by using the patent CN109090613A conjugated linoleic acid glyceride microcapsule powder and the preparation method thereof, and the content of the vitamin E acetate is 70 percent.
(3) Using the method of the invention to prepare vitamin E acetate granules, 1.8g of calcium silicate, 0.2g of tricalcium phosphate and 85g of vitamin E acetate are stirred and mixed, and stirred for 15min at the high temperature of 85 ℃; commercially available porcine gelatin 8g was hydrolyzed with 0.1M hydrochloric acid to adjust pH to 3 for 0.5h, the dissolution after hydrolysis was adjusted to neutral, glutamine transaminase was added, crosslinking was performed for 1h, gelatin freezing force was measured to be 107bloom g, and after stirring and dispersion with oil phase composition a, 5g of silica was added during drying to obtain vitamin E acetate particles 2.
(4) The surface oil and stability of different granules or microcapsules and the percentage of tablets dizzy and tablet stability were measured and the results are shown in table 3. Tabletting by using a Tianfeng ZPW-8 type rotary tablet press, wherein the addition amount of the related products of the vitamin E acetate is 50 percent, and the other parts are common tablet auxiliary materials: 30% of microcrystalline cellulose, 10% of direct compression type lactose and 20% of mannitol. Therefore, the oil leakage rate of the tablets is 50 percent at most.
TABLE 3 surface oil and stability and percentage of tablets dizzy and stability data for different granules or microcapsules
And (4) conclusion: compared with the granules in the patent, the granules can also carry oil with high content of more than 70 percent, but all oil leaks in the tabletting process, the appearance of the tablets is influenced, and the stability is poor. The high oil-loading particles obtained by the method have no damage to the particles in the process of flaking application, have no phenomena of oil leakage and oil seepage, and have better stability than other two types.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and those skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention. Therefore, the protection scope of the present invention should be subject to the protection scope of the claims.
Claims (7)
1. A high oil-loading pressure-resistant microparticle preparation is characterized in that: the high oil-loading pressure-resistant particle preparation comprises an oil phase, an embedding material 1, an embedding material 2 and a dispersing agent, wherein the addition amount of the oil phase is 65-88% of the weight of the particle preparation; wherein:
the embedding material 1 is selected from calcium silicate and/or tricalcium phosphate;
the embedding material 2 is gelatin obtained by processing according to the following method: dissolving a gelatin raw material in water, adding 0.05-0.3M hydrochloric acid to adjust the pH value to 2.5-3.5, hydrolyzing, adjusting to be neutral, adding glutamine transaminase to perform crosslinking, and hydrolyzing for 0.3-1 h;
the dispersant is silicon dioxide.
2. The oil-high pressure resistant microparticle formulation as claimed in claim 1, wherein: the oil phase is at least one selected from vitamin E, vitamin E acetate, vitamin A palmitate, vitamin A acetate and astaxanthin.
3. The oil-high pressure resistant microparticle formulation as claimed in claim 1, wherein: the addition amount of the embedding material 1 is 1-2% of the weight of the particle preparation.
4. The oil-high pressure resistant microparticle formulation as claimed in claim 1, wherein: the freezing force of the gelatin is 50-180 Bloom g; the gelatin raw materials comprise pig gelatin, ox bone gelatin and fish gelatin.
5. The oil-high pressure resistant microparticle formulation as claimed in claim 1, wherein: the addition amount of the dispersing agent is 5-8% of the weight of the final particle preparation.
6. The method for preparing a high oil-loading pressure-resistant microparticle formulation as claimed in claim 1, comprising the steps of:
a) mixing the embedding material 1 and an oil phase, and stirring for 15-30 min at 75-85 ℃ to obtain an oil phase composition;
b) dissolving a gelatin raw material in water, adding acid to adjust the pH value to 2.5-3.5, hydrolyzing, adjusting the pH value to be neutral, adding glutamine transaminase to crosslink, and obtaining gelatin with the freezing force of 50-180 Bloom g;
c) adding the oil phase composition obtained in the step a) into the gelatin obtained in the step b), stirring, homogenizing and dispersing;
d) and adding a dispersing agent in the drying process to obtain the high oil-loading pressure-resistant particle preparation.
7. Use of the oil-high pressure resistant microparticle formulation of claim 1 for the preparation of a tablet or capsule product.
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