CN110810848A - Preparation method of microcapsule with high vitamin E utilization rate - Google Patents
Preparation method of microcapsule with high vitamin E utilization rate Download PDFInfo
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- 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 title claims abstract description 112
- 229930003427 Vitamin E Natural products 0.000 title claims abstract description 56
- 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 title claims abstract description 56
- 235000019165 vitamin E Nutrition 0.000 title claims abstract description 56
- 229940046009 vitamin E Drugs 0.000 title claims abstract description 56
- 239000011709 vitamin E Substances 0.000 title claims abstract description 56
- 239000003094 microcapsule Substances 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title abstract description 4
- 239000000839 emulsion Substances 0.000 claims abstract description 40
- 229920002472 Starch Polymers 0.000 claims abstract description 25
- 239000008107 starch Substances 0.000 claims abstract description 25
- 235000019698 starch Nutrition 0.000 claims abstract description 25
- 238000010438 heat treatment Methods 0.000 claims abstract description 24
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000003921 oil Substances 0.000 claims abstract description 20
- 235000019198 oils Nutrition 0.000 claims abstract description 20
- 102000004169 proteins and genes Human genes 0.000 claims abstract description 19
- 108090000623 proteins and genes Proteins 0.000 claims abstract description 19
- 239000000243 solution Substances 0.000 claims abstract description 13
- 239000007921 spray Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000005469 granulation Methods 0.000 claims abstract description 10
- 230000003179 granulation Effects 0.000 claims abstract description 10
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 10
- 244000068988 Glycine max Species 0.000 claims abstract description 9
- 235000010469 Glycine max Nutrition 0.000 claims abstract description 9
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 239000012460 protein solution Substances 0.000 claims abstract description 7
- 238000007873 sieving Methods 0.000 claims abstract description 7
- 235000012424 soybean oil Nutrition 0.000 claims abstract description 7
- 239000003549 soybean oil Substances 0.000 claims abstract description 7
- 239000008055 phosphate buffer solution Substances 0.000 claims abstract description 6
- 238000005238 degreasing Methods 0.000 claims abstract 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 54
- 235000018102 proteins Nutrition 0.000 claims description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 12
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 239000006228 supernatant Substances 0.000 claims description 12
- 239000002244 precipitate Substances 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 6
- 238000004108 freeze drying Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 239000011780 sodium chloride Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000010419 fine particle Substances 0.000 claims description 4
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 3
- 235000004252 protein component Nutrition 0.000 claims description 3
- 239000000523 sample Substances 0.000 claims description 3
- 229910052719 titanium Inorganic materials 0.000 claims description 3
- 239000010936 titanium Substances 0.000 claims description 3
- 244000046052 Phaseolus vulgaris Species 0.000 claims 1
- 235000010627 Phaseolus vulgaris Nutrition 0.000 claims 1
- 238000005538 encapsulation Methods 0.000 abstract description 7
- 239000000463 material Substances 0.000 abstract description 6
- 238000000265 homogenisation Methods 0.000 abstract description 2
- 238000009210 therapy by ultrasound Methods 0.000 abstract description 2
- 238000003916 acid precipitation Methods 0.000 abstract 1
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- 239000004094 surface-active agent Substances 0.000 abstract 1
- 229940088594 vitamin Drugs 0.000 description 7
- 229930003231 vitamin Natural products 0.000 description 7
- 235000013343 vitamin Nutrition 0.000 description 7
- 239000011782 vitamin Substances 0.000 description 7
- 239000011162 core material Substances 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000002604 ultrasonography Methods 0.000 description 5
- 150000002333 glycines Chemical class 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000012545 processing Methods 0.000 description 4
- 210000000582 semen Anatomy 0.000 description 4
- 150000003722 vitamin derivatives Chemical class 0.000 description 3
- 235000013305 food Nutrition 0.000 description 2
- 239000008187 granular material Substances 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000000975 bioactive effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000029087 digestion Effects 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000006911 enzymatic reaction Methods 0.000 description 1
- 239000003925 fat Substances 0.000 description 1
- 235000012041 food component Nutrition 0.000 description 1
- 239000005417 food ingredient Substances 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000004530 micro-emulsion Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 239000007908 nanoemulsion Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000008363 phosphate buffer Substances 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002047 solid lipid nanoparticle Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- 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
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/15—Vitamins
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23J—PROTEIN COMPOSITIONS FOR FOODSTUFFS; WORKING-UP PROTEINS FOR FOODSTUFFS; PHOSPHATIDE COMPOSITIONS FOR FOODSTUFFS
- A23J1/00—Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites
- A23J1/14—Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites from leguminous or other vegetable seeds; from press-cake or oil-bearing seeds
- A23J1/142—Obtaining protein compositions for foodstuffs; Bulk opening of eggs and separation of yolks from whites from leguminous or other vegetable seeds; from press-cake or oil-bearing seeds by extracting with organic solvents
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23J—PROTEIN COMPOSITIONS FOR FOODSTUFFS; WORKING-UP PROTEINS FOR FOODSTUFFS; PHOSPHATIDE COMPOSITIONS FOR FOODSTUFFS
- A23J3/00—Working-up of proteins for foodstuffs
- A23J3/14—Vegetable proteins
- A23J3/16—Vegetable proteins from soybean
-
- 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
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Abstract
A preparation method of microcapsules with high vitamin E utilization rate belongs to the field of protein processing, and comprises the steps of selecting fresh soybeans, grinding and sieving, degreasing, then continuously separating by an alkali-soluble acid precipitation method to obtain lipophilic protein, dissolving the protein in phosphate buffer solution, then carrying out ultrasonic treatment to modify the protein, then dissolving the vitamin E in soybean oil as an oil phase, heating to fully dissolve the protein, then adding the protein solution into the solution, carrying out high-pressure homogenization treatment to form stable emulsion embedding the vitamin E, selecting starch and silicon dioxide as wall materials, and preparing the microcapsules by a spray granulation drying machine; the method furthest exerts the function of protein as a surfactant, finally improves the encapsulation efficiency of the vitamin E, and the obtained microcapsule can effectively improve the stability and bioavailability of the vitamin E, is green and healthy and consumes less energy.
Description
Technical Field
The invention belongs to the technical field of utilization rate of fat-soluble vitamins, and mainly relates to a method for improving utilization rate of vitamin E by using modified lipophilic protein.
Background
The structure and functional properties of proteins can be changed by physical, chemical and enzymatic methods, ultrasound is a non-heat treatment physical technique, is safe, consumes less time and consumes less energy, and due to its special cavitation, many studies have reported that the physical and functional properties of proteins, such as solubility, emulsibility, gelification, foamability, etc., can be directly modified by applying ultrasound, and at the same time, ultrasound has been proven to be effective in encapsulating particles with specific functional properties for use in food and related industries.
Currently, there is great interest in incorporating vitamin E as a functional ingredient into food systems, but because of the poorly soluble and highly oxidizable nature of highly lipophilic vitamin E, which readily deteriorates during digestion, processing and storage, encapsulation traps the bioactive material or composition into another element, protecting them from heat and oxidizing agents, a number of colloidal delivery systems have previously been used to encapsulate vitamins, including nanoemulsions, solid lipid nanoparticles, microemulsions. The emulsion system can be composed of a series of food ingredients through simple processing, and the selection and processing mode of the ingredients greatly influence the final encapsulation effect and the activity of vitamin E.
Soybean Lipophilic Protein (LP) has been shown to have a strong affinity for fats and oils, it will show a high surface activity, it can be used as an excellent emulsifier, and it has a good embedding effect on fat-soluble vitamins, but its high lipid content results in a low solubility, which affects other properties, which requires modification of lipophilic protein, while ultrasound is the safest, effective, energy-saving modification method, and the selection of ultrasound conditions is the key to modification.
In recent years, microcapsule technology is rapidly developed, which can change the surface property of a core material, protect the core material, improve the stability of the core material and achieve the purpose of controlling the release of the core material according to the release characteristics of different wall materials to the core material. Therefore, the invention utilizes the ultrasonic modified LP to develop a novel vitamin E emulsion delivery system, and uses natural high molecular materials as wall materials to prepare microcapsules, so as to protect the vitamin E from the influence of the external environment in the production and processing process and play a role in controlling the release of the vitamin E at specific time and position.
Disclosure of Invention
The invention aims to solve the problem of overcoming the defects of the prior art and provides a preparation method for preparing vitamin E microcapsules by using modified lipophilic protein so as to achieve the effects of improving the stability and bioavailability of vitamin E.
The technical problem to be solved by the invention is realized by the following technical scheme:
(1) grinding fresh soybean, sieving with 60 mesh sieve, defatting with n-hexane, centrifuging for 30min, collecting precipitate, and dry-heating at 70 deg.C for 2 hr until the nitrogen solubility index is reduced to 75%;
(2) adding 50g of the defatted soybean powder subjected to dry heat treatment into 400mL of distilled water, adjusting pH to 8.0 with NaOH, stirring at 20 deg.C for 1 hr, centrifuging at 3000g for 10min, separating the supernatant, and adding 10mM Na2SO3Then with H2SO4Adjusting pH to 5.8, centrifuging at 3000g for 10min (precipitate is 11S), and adding H2SO4Adjusting pH of the supernatant to 5.0, treating at 55 deg.C for 15min, adding 50mM NaCl, adjusting pH to 5.5 with NaOH, centrifuging at 3000g for 10min to obtain lipophilic protein component, dispersing the lipophilic protein, dialyzing for 24 hr, and freeze-drying;
(3) dissolving lipophilic protein in phosphate buffer solution (0.01mol/L pH 7.0), stirring at room temperature for 2h to obtain lipophilic protein solution (1% W/v), inserting titanium probe (diameter 0.636cm) of ultrasonic processor into liquid surface, treating under 0-480W ultrasonic power for 10-30min for 4s at interval of 2s to obtain modified lipophilic protein solution;
(4) dissolving 0.25% of vitamin E in soybean oil to form an oil phase (10% v/v), heating for 1min at 70 ℃ to fully dissolve the vitamin E, slowly adding the oil phase into an LP solution (1:9), dispersing at high speed for 2min at 12000r/min to form a crude emulsion, homogenizing the crude emulsion for three cycles (90s) at 20-50MPa by using a high-pressure homogenizer to finally obtain an emulsion with 10% of oil phase mass and 90% of LP mass, controlling the homogenizing temperature at 25 ℃ to obtain a vitamin E emulsion, and adjusting the pH of the prepared emulsion to 7.0 by using 0.1M HCl and NaOH for later use;
(5) mixing starch and silicon dioxide according to a ratio of 500:1-700:1(w/w), requiring better fluidity, opening a spray granulation dryer, adding starch, enabling the starch to rotate at high speed in the granulator to fill a granulation space, atomizing the vitamin E emulsion into small liquid drops by using a spray head, combining the small liquid drops with the starch in the granulator to prepare fine particles which fall into a fluidized bed, and heating the fluidized bed to 80 ℃ for drying for 1h to obtain the vitamin E microcapsule.
The ultrasonic power in the step (3) is 240W, and the ultrasonic time is 20 min.
And (4) the pressure of the high-pressure homogenizer in the step (4) is 35 MPa.
In the step (5), the ratio of starch to silicon dioxide is 650:1 (w/w).
The method provides a method for improving the utilization rate of vitamin E by using modified lipophilic protein, improves the functional property of the lipophilic protein by using specified ultrasonic treatment conditions, can improve the encapsulation efficiency of the vitamin E, prepares an emulsion delivery system for embedding the vitamin E by means of high-pressure homogenization, adopts natural high polymer materials as wall materials, prepares microcapsules by a spray drying method, protects the vitamin E from being degraded and oxidized by the influence of the external environment, and improves the bioavailability of the vitamin E. The method is green and healthy, has good stability and high application value, and is expected to become an effective way for delivering fat-soluble vitamins.
Drawings
FIG. 1 is a technical roadmap of the present invention;
FIG. 2 is a graph of bioavailable rate versus vitamin E stability data.
Detailed Description
The present invention is described in detail below with reference to examples:
grinding fresh soybean, sieving with 60 mesh sieve, defatting with n-hexane, centrifuging for 30min, collecting precipitate, and dry-heating at 70 deg.C for 2 hr until the nitrogen solubility index is reduced to 75%; adding 50g of the defatted soybean powder subjected to dry heat treatment into 400mL of distilled water, adjusting pH to 8.0 with NaOH, stirring at 20 deg.C for 1 hr, centrifuging at 3000g for 10min, separating the supernatant, and adding 10mM Na2SO3Then with H2SO4Adjusting pH to 5.8, centrifuging at 3000g for 10min (precipitate is 11S), and adding H2SO4Adjusting pH of the supernatant to 5.0, treating at 55 deg.C for 15min, adding 50mM NaCl, adjusting pH to 5.5 with NaOH, centrifuging at 3000g for 10min to obtain lipophilic protein component, dispersing the lipophilic protein, dialyzing for 24 hr, and freeze-drying; dissolving lipophilic protein in phosphate buffer solution (0.01mol/L pH 7.0), stirring at room temperature for 2h to obtain lipophilic protein solution (1% W/v), inserting titanium probe (diameter 0.636cm) of ultrasonic processor into liquid surface, treating under 0-480W ultrasonic power for 10-30min for 4s at interval of 2s to obtain modified lipophilic protein solution; dissolving 0.25% of vitamin E in soybean oil to form an oil phase (10% v/v), heating for 1min at 70 ℃ to fully dissolve the vitamin E, slowly adding the oil phase into an LP solution (1:9), dispersing at high speed for 2min at 12000r/min to form a crude emulsion, homogenizing the crude emulsion for three cycles (90s) at 20-50MPa by using a high-pressure homogenizer to finally obtain an emulsion with 10% of oil phase mass and 90% of LP mass, controlling the homogenizing temperature at 25 ℃ to obtain a vitamin E emulsion, and adjusting the pH of the prepared emulsion to 7.0 by using 0.1M HCl and NaOH for later use; mixing starch and silicon dioxide according to a ratio of 500:1-700:1(w/w), requiring better fluidity, opening a spray granulation dryer, adding starch, enabling the starch to rotate at high speed in the granulator to fill a granulation space, atomizing the vitamin E emulsion into small liquid drops by using a spray head, combining the small liquid drops with the starch in the granulator to prepare fine particles which fall into a fluidized bed, and heating the fluidized bed to 80 ℃ for drying for 1h to obtain the vitamin E microcapsule.
The ultrasonic power in the step (3) is 240W, and the ultrasonic time is 20 min.
And (4) the pressure of the high-pressure homogenizer in the step (4) is 35 MPa.
In the step (5), the ratio of starch to silicon dioxide is 650:1 (w/w).
Example 1: grinding fresh semen glycines into powder, sieving with 60 mesh sieve, defatting with 1:3 n-hexane, centrifuging for 30min, collecting precipitate, dry-heating at 70 deg.C for 2 hr to reduce nitrogen solubility index to 75%, adding 50g of defatted semen glycines powder after dry-heating into 400mL of distilled water, adjusting pH to 8.0 with NaOH, stirring at 20 deg.C for 1 hr, centrifuging for 10min at 3000g, separating supernatant, and adding 10mM Na2SO3Then with H2SO4Adjusting pH to 5.8, centrifuging at 3000g for 10min, and treating with H2SO4Adjusting the pH of the supernatant to 5.0, and treating at 55 deg.C for 15 min. Adding 50mM NaCl, adjusting the pH value to 5.5 by NaOH, centrifuging for 10min at 3000g, obtaining an LP component through precipitation, freeze-drying and storing, dissolving LP in a phosphate buffer solution (0.01mol/L pH 7.0), stirring for 2h to obtain an LP solution (1% W/v), treating for 10min at an ultrasonic power of 360W by using an ultrasonic processor (the diameter is 0.636cm), working for 4s and spacing for 2s to obtain a modified LP solution, dissolving vitamin E with the mass fraction of 0.25% in soybean oil to form an oil phase (10% v/v), heating for 1min at 70 ℃ to fully dissolve the vitamin E, slowly adding the oil phase into the LP solution (1:9), and dispersing for 2min at a high speed of 12000r/min to form a crude emulsion. Homogenizing the emulsion at 20MPa for three cycles (90s) by a high-pressure homogenizer to obtain emulsion with oil phase mass fraction of 10% and LP mass fraction of 90%, controlling the homogenizing temperature at 25 ℃ to obtain vitamin E emulsion, adjusting the pH of the prepared emulsion to 7.0 by 0.1M HCl and NaOH, mixing starch and silicon dioxide according to a ratio of 650:1(w/w), requiring good fluidity, turning on a spray granulation dryer to rotate the starch in a granulator at high speed, atomizing the vitamin E emulsion into small droplets by using an atomizing spray head, combining with starch in a granulator, making into fine granules, falling into a fluidized bed, heating to 80 deg.C, drying for 1h to obtain LP vitamin E-embedded microcapsule with average particle diameter of 368.7 + -20.53 nm, potential of-33.63 + -2.3 mV, PDI value of 0.41 + -0.01, encapsulation efficiency of 51.71 + -1.37%, bioavailability and vitamin E stability shown in figure 2.
Example 2: grinding fresh soybean, sieving with 60 mesh sieve, defatting with 1:3 n-hexane, centrifuging for 30min, collecting precipitate, dry-heating at 70 deg.C for 2 hr to reduce nitrogen solubility index to 75%, adding 50g of defatted soybean powder after dry-heating into 400mL of distilled water, adjusting pH to 8.0 with NaOH, stirring at 20 deg.C for 1 hr, and centrifuging for 10min at 3000 g. The supernatant was separated and 10mM Na added2SO3Then with H2SO4Adjusting pH to 5.8, centrifuging at 3000g for 10min, and treating with H2SO4Adjusting the pH value of the supernatant to 5.0, treating at 55 ℃ for 15min, adding 50mM NaCl, adjusting the pH value to 5.5 with NaOH, centrifuging for 10min at 3000g to obtain a precipitate LP component, freeze-drying and storing, dissolving LP in a phosphate buffer (0.01mol/L pH 7.0), stirring for 2h to obtain an LP solution (1% W/v), treating for 20min at 240W ultrasonic power by using an ultrasonic processor (diameter of 0.636cm), working for 4s at intervals of 2s to obtain a modified LP solution, dissolving vitamin E with the mass fraction of 0.25% in soybean oil to form an oil phase (10% v/v), heating at 70 ℃ for 1min to fully dissolve the vitamin E, slowly adding the oil phase into the LP solution (1:9), and dispersing at a high speed of 12000r/min for 2min to form a crude emulsion. Homogenizing the emulsion at 35MPa for three cycles (90s) by a high-pressure homogenizer to obtain emulsion with oil phase mass fraction of 10% and LP mass fraction of 90%, controlling the homogenizing temperature at 25 ℃ to obtain vitamin E emulsion, adjusting the pH of the prepared emulsion to 7.0 by 0.1M HCl and NaOH, mixing starch and silicon dioxide according to a ratio of 650:1(w/w), requiring good fluidity, turning on a spray granulation dryer to rotate the starch in a granulator at high speed, atomizing the vitamin E emulsion into small droplets by using an atomizing spray head, combining with starch in a granulator, making into fine granules, falling into a fluidized bed, heating to 80 deg.C, drying for 1h to obtain LP vitamin E-embedded microcapsule with average particle diameter of 365.4 + -12.78 nm, potential-39.82 + -1.5 mV, PDI value of 0.18 + -0.03, encapsulation efficiency of 64.43 + -0.86%, bioavailability and vitamin E stability shown in figure 2.
Example 3: grinding fresh semen glycines into powder, sieving with 60 mesh sieve, defatting with 1:3 n-hexane, centrifuging for 30min, collecting precipitate, dry-heating at 70 deg.C for 2 hr until nitrogen solubility index is reduced to 75%, and drying 50g of defatted semen glycines powder after dry-heatingAdding into 400mL distilled water, adjusting pH to 8.0 with NaOH, stirring at 20 deg.C for 1 hr, centrifuging at 3000g for 10min, separating supernatant, and adding 10mM Na2SO3Then with H2SO4Adjusting pH to 5.8, centrifuging at 3000g for 10min, and treating with H2SO4Adjusting the pH value of the supernatant to 5.0, treating at 55 ℃ for 15min, adding 50mM NaCl, adjusting the pH value to 5.5 with NaOH, centrifuging for 10min at 3000g to obtain a precipitate LP component, freeze-drying and storing, dissolving LP in a phosphate buffer solution (0.01mol/L pH 7.0), stirring for 2h to obtain an LP solution (1% W/v), treating with an ultrasonic processor (diameter 0.636cm) at an ultrasonic power of 360W for 20min, working for 4s, and spacing for 2s to obtain a modified LP solution, dissolving vitamin E in a mass fraction of 0.25% in soybean oil to form an oil phase (10% v/v), heating at 70 ℃ for 1min to fully dissolve the vitamin E, slowly adding the oil phase into the LP solution (1:9), dispersing at a high speed of 12000r/min for 2min to form a coarse emulsion, homogenizing the coarse emulsion with a high-pressure homogenizer for three cycles (90s) of 50MPa, obtaining an emulsion with an oil phase mass fraction of 10% and an LP mass fraction of 90%, homogenizing at 25 ℃ to obtain a vitamin E emulsion, adjusting the pH of the prepared emulsion to 7.0 by using 0.1M HCl and NaOH for standby, mixing starch and silicon dioxide according to a ratio of 650:1(w/w), requiring better fluidity, opening a spray granulation dryer, enabling the starch to rotate at a high speed in the granulator, atomizing the vitamin E emulsion into small droplets by using a spray head, combining the small droplets with the starch in the granulator to prepare fine particles, falling into a fluidized bed, heating to 80 ℃ and drying for 1h to obtain the LP vitamin E-embedded microcapsules, wherein the average particle size is 315.63 +/-12.15 nm, the potential is-35.17 +/-1.8 mV, the PDI value is 0.28 +/-0.02, the encapsulation efficiency is 60.52 +/-1.54%, and the bioavailability and the vitamin E stability are shown in figure 2.
Claims (4)
1. A method for preparing microcapsules with high vitamin E utilization rate is characterized by comprising the following steps:
(1) grinding fresh soybean, sieving with 60 mesh sieve, defatting with n-hexane, centrifuging for 30min, collecting precipitate, and dry-heating at 70 deg.C for 2 hr until the nitrogen solubility index is reduced to 75%;
(2)50g of degreasing after dry heat treatmentAdding bean powder into 400mL distilled water, adjusting pH to 8.0 with NaOH, stirring at 20 deg.C for 1 hr, centrifuging at 3000g for 10min, separating supernatant, and adding 10mM Na2SO3Then with H2SO4Adjusting pH to 5.8, centrifuging at 3000g for 10min (precipitate is 11S), and adding H2SO4Adjusting pH of the supernatant to 5.0, treating at 55 deg.C for 15min, adding 50mM NaCl, adjusting pH to 5.5 with NaOH, centrifuging at 3000g for 10min to obtain lipophilic protein component, dispersing the lipophilic protein, dialyzing for 24 hr, and freeze-drying;
(3) dissolving lipophilic protein in phosphate buffer solution (0.01mol/L pH 7.0), stirring at room temperature for 2h to obtain lipophilic protein solution (1% W/v), inserting titanium probe (diameter 0.636cm) of ultrasonic processor into liquid surface, treating under 0-480W ultrasonic power for 10-30min for 4s at interval of 2s to obtain modified lipophilic protein solution;
(4) dissolving 0.25% of vitamin E in soybean oil to form an oil phase (10% v/v), heating for 1min at 70 ℃ to fully dissolve the vitamin E, slowly adding the oil phase into an LP solution (1:9), dispersing at high speed for 2min at 12000r/min to form a crude emulsion, homogenizing the crude emulsion for three cycles (90s) at 20-50MPa by using a high-pressure homogenizer to finally obtain an emulsion with 10% of oil phase mass and 90% of LP mass, controlling the homogenizing temperature at 25 ℃ to obtain a vitamin E emulsion, and adjusting the pH of the prepared emulsion to 7.0 by using 0.1M HCl and NaOH for later use;
(5) mixing starch and silicon dioxide according to a ratio of 500:1-700:1(w/w), requiring better fluidity, opening a spray granulation dryer, adding starch, enabling the starch to rotate at high speed in the granulator to fill a granulation space, atomizing the vitamin E emulsion into small liquid drops by using a spray head, combining the small liquid drops with the starch in the granulator to prepare fine particles which fall into a fluidized bed, and heating the fluidized bed to 80 ℃ for drying for 1h to obtain the vitamin E microcapsule.
2. The method for preparing microcapsules with high vitamin E utilization rate according to claim 1, wherein the ultrasonic power in step (3) is 240W, and the ultrasonic time is 20 min.
3. The method for preparing microcapsules with high vitamin E utilization rate according to claim 1, wherein the pressure of the high-pressure homogenizer in the step (4) is 35 MPa.
4. The method for preparing microcapsules with high vitamin E utilization according to claim 1, wherein the ratio of starch to silica in step (5) is 650:1 (w/w).
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