CN113273635A - Method for improving antioxidant property of microcapsule wall material and application thereof - Google Patents
Method for improving antioxidant property of microcapsule wall material and application thereof Download PDFInfo
- Publication number
- CN113273635A CN113273635A CN202110147676.3A CN202110147676A CN113273635A CN 113273635 A CN113273635 A CN 113273635A CN 202110147676 A CN202110147676 A CN 202110147676A CN 113273635 A CN113273635 A CN 113273635A
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- protein
- microcapsule
- ultrasonic
- improving
- wall material
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Classifications
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- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
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- A—HUMAN NECESSITIES
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- 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
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/5089—Processes
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
-
- 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
Abstract
The invention provides a method for improving the oxidation resistance of a microcapsule wall material by using modified protein and application thereof. The method comprises the following steps: dissolving the protein in water; ultrasonically modifying the solution; adding an emulsifier, and adding a liquid grease material and/or a fat-soluble material for emulsification treatment; adding one or more macromolecular materials to prepare the oil or fat-soluble microcapsule. The microcapsule wall material prepared by the method has a more compact structure and better oxidation resistance. The prepared microcapsule is used in products such as food, medicine or cosmetics, can effectively protect core material components from being invaded by external factors such as high temperature, illumination, oxygen and the like, and can cover unpleasant taste or smell carried by certain ingredient components or generated in the processing or storage process.
Description
Technical Field
The invention belongs to the field of chemical ingredients such as food, medicine and cosmetics, and relates to a method for improving the oxidation resistance of a microcapsule wall material and application thereof, in particular to a physical modification method for ultrasonic treatment of protein for the wall material for improving the oxidation resistance of the microcapsule and a method for preparing microcapsules by using the obtained modified wall material.
Background
The microcapsule technology is widely applied to food, pharmacy, cosmetics and light industrial manufactured products such as textile, printing and dyeing and the like. The microcapsule is composed of a core material and a wall material, and the microcapsule technology takes a plurality of sensitive substances with unstable properties as the core material to be embedded in the wall material, thereby protecting the sensitive substances from being damaged by external environmental factors such as oxygen, illumination, high temperature and the like. The microcapsule wall material is generally composed of macromolecular materials such as protein, polysaccharide and derivatives thereof, and the deterioration process of easily-deteriorated substances in the core material is inhibited and the loss of volatile substances is controlled by the physical barrier and chemical antioxidation of the wall material.
Among substances used as the core material of microcapsules, fats and oils including unsaturated fats and oils and derivatives thereof and fat-soluble components account for a large proportion, and these substances have various nutritional values and functional activities, and are therefore often used in the industrial fields of foods, medical supplies, cosmetics, and the like. Unsaturated fats and some fat-soluble ingredients exist in liquid form at normal temperature, and many fat-soluble ingredients also exist naturally or are added to liquid fats and fat-soluble substances for preservation or use. However, the above unsaturated fats and oils and fat-soluble components have many problems in industrial application: the higher the unsaturation degree of the grease, the poorer the stability of the grease is, the more easily the grease is oxidized, peculiar smell is generated and oxidation products which are harmful to the body health of a product user are generated, and some fat-soluble ingredients also face the problems of easy oxidation, easy volatilization and poor stability. The unsaturated oil and fat-soluble components are embedded by using a microcapsule technology, which is also called as microencapsulation, so that physical barrier can be formed between the unsaturated oil and fat-soluble components and the outside. The reasonable selection of the wall material, especially the wall material with oxidation resistance can further effectively improve the stability of the core material and prolong the shelf life of the product added with the microcapsule.
In recent years, the attention on the steady-state research of the oil and fat-soluble components with unstable chemical properties at home and abroad is high, wherein the unsaturated oil and the multiple unstable fat-soluble components are embedded by using a microencapsulation method, so that the stability of the oil and fat-soluble components can be greatly improved, the shelf life of the oil and fat-soluble components can be prolonged, and the adverse effects caused by oxygen, light and high temperature in the external environment in the storage process can be reduced as much as possible. Therefore, microencapsulation of the easily oxidized unsaturated oil or sensitive fat-soluble food ingredients is helpful for enhancing the stability of the unsaturated oil or sensitive fat-soluble food ingredients, prolonging the shelf life of the product, benefiting the sensory and nutritional quality of the product, and ensuring the stability of the product performance and quality.
At present, common methods for preparing microcapsules include spray drying, coating, extrusion, in-situ polymerization, complex coacervation, and the like. The complex coacervation method is one of the most common methods for embedding grease and fat-soluble components, and the method has the main advantages that special equipment is not needed, the preparation process does not involve higher temperature and extreme pH conditions, the overall process conditions are relatively mild, the damage to the core material quality in the preparation process is small, and the loading capacity of the obtained microcapsule product is relatively high.
Particularly, the protection of the unsaturated oil and fat-soluble component microcapsules on the core material content is mainly researched by optimizing the microencapsulation process and comparing and screening different wall materials, and the research on methods which are helpful for improving the stability of the core material of the product when the microcapsule is used as the wall material of the microcapsule, such as modification of the common wall material, is very limited, and no good effect is found yet. In order to prevent oxidation or deterioration of microencapsulated unsaturated fats and oils and sensitive fat-soluble components, a method of adding an antioxidant is currently generally used in the relevant industrial fields.
Antioxidants include both natural and synthetic substances. Many natural antioxidants are relatively expensive, and in addition, the natural antioxidants are not chemically stable enough, and are prone to deterioration and degradation over time. Although synthetic antioxidants are inexpensive and have good stability, the antioxidant method using synthetic antioxidants is becoming obsolete because consumers do not want to add more synthetic materials to products such as food, medicine, and cosmetics.
Patent application 201710190823.9 discloses a method for preparing an antioxidant microcapsule wall material, which involves adding rutin extracted from fresh sophora flower bud into the microcapsule wall material to prepare a microcapsule wall material raw material with antioxidant property. However, the rutin component selected in the method disclosed in the patent is not very stable, and the rutin is decomposed under the condition of exceeding 160 ℃, which means that the rutin component in the wall material is easy to decompose in the technological links of spray drying and the like, or the product added with the microcapsule is decomposed after high-temperature frying and other operations in the processing or using process, so that the antioxidant effect is lost.
Patent application 201710665415.4 discloses a method for preparing microcapsules from a microcapsule wall material modified by nano-silica, which is to add a nano-silica component into the microcapsule wall material to prepare a microcapsule wall material with improved stability of the microcapsule core material. However, the method is not suitable for microencapsulation of unsaturated oil and fat-soluble components in food and edible drugs. Patent application 201711432206.1 discloses a nano-zinc oxide modified microcapsule composite phase change material and a preparation method thereof, and the method is also limited by the addition of components of wall materials and the wall materials, so that the method cannot be applied to the fields of food, edible medicines and the like.
In summary, how to produce a microcapsule wall material with good oxidation resistance, which can be widely applied to the fields of food, medical supplies and cosmetics and does not depend on adding natural or artificially synthesized antioxidant ingredients, remains a technical problem to be solved by the technical staff in the field.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides the following technical scheme:
a method for improving the oxidation resistance of microcapsule wall materials by using modified proteins comprises the following steps:
(1) dissolving a protein used as a microcapsule wall material in water to obtain a solution A;
(2) carrying out ultrasonic modification on the solution A to obtain a solution B;
(3) adding an emulsifier into the solution B to obtain a solution C; adding a liquid grease material and/or a fat-soluble material into the solution C, and emulsifying to obtain a liquid D;
(4) adding one or more macromolecular materials into the liquid D to prepare grease or fat-soluble microcapsules; the macromolecular material is polysaccharide or cellulose.
Preferably, the protein used as the wall material of the microcapsule in step (1) includes, but is not limited to, a mixture of one or more of gelatin protein, whey protein, soy protein, chickpea protein, broad bean protein, pea protein and peanut protein; the protein used as the wall material of the microcapsule is further preferably gelatin protein because gelatin protein has good solubility, emulsifiability and gelation properties.
More preferably, the mass ratio of the protein to water is 1:15 to 1: 30; the dissolution temperature is 45-55 ℃.
Preferably, the ultrasonic modification in step (2) is performed by using an ultrasonic extractor or a water bath ultrasonic extractor.
More preferably, when the apparatus used for ultrasonic modification is an ultrasonic extractor, the specific steps are as follows: and (2) placing the solution A in a beaker, then placing the beaker in a constant-temperature water bath for a certain time to ensure that the temperature of the solution A is the same as that of the constant-temperature water bath, then transferring the beaker to a box body of an ultrasonic extraction instrument (or called an amplitude transformer ultrasonic cell disruption instrument), inserting an amplitude transformer below the solution, and setting ultrasonic power and time for modification operation to obtain a solution B.
Further preferably, the ultrasonic power of the ultrasonic extractor is set to 900-.
It is further preferable that the ultrasonic time of the ultrasonic extractor in step (2) is set to 15-25min, and the ultrasonic time of the horn is further preferably set to 20min, because the relatively short ultrasonic modification time cannot make the degree of modification of the protein to be required, and the relatively long ultrasonic modification time may cause an overheating effect to adversely affect the protein.
More preferably, when the ultrasonic modification apparatus is a water bath ultrasonic apparatus, the specific steps are as follows: and (2) placing the solution A in a closed container which can be covered or sealed, placing the closed container in a constant-temperature water bath set at a certain temperature for a certain time to ensure that the temperature of the solution A is the same as that of the constant-temperature water bath, simultaneously setting the temperature of the water bath in the ultrasonic water bath cleaning tank to be consistent, and setting the temperature, the ultrasonic power, the ultrasonic frequency and the ultrasonic time of the water bath to carry out modification operation, thereby obtaining a solution B.
Further preferably, the temperature of the water bath ultrasonic instrument is set to 60-75 ℃, a proper increase of the temperature is favorable for enhancing the hydration of the protein and for improving the ultrasonic modification effect, while an excessively high temperature may adversely affect the hydration and reduce the solubility of the protein, so that the temperature of the water bath is further preferably 65 ℃.
It is further preferable that the ultrasonic power of the water bath ultrasonic instrument is set to 490-630W, as an important parameter of the water bath ultrasonic, the influence of the ultrasonic power on the protein modification effect is very large, the lower power cannot effectively change the structure of the protein, and the excessively high power may cause the overheating denaturation to adversely affect the functional properties of the protein, so the ultrasonic power is further preferably 560W.
Further preferably, the ultrasonic frequency of the water bath ultrasonic instrument is set to be 45-100kHz, and according to the result of experimental study, when the protein is ultrasonically modified by the ultrasonic water bath cleaning tank, the ultrasonic frequency is set within the experimental range without significant influence on the modification effect, so that the ultrasonic frequency of the water bath is artificially selected to be 100 kHz.
Further preferably, the ultrasonic time of the water bath ultrasonic instrument is set to be 10-25min, similar to the ultrasonic modification of the amplitude transformer, the short ultrasonic time is not enough to induce the structural change capable of changing the physicochemical property of the protein, and the overlong ultrasonic time can generate an overheating effect to excessively denature the protein, so the water bath ultrasonic time is further preferably 20 min.
Generally, in the process of microencapsulating easily oxidized liquid lipid material and/or fat-soluble material, one skilled in the art usually delays the progress of core material oxidation by increasing the thickness of wall material layer of the microcapsule or adding natural/synthetic antioxidant.
Applicants have found that the progress of core oxidation can also be retarded when using proteins sonicated via horn or water bath as microcapsule wall materials. After a great deal of research work, the applicant found that the degree of denaturation of protein can be controlled to a desirable level by controlling the degree of horn ultrasound or bath ultrasound, so that the protection of the core material can be effectively enhanced when the microcapsule is used as a microcapsule wall material. A small degree of denaturation is not sufficient to enhance the ability of the protein to protect the core material when used as a wall material, and a large degree of denaturation is also suitable to the contrary, which adversely affects the structure of the protein to exert its protective effect on the core material when used as a wall material. The technical scheme provided by the invention has wide applicability of adjustable parameter items, so that the method can be suitable for preparing microcapsules with various wall material combinations including different protein wall materials.
For the reasons, the power of the ultrasonic modification of the horn is 900-. The power of the water bath ultrasonic modification is 490-630W, the water bath temperature is 60-75 ℃, the ultrasonic frequency is 80-100kHz, and the ultrasonic time is 15-25 min.
Preferably, the emulsifier in step (3) includes, but is not limited to, Tween 80, Tween 60, ML-750, or may be an emulsifier such as a fatty acid ester used as a food emulsifier. The emulsifier is preferably Tween 80 in some embodiments, due to its good emulsifying properties and its wide applicability in the food industry.
More preferably, the mass ratio of the emulsifier to the protein is 0.03:1-0.08: 1.
Preferably, the liquid oil material in step (3) is natural oil or synthetic/purified oil which is liquid at room temperature, such as soybean oil, peanut oil, corn oil, sunflower oil, olive oil and other natural oils, and various synthetic triglycerides and diglycerides and the like, as well as non-triglyceride components such as sterols and phospholipids; the fat-soluble material is a natural or synthetic/purified functional component which can be dissolved in the liquid fat material, such as fatty acid such as EPA, DHA, etc. and esterified derivatives thereof, fat-soluble pigment such as chlorophyll, carotenoid, etc., and fat-soluble vitamin such as vitamin A, D, E.
Preferably, the mass ratio of the liquid grease material and/or the fat-soluble material to the protein in the step (3) is 4:1-1: 2.
Preferably, the macromolecular material in step (4) refers to a macromolecular material negatively charged under acidic conditions, and includes but is not limited to polysaccharide, cellulose or a mixture thereof negatively charged under acidic conditions, and in some aspects is preferably one or more of acacia gum, pectin, carrageenan, chitosan, sodium carboxymethylcellulose and sodium alginate. The macromolecular material negatively charged under acidic conditions is further preferably gum arabic, since gum arabic has good solubility, low viscosity, good adhesion and film-forming properties.
Preferably, the mass ratio of the macromolecular material to the protein in the step (4) is 2:1-1: 2.
Further, the invention provides a method for improving the oxidation resistance of a microcapsule wall material by using the modified protein, which comprises the following steps:
(5) and (3) curing: adjusting the pH value of the system to 3-5, cooling to 10-15 ℃, adjusting the pH value of the system to 5.5-6.5 by using an alkali solution, and adding enzyme for solidification;
(6) enzyme deactivation: transferring the system to a water bath at 90-95 ℃ for 5-10min to inactivate enzyme, and then cooling the system to room temperature;
(7) and (3) drying: and standing the system until the system is layered, removing supernatant, and taking the rest part for drying.
Preferably, the alkali solution in the step (5) is sodium bicarbonate solution or sodium carbonate solution; the kind of the added enzyme is TGase enzyme; the curing time is 3-5 h.
Preferably, the drying device in the step (7) is an air-blast drying oven, the drying temperature is 40-50 ℃, and the drying time is 2-3 h.
The invention also provides a microcapsule product prepared by the method for improving the oxidation resistance of the microcapsule wall material by using the modified protein. The strength of the oxidation resistance of the microcapsule product can be evaluated by measuring the oxidation induction time of the microcapsule embedded with the oil or the oil-soluble core material by an oil oxidation stability tester.
The wall material of the present invention refers to the material constituting the microcapsule wall, and the constituents include protein and negatively charged macromolecular material, as well as part of emulsifier and trace impurities brought by the preparation method which do not affect various chemical and physical properties of the wall material, unless otherwise specified.
Unless otherwise specified, the core material of the present invention refers to the material enclosed by the microcapsule wall in the microcapsule, which comprises liquid fatty material and/or fat-soluble material, and trace impurities brought by the preparation method which do not affect various chemical and physical properties of the wall core.
Meanwhile, the invention also provides an application of the microcapsule product in food, medicine and cosmetic ingredients.
Compared with the prior art, the invention has the following beneficial effects:
(1) the core material of the microcapsule is protected by a pure physical method rather than a chemical method of adding an antioxidant and the like into a wall material or the core material, so that the core material is better protected by the microcapsule. The microencapsulation method is characterized in that a sensitive core material is protected by a physical barrier, and the characteristic advantage of the microencapsulation method is overcome by adding the antioxidant. In addition, the antioxidant itself has the possibility of oxidizing itself or leaching out of the microcapsule, which affects the durability and stability of the antioxidant property of the microcapsule product. Therefore, the modification and preparation method provided by the invention can realize the pure physical protection of unsaturated fat or sensitive fat-soluble ingredient components, and has the advantages of relatively low cost, stable and durable antioxidant effect, easy acceptance by consumers and the like compared with a method for adding an antioxidant to assist in improving the oxidation stability.
(2) In the prior art, the method for increasing the thickness of the wall material layer of the microcapsule can also enhance the protection of the core material of the microcapsule by changing the core-wall ratio, but the loading capacity of the microcapsule is also reduced, so that more macromolecular materials are used as the wall material if a liquid grease material and/or a fat-soluble material with certain mass needs to be microencapsulated, thereby greatly increasing the production cost. The antioxidant property of the microcapsule can be improved without reducing the loading capacity and slightly increasing the production cost by modifying the protein for the microcapsule wall material through a physical method.
(3) The modification of the wall material and the corresponding microcapsule preparation method disclosed by the invention can be popularized to various protein wall materials for improving the oxidation resistance of the microcapsule, and have higher universality. The two ultrasonic modification methods can be suitable for modification of almost all proteins, the protein wall material is one of two most common types in the microcapsule wall material, and the ultrasonic extraction instrument and the ultrasonic water bath cleaning tank are common equipment which are low in price and do not need consumables. Therefore, the modification and preparation method provided by the invention has the advantages of strong operability, wide applicability and low cost.
Detailed Description
The present invention will be further explained with reference to specific examples in order to make the technical means, the technical features, the technical objectives and the effects of the present invention easier to understand, but the following examples are only preferred embodiments of the present invention, and not all embodiments of the present invention. Based on the embodiments in the implementation, other embodiments obtained by those skilled in the art without any creative efforts belong to the protection scope of the present invention.
The experimental methods in the following examples are conventional methods unless otherwise specified, and materials, reagents and the like used in the following examples are commercially available unless otherwise specified. Wherein, the purchasing manufacturers of the gelatin protein, the whey protein, the soybean protein, the chickpea protein, the Arabic gum and the chitosan used in the specific embodiment of the application are Sigma-Aldrich company, and the specification is reagent grade; the purchasing manufacturer of the methyl oleate and the EPA is TCI chemical industry Co., Ltd, and the specification is analytically pure; the olive oil is purchased from Betty and is in food grade. The apparatus used was: the ultrasonic extraction instrument purchasing manufacturer is Shanghai Bilang instrument manufacturing company, and the model is 1000 CT; the water bath ultrasonic instrument is purchased from ultrasonic instrument Co., Ltd of Kunshan city, and has the model of KQ-700 GVDV.
Example 1 (amplitude transformer ultrasonic modified gelatin protein for preparing methyl oleate microcapsule)
A method for improving the oxidation resistance of microcapsule wall materials by using modified gelatin protein comprises the following steps:
1) dissolving 5.00g of gelatin protein in 100mL of water at 55 ℃ under stirring, wherein the dissolving process lasts for more than 60min to ensure full and complete hydration, and performing ultrasonic modification by using a horn ultrasonic cell disruption instrument with the ultrasonic power of 1000W and the ultrasonic time of 20 min;
2) adding 0.25g of Tween 80 into the gelatin protein solution subjected to ultrasonic modification, adding 10.00g of methyl oleate, performing vortex oscillation for 15s in a centrifugal tube for pre-emulsification, transferring to a syringe connected with a 10-micron SPG membrane emulsifier, performing injection by using an injection pump, and repeatedly passing through a membrane for 3 times;
3) mixing the emulsion with 5.00g of Arabic gum in a 45 ℃ constant-temperature container by stirring, adding water to dilute the system to a required concentration, adjusting the system to a target stirring speed, and ensuring that the stirring at the speed is kept until the microcapsule preparation is finished;
4) adjusting the pH value of the system to 3-5 by using acetic acid, slowly reducing the temperature of the system to 15 ℃ after 10min after the target pH value is reached, adjusting the pH value of the system to 6 by using 1mol/L sodium bicarbonate, adding TGase enzyme for starting curing, wherein the addition amount of the enzyme is 100U/g protein, and the curing time is 3 h; the purpose of this step is: the solidification of the wall material layer is carried out, otherwise the binding of the protein to the polysaccharide (complex coacervation process) is a reversible physical change rather than a chemical change.
5) Transferring the system into a water bath at 90 ℃ for 10min to inactivate enzyme, and then transferring into an ice water bath for 10min to reduce the temperature of the system to room temperature; the purpose of this step is: the TGase enzyme used in the previous step was inactivated.
6) Standing the system containing the cured microcapsules for 15min, removing the supernatant, and drying the rest part by using an air-blast drying oven, wherein the drying temperature is 45 ℃ and the drying time is 2 h; the purpose of this step is: the wet microcapsules were dried to obtain microcapsule powder (dry powder).
The oxidation induction time of the methyl oleate microcapsule is measured by using a grease oxidation stability tester, and the result shows that compared with a product prepared by using gelatin protein which is not subjected to ultrasonic modification by an amplitude transformer, the oxidation induction time of the microcapsule prepared by using the modified wall material is improved by 56.5%.
Example 2 (Water bath ultrasound modification of gelatin protein to prepare methyl oleate microcapsules)
A method for improving the oxidation resistance of microcapsule wall materials by using modified gelatin protein comprises the following steps:
1) dissolving 5.00g of gelatin protein in 100mL of water at 55 ℃ under stirring, wherein the dissolving process lasts for more than 60min to ensure sufficient and complete hydration, sealing the container, and then putting the container into an ultrasonic water bath cleaning tank for ultrasonic modification, wherein the water bath temperature is 65 ℃, the ultrasonic power is 560W, the ultrasonic frequency is 100kHz, and the ultrasonic time is 20 min;
2) adding 0.25g of Tween 80 into the gelatin protein solution subjected to ultrasonic modification, adding 10.00g of methyl oleate, performing vortex oscillation for 15s in a centrifugal tube for pre-emulsification, transferring to a syringe connected with a 10-micron SPG membrane emulsifier, performing injection by using an injection pump, and repeatedly passing through a membrane for 3 times;
3) mixing the emulsion with 5.00g of Arabic gum in a 45 ℃ constant-temperature container by stirring, adding water to dilute the system to a required concentration, adjusting the system to a target stirring speed, and ensuring that the stirring at the speed is kept until the microcapsule preparation is finished;
4) adjusting the pH value of the system to 3-5 by using acetic acid, slowly reducing the temperature of the system to 15 ℃ after 10min after the target pH value is reached, adjusting the pH value of the system to 6 by using 1mol/L sodium bicarbonate, adding TGase enzyme for starting curing, wherein the addition amount of the enzyme is 100U/g protein, and the curing time is 3 h;
5) transferring the system into a water bath at 90 ℃ for 10min to inactivate enzyme, and then transferring into an ice water bath for 10min to reduce the temperature of the system to room temperature;
6) standing the system containing the cured microcapsule for 15min, removing the supernatant, and drying the rest part with forced air drying oven at 45 deg.C for 2 hr. The oxidation induction time of the methyl oleate microcapsule is measured by using a grease oxidation stability tester, and the result shows that the oxidation induction time of the microcapsule prepared by the modified wall material is improved by 44.0% compared with the product prepared by gelatin protein which is not subjected to water bath ultrasonic modification.
Example 3 (amplitude transformer ultrasonic modified soy protein to prepare methyl oleate microcapsule)
A method for improving the oxidation resistance of microcapsule wall materials by using modified soybean protein comprises the following steps:
1) dissolving 4.00g of soybean protein in 100mL of water at 45 ℃ under stirring, wherein the dissolving process lasts for more than 60min to ensure full and complete hydration, and performing ultrasonic modification by using a horn ultrasonic cell disruption instrument with the ultrasonic power of 1000W and the ultrasonic time of 25 min;
2) adding 0.20g of Tween 80 into the soybean protein solution subjected to ultrasonic modification, adding 8.00g of methyl oleate, performing vortex oscillation for 15s in a centrifugal tube for pre-emulsification, transferring to a syringe connected with a 10-micron SPG membrane emulsifier, performing bolus injection by using a syringe pump, and repeatedly passing through a membrane for 3 times;
3) mixing the emulsion with 4.00g of Arabic gum in a 45 ℃ constant-temperature container by stirring, adding water to dilute the system to a required concentration, adjusting the system to a target stirring speed, and ensuring that the stirring at the speed is kept until the microcapsule preparation is finished;
4) adjusting the pH value of the system to 2.5-4.5 by using acetic acid, slowly reducing the temperature of the system to 15 ℃ after 10min after the target pH value is reached, adjusting the pH value of the system to 6 by using 1mol/L sodium bicarbonate, adding TGase enzyme to start curing, wherein the addition amount of the enzyme is 80U/g protein, and the curing time is 3 h;
5) transferring the system into a water bath at 90 ℃ for 10min to inactivate enzyme, and then transferring into an ice water bath for 10min to reduce the temperature of the system to room temperature;
6) standing the system containing the cured microcapsules for 15min, removing the supernatant, and drying the rest part by using an air-blast drying oven, wherein the drying temperature is 45 ℃ and the drying time is 2 h;
the oxidation induction time of the methyl oleate microcapsule is measured by using a grease oxidation stability tester, and the result shows that the oxidation induction time of the microcapsule prepared by the modified wall material is improved by 40.2 percent compared with the product prepared by using the soybean protein which is not subjected to ultrasonic modification by an amplitude transformer.
Example 4 preparation of Olive oil microcapsule by ultrasonic modification of whey protein with amplitude transformer
The differences from example 1 are: the steps 1) to 3) are replaced by the following steps:
1) dissolving 5.00g of whey protein in 100mL of water at 50 ℃ under stirring, wherein the dissolving process lasts for more than 60min to ensure full and complete hydration, and performing ultrasonic modification by using a horn ultrasonic cell disruption instrument with the ultrasonic power of 1000W and the ultrasonic time of 20 min;
2) adding 0.20g of ML-750 into the whey protein solution which is subjected to ultrasonic modification treatment, adding 8.50g of olive oil into a centrifugal tube, performing vortex oscillation for 15s for pre-emulsification, transferring to a syringe connected with a 10-micron SPG membrane emulsifier, performing bolus injection by using a syringe pump, and repeatedly passing through a membrane for 3 times;
3) the emulsion was mixed with 3.50g of chitosan in a 45 ℃ thermostatic vessel using stirring, and the system was diluted to the desired concentration by adding water, adjusted to the target stirring speed, and ensured that stirring was maintained at this speed until the end of microcapsule preparation.
The oxidation induction time of the microcapsule prepared by the modified wall material is improved by 39.8 percent.
Example 5 (Water bath ultrasound modified chickpea protein preparation of EPA microcapsules)
The difference from example 3 is: the steps 1) to 3) are replaced by the following steps:
1) dissolving 4.00g of chickpea protein in 100mL of water at 50 ℃ under stirring, wherein the dissolving process lasts for more than 60min to ensure sufficient and complete hydration, sealing the container, and then putting the container into an ultrasonic water bath cleaning tank for ultrasonic modification, wherein the water bath temperature is 70 ℃, the ultrasonic power is 520W, the ultrasonic frequency is 80kHz, and the ultrasonic time is 25 min;
2) adding 0.24g of Tween 60 into the chickpea protein solution subjected to ultrasonic modification, adding 6.00g of EPA into a centrifugal tube, performing vortex oscillation for 15s for pre-emulsification, transferring to a syringe connected with a 10-micron SPG membrane emulsifier, performing injection by using a syringe pump, and repeatedly passing through a membrane for 3 times;
3) the emulsion was mixed with 3.00g gum arabic in a 45 ℃ thermostatic vessel with stirring, and the system was diluted to the desired concentration by adding water, adjusted to the target stirring speed, and kept under stirring at this speed until the end of microcapsule preparation.
The oxidation induction time of the microcapsule prepared by the modified wall material is improved by 43.5 percent.
Comparative example 1
The only difference from example 1 is that: in the step 1), the ultrasonic modification is carried out on the horn ultrasonic cell disruptor, the ultrasonic power is set to 400W, and the rest steps and experimental parameters are the same as those in the embodiment 1. The oxidation induction time of the obtained microcapsule is improved by 20.9 percent.
Comparative example 2
The only difference from example 1 is that: and (3) carrying out ultrasonic modification on the horn ultrasonic cell disruptor in the step 1), setting the ultrasonic time to be 10min, and keeping the rest steps and experimental parameters the same as those in the example 1. The oxidation induction time of the obtained microcapsule is improved by 32.6 percent.
Comparative example 3
The only difference from example 2 is that: the temperature of the water bath in the step 1) was set to 85 ℃, and the rest of the steps and experimental parameters were the same as those in example 2. The oxidation induction time of the obtained microcapsule is improved by 34.8 percent.
Comparative example 4
The only difference from example 2 is that: the ultrasonic time in the step 1) is set to be 40min, and the rest steps and experimental parameters are the same as those in the example 2. The oxidation induction time of the obtained microcapsule is improved by 14.5 percent.
Comparative example 5
The only difference from example 2 is that: step 1) 20.00g of gelatin were dissolved at 55 ℃ with stirring, and the rest of the steps and experimental parameters were the same as in example 2. The experimental results are as follows: solutions of gelatin protein at this concentration are not essentially liquid and have no workable conditions.
Comparative example 6
The only difference from example 3 is that: 0.04g of Tween 80 was added to the ultrasonically modified soybean protein solution in step 2), and the rest of the steps and experimental parameters were the same as those in example 3. The experimental results are as follows: the addition amount of the emulsifier influences the emulsification effect, thereby influencing the embedding rate of the microcapsule and further influencing the oxidation stability of the methyl oleate.
Comparative example 7
The only difference from example 3 is that: and 2) adding 24.0g of methyl oleate into the centrifugal tube, performing vortex oscillation for 15s for pre-emulsification, and performing the rest steps and experimental parameters which are the same as those in the example 1. The experimental results are as follows: the proportion change of the methyl oleate influences the embedding rate of the microcapsules and further influences the oxidation stability of the methyl oleate.
Comparative example 8
The only difference from example 3 is that: step 3) the emulsion was mixed with 15.0g of gum arabic solution in a thermostatic vessel at 45 ℃ with stirring, and the rest of the steps and experimental parameters were the same as those of example 3. The experimental results are as follows: the proportion of the Arabic gum to the protein is changed, so that the complex coacervation effect of the Arabic gum and the gelatin is influenced, and the oxidation stability of the methyl oleate is further influenced.
Finally, it should be noted that the above-mentioned contents are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, and that the simple modifications or equivalent substitutions of the technical solutions of the present invention by those of ordinary skill in the art can be made without departing from the spirit and scope of the technical solutions of the present invention.
Claims (10)
1. A method for improving the oxidation resistance of microcapsule wall materials by using modified proteins is characterized by comprising the following steps:
(1) dissolving protein in water to obtain solution A;
(2) carrying out ultrasonic modification on the solution A to obtain a solution B;
(3) adding an emulsifier into the solution B to obtain a solution C; adding a liquid grease material and/or a fat-soluble material into the solution C, and emulsifying to obtain a liquid D;
(4) adding one or more macromolecular materials into the liquid D to prepare grease or fat-soluble microcapsules; the macromolecular material is polysaccharide or cellulose.
2. The method for improving the antioxidation performance of the wall material of the microcapsule according to claim 1, wherein the protein in the step (1) is one or more selected from gelatin protein, whey protein, soy protein, chickpea protein, broad bean protein, pea protein and peanut protein; the mass ratio of the protein to the water is 1:15-1: 30; the dissolution temperature is 45-55 ℃.
3. The method for improving the antioxidation performance of the microcapsule wall material by using the modified protein according to claim 1, wherein the ultrasonic modification apparatus used in the step (2) is an ultrasonic extraction apparatus or a water bath ultrasonic apparatus.
4. The method for improving the oxidation resistance of the microcapsule wall material by using the modified protein as claimed in claim 3, wherein the ultrasonic power of the ultrasonic extraction instrument is set to 900-; the water bath temperature of the water bath ultrasonic instrument is set to be 60-75 ℃, the ultrasonic power is 490-630W, the ultrasonic frequency is 45-100kHz, and the ultrasonic time is 10-25 min.
5. The method for improving the anti-oxidation performance of the wall material of the microcapsule by using the modified protein as claimed in claim 1, wherein the emulsifier in the step (3) is Tween 80, Tween 60, ML-750 or fatty acid ester; the mass ratio of the emulsifier to the protein is 0.03:1-0.08: 1.
6. The method for improving the antioxidation performance of microcapsule wall materials by using modified proteins as claimed in claim 1, wherein the liquid oil material in step (3) is natural oil or synthetic/purified oil which is liquid at normal temperature, preferably soybean oil, peanut oil, corn oil, sunflower seed oil, olive oil, EPA, DHA; the fat-soluble material is natural or synthetic/purified functional component soluble in liquid oil material, preferably chlorophyll, carotenoid, vitamin A, vitamin D, and vitamin E.
7. The method for improving the oxidation resistance of the wall material of the microcapsule by using the modified protein as claimed in claim 1, wherein the mass ratio of the liquid lipid material and/or the fat-soluble material to the protein in the step (3) is 4:1-1: 2.
8. The method for improving the oxidation resistance of the wall material of the microcapsule by using the modified protein as claimed in claim 1, wherein the macromolecular material in the step (4) is one or more of acacia gum, pectin, carrageenan, chitosan, sodium carboxymethylcellulose and sodium alginate; the mass ratio of the macromolecular material to the protein is 2:1-1: 2.
9. A microcapsule product prepared by the method for improving the oxidation resistance of the microcapsule wall material by using the modified protein according to any one of claims 1 to 8.
10. Use of the microcapsule product according to claim 9 in food, pharmaceutical and cosmetic ingredients.
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