Dha microcapsule powder and method of making the same

By combining enzymatically modified edible protein with small molecule fillers and natural antioxidants in an irreversible thermal colloid, highly stable DHA microcapsule powder was prepared, solving the problem of easy oxidation of DHA oil microencapsulation products at high temperatures and in external environments, and achieving high oil loading capacity, high encapsulation rate and excellent stability.

CN117770453BActive Publication Date: 2025-12-26SHANGHAI TONGYI BIOTECHNOLOGY CO LTD
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Patent Information

Application Number
CN202410082684.8
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-01-19
Publication Date
2025-12-26
Estimated Expiration
2044-01-19

AI Technical Summary

Technical Problem

Existing DHA lipid microencapsulated products are prone to oxidation at high temperatures and in external environments, resulting in unstable capsule wall structures, nutrient loss, and product insensitivity to high temperatures.

Method used

Enzyme-modified edible protein and thermally irreversible colloid were used as microcapsule wall materials, combined with small molecule fillers and natural antioxidants, to prepare DHA microcapsule powder by spray drying, forming a dense network spatial thin shell to improve stability.

Benefits of technology

This improves the oil loading capacity, encapsulation efficiency, and excellent stability of DHA microcapsule powder, making it suitable for use in beverages, cheese, and baking industries, extending product shelf life and reducing oxidation rates.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application relates to a DHA microcapsule powder and a preparation method thereof, which comprises the following components in percentage by mass: DHA oil 25-50%, edible protein 20-40%, small molecule filler 5-25%, edible colloid 2-10%, emulsifier 0.5-8% and antioxidant 0.1-5%. The edible protein, the small molecule filler and the edible colloid are microcapsule wall materials in the DHA microcapsule powder, and the edible protein is an enzyme-modified edible protein obtained through a deamidation reaction by using a protein glutamine enzyme. The enzyme-modified edible protein is obtained through a deamidation reaction by using a protein glutamine enzyme, the solubility, emulsification and oil holding capacity of the protein wall material are effectively improved, the edible colloid is used to form a protein-colloid embedding network system, the small molecule filler is added to exist in a glass state between capsules and on the surface of capsule walls, and the antioxidant is used to inhibit oxidation, so that the obtained DHA oil microcapsule powder has high oil loading, high embedding rate, excellent stability and mixing performance, and is widely applicable to the fields of drinks, cheese and baking.
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Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of polyunsaturated fatty acid nutritional product preparation, in particular to a DHA microcapsule powder and a preparation method thereof. BACKGROUND

[0002] DHA (docosahexaenoic acid) is commonly known as brain gold, and belongs to omega-3 series polyunsaturated fatty acids. As a highly unsaturated fatty acid, it contains 22 carbon atoms and 6 double bonds, and cannot be synthesized by the human body itself and must be obtained from the outside world. Since DHA accounts for about 20% in the cerebral cortex of the human brain and about 50% in the retina of the eye, it has important functions such as promoting the intelligence and visual development of fetuses, infants and young children, and therefore has good market development prospects.

[0003] DHA is a polyunsaturated fatty acid containing multiple "carbon double bond" structures and 5 active methylene groups. These active methylene groups make DHA extremely susceptible to external environmental factors such as light, oxygen, heat and metal elements, as well as free radicals, resulting in chemical reactions such as oxidation, rancidity, polymerization and double bond conjugation, producing fishy substances mainly in the form of carbonyl compounds. Oxidized DHA not only loses its original nutritional and medicinal value, but also is harmful to the human body. Moreover, the direct use of DHA oil products in food increases the opportunity of contact with external environmental factors, and oxidation is extremely easy to occur. Therefore, the powder product of microencapsulated DHA is generally added.

[0004] Microencapsulation is a technology of embedding solid, liquid and gaseous substances into small, semi-permeable or closed capsules. When DHA oil is used in food, microencapsulated products are mainly used, and the oil rich in DHA is microencapsulated. After microencapsulation, a protective layer is formed on the oil by the wall material, which can improve the operability of the oil, isolate it from the external environment, reduce the oxidation and rancidity rate, reduce the fishy smell of the oil, and maximize the preservation of the original color, aroma and taste, prevent the destruction of nutritional ingredients, and change the form of the oil from liquid to solid, making it easier to use and store.

[0005] It should be noted that the selection of wall material and antioxidant is a key factor affecting the microencapsulation and stability of DHA oil. The wall material not only has high water solubility, but also has good film-forming property, emulsifying property and high temperature resistance. At present, protein, plant gum and starch are commonly used as wall materials. However, under normal circumstances, the wall material is simply compounded to form an emulsion, the formed capsule wall is easy to be loose and porous, and cannot withstand the high energy during the spray drying atomization in the preparation process, which easily causes "demulsification", and the fat is exposed to high temperature oxidation. In addition, the formed microcapsules are easily affected by external environment such as humidity and temperature, resulting in the collapse of the capsule wall structure and the entry of oxygen for oxidation.

[0006] Therefore, it is an urgent problem to provide a DHA oil microcapsule powder product with high temperature resistance and high stability to meet the application development needs of market products. SUMMARY

[0007] Therefore, the present application provides a DHA microcapsule powder and a preparation method thereof to solve the above problems.

[0008] According to an aspect of the present application, a DHA microcapsule powder is provided, comprising the following components in mass percentage:

[0009] DHA oil 25-50%, edible protein 20%-40%, small molecule filler 5-25%, edible colloid 2-10%, emulsifier 0.5-8%, and antioxidant 0.1-5%;

[0010] The edible protein, the small molecule filler, and the edible colloid are microcapsule wall materials in the DHA microcapsule powder, and the edible protein is an enzyme-modified edible protein obtained by a deamidation reaction using a protein glutamine enzyme.

[0011] In a possible implementation, the edible protein includes at least one of whey protein, sodium caseinate, soy protein, pea protein, or walnut protein.

[0012] In a possible implementation, the small molecule filler includes at least one of trehalose, pullulan, soybean polysaccharide, lactose, maltose, glucose, fructose, cluster dextrin, glucose syrup, or solid corn syrup.

[0013] In a possible implementation, the edible colloid is curdlan.

[0014] In a possible implementation, the emulsifier includes at least one of polyglyceryl ricinoleate, glyceryl caprylocaprate, polyglyceryl-10-myristate, decaglyceryl monostearate, decaglyceryl pentaoleate, pentaerythritol trioleate, polyoxyethylene sorbitol monolaurate, or sodium stearoyl lactylate.

[0015] In a possible implementation, the antioxidant includes an oil-phase antioxidant and a water-phase antioxidant.

[0016] In a possible implementation, the oil-phase antioxidant includes at least one of r-glutamic acid, bamboo leaf antioxidant, liquorice antioxidant, rosemary, or gallic propionic acid ester.

[0017] In a possible implementation, the water-phase antioxidant includes at least one of tea polyphenol, sodium ascorbate, ascorbic acid, lactic acid, malic acid, tannic acid, or citric acid and salts thereof.

[0018] According to another aspect of the present application, a preparation method of the DHA microcapsule powder is provided for preparing the DHA microcapsule powder of any one of the above, comprising the following preparation steps:

[0019] The edible protein is put into water, and a protein glutamine enzyme is added to react with a substrate ratio of 3-20 u / g, and then inactivated after the reaction is completed, and cooled to obtain an enzyme-modified edible protein;

[0020] The small molecule filler, edible colloid and emulsifier are added to the enzyme-modified edible protein, and the mixture is heated and stirred under a preset heating condition to obtain an aqueous phase liquid;

[0021] The DHA oil and the oil-phase antioxidant in the antioxidant are mixed to obtain an oil-phase liquid;

[0022] The oil-phase liquid and the aqueous-phase liquid are mixed, and the water-phase antioxidant in the antioxidant is added, and the mixture is sheared to obtain an emulsion;

[0023] The emulsion is subjected to two times of homogenization under a preset homogenization condition, and then sterilized;

[0024] The emulsion after sterilization is subjected to spray drying to obtain the DHA microcapsule powder; and when the spray drying is performed, the inlet air temperature is 170-190 DEG C, and the outlet air temperature is 80-100 DEG C.

[0025] In a possible implementation manner, the preset homogenization condition comprises:

[0026] The first homogenization pressure is 20-30 MPa, and the second homogenization pressure is 30-40 MPa.

[0027] The DHA microcapsule powder of the present application has the following beneficial effects:

[0028] The DHA microcapsule powder of the present application uses edible protein as the main part of the wall material in the DHA microcapsule powder, and specifically uses enzyme-modified edible protein obtained by using a protein glutamine enzyme for deamidation reaction to effectively improve the solubility, emulsification and oil holding capacity of the protein wall material, and comprises the following components in percentage by mass: DHA oil 25-50%, edible protein 20%-40%, small molecule filler 5-25%, edible colloid 2-10%, emulsifier 0.5-8% and antioxidant 0.1-5%. That is, the enzyme-modified edible protein is supplemented with edible colloid to form a protein-colloid embedding network system, and the small molecule filler is added to exist in a glass state in the capsules and on the surface of the capsule wall to inhibit the entry of oxygen. And the natural antioxidant is added to inhibit the oxidation reaction, and the formed DHA oil microcapsule powder has high oil loading, high embedding rate, excellent stability and reconstitution, and is widely applicable to the edible fields such as drinks, cheese and baking.

[0029] Other features and aspects of the present application will become apparent from a detailed description of exemplary embodiments with reference to the accompanying drawings. BRIEF DESCRIPTION OF DRAWINGS

[0030] The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate exemplary embodiments, features, and aspects of the application and serve to explain the principles of the application.

[0031] Figure 1 Flow chart of the preparation method of DHA microcapsule powder of the embodiments of the present application. DETAILED DESCRIPTION

[0032] Various exemplary embodiments, features, and aspects of the present application will be described below in detail with reference to the accompanying drawings. The same reference numbers in different drawings represent the same or similar elements. Although various aspects of the embodiments are illustrated in the drawings, the drawings are not necessarily drawn to scale unless specifically indicated.

[0033] Wherein, it is to be understood that the terms "center", "longitudinal", "lateral", "length", "width", "upper", "lower", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", "clockwise", "counterclockwise", "axial", "radial", "circumferential" and the like indicate the orientation or positional relationship based on the orientation or positional relationship shown in the drawings, and are only for the convenience of describing the present application or simplifying the description, and therefore cannot be understood as indicating or implying that the devices or elements referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore cannot be understood as limiting the present application.

[0034] In addition, the terms "first", "second" are only for descriptive purposes and cannot be understood as indicating or implying relative importance or implicitly indicating the number of the technical features indicated. Therefore, the features defined with "first", "second" can explicitly or implicitly include one or more of the features. In the description of the present application, the meaning of "a plurality of" is two or more, unless otherwise specifically limited.

[0035] The word "exemplary" is used herein to mean "serving as an example, instance, or illustration." Any implementation described herein as "exemplary" is not necessarily to be construed as preferred or advantageous over other implementations.

[0036] In addition, in order to better illustrate the present application, a large number of specific details are given in the specific embodiments below. Those skilled in the art should understand that the present application can also be implemented without certain specific details. In some examples, methods, means, elements and circuits well known to those skilled in the art are not described in detail, in order to highlight the main idea of the present application.

[0037] As shown in Table 1, in one aspect of the present application, a DHA microcapsule powder is provided, which comprises the following components in mass percentage:

[0038] DHA oil 25-50%, edible protein 20%-40%, small molecule filler 5-25%, edible colloid 2-10%, emulsifier 0.5-8%, and antioxidant 0.1-5%;

[0039] The edible protein, the small molecule filler, and the edible colloid are microcapsule wall materials in the DHA microcapsule powder, and the edible protein is an enzyme-modified edible protein obtained by a deamidation reaction using a protein glutamine enzyme.

[0040] Raw material composition Mass percentage (%) DHA oil 25-50 Edible protein 20-40 Small molecule filler 5-25 Edible colloid 2-10 Emulsifier 0.5-8 Antioxidant 0.1-5

[0041] Table 1: Mass percentage of each raw material in the DHA microcapsule powder

[0042] In this embodiment, the edible protein is the main part of the wall material in the DHA microcapsule powder, and specifically, an enzyme-modified edible protein is used, and a deamidation reaction is performed using a protein glutamine enzyme to effectively improve the solubility, emulsification, and oil holding capacity of the protein wall material. The edible colloid forms a protein-colloid embedding network system, and the small molecule filler exists in a glassy state between the capsules and on the surface of the capsule wall to inhibit the entry of oxygen. In addition, natural antioxidants are added to inhibit oxidation reactions, and the formed DHA oil microcapsule powder has high oil loading, high embedding rate, excellent stability, and excellent reconstitution, and is widely applicable in the fields of food, cheese, and baking.

[0043] Specifically, the mass percentage of each raw material is as follows: DHA oil 25-50%, edible protein 20%-40%, small molecule filler 5-25%, edible colloid 2-10%, emulsifier 0.5-8%, and antioxidant 0.1-5%. The enzyme-modified edible protein, the small molecule filler, and the edible colloid are used as the microcapsule wall material, and the emulsifier and the antioxidant are used as auxiliary materials. It should be noted that the DHA oil is microencapsulated by a spray drying method. Preferably, the DHA oil is 30-40%, the edible protein is 30-40%, the small molecule filler is 10-15%, the edible colloid is 5-10%, the emulsifier is 2-5%, and the antioxidant is 0.5-3%.

[0044] In one possible implementation, the edible protein includes at least one of whey protein, sodium caseinate, soy protein, pea protein, or walnut protein.

[0045] It should be noted that the enzyme-modified edible protein in the embodiment is an edible protein after deamidation reaction by protein glutamine enzyme, i.e., PG enzyme, and preferably one or more of whey protein, sodium caseinate, soy protein, pea protein and walnut protein, and the content of the enzyme-modified edible protein is controlled to be between 25-45%.

[0046] In a possible implementation manner, the small molecule filler includes at least one of trehalose, pullulan, soybean polysaccharide, lactose, maltose, glucose, fructose, cluster dextrin, glucose syrup or solid corn syrup.

[0047] That is, the small molecule filler as the wall material in the embodiment preferably includes one or more of trehalose, pullulan, soybean polysaccharide, lactose, maltose, glucose, fructose, cluster dextrin, glucose syrup and solid corn syrup, and the specific content is controlled to be between 5-25%.

[0048] In a possible implementation manner, the edible colloid is gellan gum.

[0049] It should be noted that the edible colloid in the embodiment is a thermal irreversible colloid, and preferably gellan gum, and the enzyme-modified edible protein is used as the main wall material, and the thermal irreversible colloid is supplemented, so as to form a protein-colloid embedding network system.

[0050] In a possible implementation manner, the emulsifier includes at least one of polyglycerol ricinoleate, glyceryl caprylocaprate, polyglyceryl-10-myristate, decaglyceryl monostearate, decaglyceryl pentaoleate, pentaerythritol trioleate, polyoxyethylene sorbitol monolaurate or sodium stearoyl lactylate.

[0051] In a possible implementation manner, the antioxidant includes an oil-phase antioxidant and a water-phase antioxidant. That is, the antioxidant in the embodiment is a mixture of the oil-phase antioxidant and the water-phase antioxidant. In a possible implementation manner, the oil-phase antioxidant includes at least one of r-glutamic acid, bamboo leaf antioxidant, liquorice antioxidant, rosemary or gallic propionic acid ester. In a possible implementation manner, the water-phase antioxidant includes at least one of tea polyphenol, sodium ascorbate, ascorbic acid, lactic acid, malic acid, tannic acid or citric acid and salts thereof. That is, the oil-phase antioxidant preferably includes one or more of r-glutamic acid, bamboo leaf antioxidant, liquorice antioxidant, rosemary and gallic propionic acid ester, which is used to mix with DHA oil to prepare an oil-phase liquid during preparation. The water-phase antioxidant preferably includes one or more of tea polyphenol, sodium ascorbate, ascorbic acid, lactic acid, malic acid, tannic acid and citric acid and salts thereof, which is used to mix with the water-phase liquid prepared by the small molecule filler, the edible colloid and the emulsifier, and the oil-phase liquid to prepare an emulsion liquid. In a possible implementation manner, the antioxidant includes an oil-phase antioxidant and a water-phase antioxidant. That is, the antioxidant in the embodiment is a mixture of the oil-phase antioxidant and the water-phase antioxidant. In a possible implementation manner, the oil-phase antioxidant includes at least one of r-glutamic acid, bamboo leaf antioxidant, liquorice antioxidant, rosemary or gallic propionic acid ester. In a possible implementation manner, the water-phase antioxidant includes at least one of tea polyphenol, sodium ascorbate, ascorbic acid, lactic acid, malic acid, tannic acid or citric acid and salts thereof. That is, the oil-phase antioxidant preferably includes one or more of r-glutamic acid, bamboo leaf antioxidant, liquorice antioxidant, rosemary and gallic propionic acid ester, which is used to mix with DHA oil to prepare an oil-phase liquid during preparation. The water-phase antioxidant preferably includes one or more of tea polyphenol, sodium ascorbate, ascorbic acid, lactic acid, malic acid, tannic acid and citric acid and salts thereof, which is used to mix with the water-phase liquid prepared by the small molecule filler, the edible colloid and the emulsifier, and the oil-phase liquid to prepare an emulsion liquid.

[0052] Therefore, it can be known that in order to provide a DHA microcapsule powder with high stability, the enzyme modified protein, small molecule filler and heat irreversible colloid are used as the microcapsule wall material, supplemented with emulsifiers and natural antioxidants, and the spray drying method is used for microencapsulating the DHA oil. It should be particularly emphasized that the protein glutamine enzyme, i.e., PG enzyme, can convert glutamine on the side chain of the protein into glutamic acid, thereby increasing the number of negatively charged carboxyl groups in the protein, so as to improve the solubility, flexibility, emulsification and oil holding capacity of the edible protein. According to research, with the increase of the deamidation degree, the emulsification performance and oil holding capacity of the protein will be improved. At the same time, the cysteine residues in the protein mainly exist in the form of disulfide bond or sulfhydryl. The disulfide bond can make the spatial structure of the protein peptide chain more compact, and plays an important role in maintaining the natural conformation of the protein. With the increase of the deamidation degree, the surface sulfhydryl is reduced, and the PG deamidation reaction can promote the conversion to disulfide bond, so that the spatial structure of the protein is more compact. It should be further pointed out that the konjac gum can form a complex and stable three-helix structure due to the interaction between the molecules and the combination of intermolecular hydrogen bonds. The konjac gum has heat gelation and strong oil encapsulation, and the gel does not separate from the oil during and after the formation. Due to the good heat resistance, adhesion and film forming property, the konjac gum is widely used in various fields of food industry. Therefore, the DHA oil microcapsule powder prepared by combining the enzyme modified protein and the heat irreversible colloid has excellent high embedding rate, high temperature resistance, excellent stability and reconstitution property, can effectively reduce and delay the oxidation speed of DHA in the process of high temperature treatment such as cooking, sterilization and drying, improve the oxidation stability of DHA in the application process and storage period, and prolong the shelf life of the product.

[0053] As shown in Figure 1 According to another aspect of the present application, a preparation method of the DHA microcapsule powder is provided for preparing the DHA microcapsule powder described in any one of the above, comprising the following preparation steps:

[0054] S100, putting edible protein into water, adding protein glutamine enzyme, controlling the ratio of the protein glutamine enzyme to the substrate to be 3-20 u / g for reaction, inactivating after the reaction is completed, cooling, and obtaining enzyme modified edible protein;

[0055] S200, adding small molecule filler, edible colloid and emulsifier into the enzyme modified edible protein, and heating and stirring under a preset heating condition to obtain an aqueous phase liquid;

[0056] S300, mixing DHA oil and oil phase antioxidant in the antioxidant to obtain an oil phase liquid;

[0057] S400, mixing the oil phase liquid and the aqueous phase liquid, and adding the aqueous phase antioxidant in the antioxidant, and shearing to obtain an emulsion.

[0058] S500, sterilizing the emulsion after twice homogenization under preset homogenization conditions;

[0059] S600, spray drying the sterilized emulsion to obtain DHA microcapsule powder; and during the spray drying, the inlet air temperature is 170-190°C, and the outlet air temperature is 80-100°C.

[0060] It should be noted that during the preparation of the DHA microcapsule powder, the selection of the wall material, the antioxidant, and the processing technology of the wall material are crucial. Therefore, in the preparation of the DHA microcapsule powder, the application selects edible proteins such as whey protein and edible colloids such as gellan gum, which are all high molecular compounds. After the protein is modified by PG enzyme treatment, it has excellent solubility, emulsifying property, flexibility, film-forming property, and stability. Gellan gum has a unique three-dimensional spiral structure, thermal gelation property, and high oil loading capacity. The cross-linking effect of the modified protein greatly improves the microcapsule embedding rate, oil loading rate, and thermal stability. After the DHA oil is microencapsulated by the spray drying method, the obtained DHA microcapsule powder has a dense network space shell. The use of natural antioxidants maximally protects the occurrence of DHA oxidation failure, so that the DHA microcapsule powder has good high temperature resistance, high embedding rate, and high oxidation stability.

[0061] Specifically, in step S100, the edible protein is put into water, and protein glutamine enzyme is added, and the ratio of the protein glutamine enzyme to the substrate is controlled to be 3-20 u / g for reaction. After the reaction is completed, the enzyme is inactivated, and the temperature is lowered to obtain the enzyme-modified edible protein.

[0062] Before step S100 is performed, the preparation raw materials of the DHA microcapsule powder are obtained according to a preset ratio, specifically including DHA oil 25-50%, edible protein 20%-40%, small molecule filler 5-25%, edible colloid 2-12%, emulsifier 0.5-8%, and antioxidant 0.1-5%. It should be noted that the antioxidant includes oil-phase antioxidant and water-phase antioxidant, that is, the antioxidant of the application is a combination of oil-soluble antioxidant and water-soluble antioxidant. After obtaining each preparation raw material, the edible protein therein is put into water at 50-55°C, PG enzyme is added, the ratio of the enzyme to the substrate is 3-20 u / g, and the reaction is performed for 1 h. After the reaction is completed, the enzyme is inactivated in a water bath at 80°C for 5 min, and then the temperature is lowered to 50-60°C for standby.

[0063] Subsequently, in step S200, the small molecule filler, the edible colloid, and the emulsifier are added to the enzyme-modified edible protein, and the mixture is heated and stirred under preset heating conditions to obtain the water-phase liquid.

[0064] Specifically, the small molecule filler, edible colloid and emulsifier are added into the enzyme-modified edible protein obtained in step S100, and the mixture is incubated and stirred under preset incubation conditions, wherein the preset incubation conditions include: an incubation temperature of 50-60°C, an incubation time of 20-30 min, and stirring during incubation, to obtain an aqueous phase liquid.

[0065] Further, the DHA oil is mixed with the oil-soluble antioxidant to obtain a uniform oil phase liquid.

[0066] Further, the oil phase liquid and the aqueous phase liquid are mixed, and the water-soluble antioxidant is added, and the mixture is sheared to obtain an emulsion.

[0067] It should be noted that in step S400, the oil phase liquid is first added to the aqueous phase liquid, and then the water-soluble antioxidant is added, and the mixture is sheared at a speed of 5000-7000 r / min for 10-15 min to obtain an emulsion.

[0068] The emulsion obtained in step S400 is subjected to two homogenization processes under preset homogenization conditions, and then subjected to sterilization treatment.

[0069] In one possible implementation, the preset homogenization conditions include:

[0070] The first homogenization pressure is 20-30 MPa, and the second homogenization pressure is 30-40 MPa.

[0071] That is, the emulsion obtained in step S400 is subjected to two homogenization processes, wherein the first homogenization pressure is 20-30 MPa, and the second homogenization pressure is 30-40 MPa, and then sterilization is performed at a temperature of 65-70°C for 25-30 min.

[0072] Finally, the sterilized emulsion is subjected to spray drying in step S600 to obtain a DHA microcapsule powder; and during the spray drying, the inlet air temperature is 170-190°C, and the outlet air temperature is 80-100°C.

[0073] That is, the homogenized and sterilized emulsion is subjected to spray drying, wherein the spray drying conditions are an inlet air temperature of 170-190°C and an outlet air temperature of 80-100°C, thereby obtaining a DHA oil microcapsule powder with high temperature resistance and high embedding rate. In step S600, the DHA microcapsule powder after spray drying is preferably passed through a 60-80 mesh vibrating screen to screen out particles with a size that is too large.

[0074] Therefore, the high-stable DHA oil microcapsule powder prepared by the application adopts the complexation of the modified protein wall material, heat-resistant colloid and food emulsifier to form a dense network space shell around the core material DHA oil, which can make the DHA hardly affected by the external high-temperature environmental factors, and the addition of the natural antioxidant composition can effectively prevent the damage of metal ions and peroxides to DHA, so that the prepared DHA oil microcapsule powder has high embedding rate, good high-temperature resistance and oxidation stability, and solves the problems of low embedding rate, poor high-temperature resistance and easy oxidation of the existing DHA oil microcapsule powder.

[0075] Moreover, the DHA oil microcapsule powder prepared by the application has high stability, wide high-temperature resistance range and strong oxidation stability, can be added to baked foods and can be applied to other foods (such as milk tablets, candies, ham sausages, beverages, rice products, etc.) with high-temperature processing technology, and due to the dense structure of the DHA oil microcapsule powder, the oxidation damage of metal ions and oxygen to DHA can be effectively isolated, the oxidation speed of DHA can be more effectively reduced and delayed, the oxidation stability of DHA can be improved, and the shelf life of the product can be prolonged.

[0076] The following will provide examples 1-3 and comparative example 1 for further illustration.

[0077] Example 1

[0078] A DHA microcapsule powder, comprising the following components in mass percentage:

[0079] DHA oil 35%, antioxidant 0.5%, whey protein 34%, emulsifier 3.5%, small molecule filler 20% and gum 7.0%;

[0080] The antioxidant comprises rosemary 0.2%, tea polyphenol 0.2% and sodium ascorbate 0.1%;

[0081] The emulsifier is polyglycerol ricinoleate;

[0082] The small molecule filler is lactose.

[0083] The preparation method of the DHA microcapsule powder comprises the following preparation steps:

[0084] 1. The whey protein is put into 50-55 DEG C. water, PG enzyme is added, the enzyme to substrate ratio is 7u / g, and the reaction is carried out for 1h. After the reaction is completed, the enzyme is inactivated in a water bath at 80 DEG C. for 5min, and then the temperature is reduced to 50-60 DEG C. for standby;

[0085] 2. Add the small molecule filler lactose, gellan gum, and emulsifier polyglyceryl ricinoleate to the enzyme-modified protein obtained in 1, and incubate at 50-60°C for 20-30 min while stirring to obtain an aqueous phase liquid;

[0086] 3. Mix the DHA oil and the oil phase antioxidant rosemary at 50-60°C for 10-20 min to obtain a uniform oil phase liquid;

[0087] 4. Add the oil phase liquid to the aqueous phase liquid, and add the aqueous phase antioxidant tea polyphenol and sodium ascorbate, and shear at a speed of 5000-7000 r / min for 10-15 min to obtain an emulsion;

[0088] 5. Homogenize the emulsion twice, at a first homogenization pressure of 20-30 MPa and a second homogenization pressure of 30-40 MPa, and then sterilize at 65-70°C for 25-30 min;

[0089] 6. Spray dry the homogenized and sterilized emulsion under the following conditions: 170-190°C and an air outlet temperature of 80-100°C to obtain a DHA oil microcapsule powder with high temperature resistance and high embedding rate.

[0090] The DHA oil microcapsule powder obtained in Example 1 is a white powder with uniform particle size, can pass through a 60-80 mesh standard sieve, the surface oil rate of the microcapsule powder is 0.14%, the embedding rate is 99.86%, the DHA content of the DHA algal oil microcapsule powder is 14%, and the peroxide value after 21 days of accelerated experiment at 60°C is 0.45 mmol / kg.

[0091] Example 2

[0092] A DHA microcapsule powder, comprising the following components by mass percentage:

[0093] DHA oil 34%, antioxidant 0.5%, soybean protein 34%, emulsifier 3.5%, small molecule filler 20%, and gellan gum 7.0%;

[0094] The antioxidant includes bamboo leaf antioxidant 0.2%, tea polyphenol 0.2%, and ascorbic acid 0.1%;

[0095] The emulsifier is glyceryl caprylocaprate;

[0096] The small molecule filler is lactose;

[0097] A preparation method of the DHA microcapsule powder, comprising the following preparation steps:

[0098] 1. Put soybean protein into 50-55℃ water, add PG enzyme, so that the enzyme to substrate ratio is 7u / g, and react for 1h. After the reaction, inactivate at 80℃ water bath for 5min, then cool to 50-60℃, and reserve;

[0099] 2. Add small molecule fillers lactose, pullulan, and emulsifier glyceryl monolinoleate into the enzyme-modified protein obtained in 1, and incubate at 50-60℃ for 20-30min, and stir at the same time, to obtain an aqueous phase liquid;

[0100] 3. Mix DHA oil and oil phase antioxidant bamboo leaf antioxidant at 50-60℃ for 10-20min, to obtain a uniform oil phase liquid;

[0101] 4. Put the oil phase liquid into the aqueous phase liquid, and add aqueous phase antioxidants tea polyphenol and ascorbic acid, and shear at a speed of 5000-7000r / min for 10-15min, to obtain an emulsion;

[0102] 5. Homogenize the emulsion twice, the first time at a pressure of 20-30MPa, and the second time at a pressure of 30-40MPa, then sterilize at 65-70℃ for 25-30min;

[0103] 6. Spray dry the homogenized and sterilized emulsion, the spray drying conditions are 170-190℃, and the air outlet temperature is 80-100℃, to obtain a high-temperature-resistant, high-embedding-rate DHA oil microcapsule powder.

[0104] The DHA oil microcapsule powder obtained in Example 2 is white powder, the particle size is uniform, can pass through a 60-80 mesh standard sieve, the surface oil rate of the microcapsule powder is 0.17%, and the embedding rate is 99.83%. The DHA content of the DHA algal oil microcapsule powder this time is 14%, and the peroxide value after 21 days of accelerated experiment at 60℃ is 0.37mmol / kg.

[0105] Example 3

[0106] A DHA microcapsule powder, comprising the following components in mass percentage:

[0107] DHA oil 38%, antioxidant 0.5%, pea protein 33%, emulsifier 3.5%, small molecule filler 18%, and pullulan 7.0%;

[0108] The antioxidant comprises glycyrrhizic antioxidant 0.2%, tea polyphenol 0.2%, and sodium citrate 0.1%;

[0109] The emulsifier is polyoxyethylene sorbitol monolaurate;

[0110] The small molecule filler is cluster dextrin.

[0111] The preparation method of the DHA microcapsule powder comprises the following preparation steps:

[0112] 1. Put the pea protein into water at 50-55℃, add PG enzyme to make the enzyme to substrate ratio 10u / g, and react for 1h. After the reaction, inactivate at 80℃ water bath for 5min, then cool to 50-60℃ for standby;

[0113] 2. Add the small molecule filler cluster dextrin, curdlan, and emulsifier polyoxyethylene sorbitol monolaurate into the enzyme modified protein obtained in 1, and keep at 50-60℃ for 20-30min, and stir at the same time to obtain the water phase liquid;

[0114] 3. Mix the DHA oil and oil phase antioxidant glycyrrhizin antioxidant at 50-60℃ for 10-20min to obtain a uniform oil phase liquid;

[0115] 4. Put the oil phase liquid into the water phase liquid, and add the water phase antioxidant tea polyphenol and sodium citrate, and shear at a speed of 5000-7000r / min for 10-15min to obtain an emulsion;

[0116] 5. Homogenize the emulsion twice, the first time at a pressure of 20-30MPa, and the second time at a pressure of 30-40MPa, and then sterilize at 65-70℃ for 25-30min;

[0117] 6. Spray dry the homogenized and sterilized emulsion, and the spray drying conditions are 170-190℃ and an air outlet temperature of 80-100℃ to obtain a DHA oil microcapsule powder with high temperature resistance and high embedding rate.

[0118] The DHA oil microcapsule powder obtained in Example 3 is a white powder with uniform particle size, can pass through a 60-80 mesh standard sieve, the surface oil rate of the microcapsule powder is 0.2%, the embedding rate is 99.80%, the DHA content of the DHA algal oil microcapsule powder is 15.2%, and the peroxide value after 21 days of accelerated experiment at 60℃ is 0.51mmol / kg.

[0119] Comparative Example 1

[0120] A DHA microcapsule powder comprises the following components by mass percentage:

[0121] DHA oil 38%, antioxidant 0.5%, whey protein 33%, emulsifier 3.5%, and small molecule filler 25%;

[0122] The antioxidant comprises VE 0.2%, ascorbic acid palmitate 0.2%, and sodium citrate 0.1%;

[0123] The emulsifier is polyoxyethylene sorbitan monolaurate;

[0124] The small molecule filler is maltodextrin;

[0125] The preparation method of the DHA microcapsule powder comprises the following preparation steps:

[0126] 1. The whey protein, the small molecule filler maltodextrin, and the emulsifier polyoxyethylene sorbitan monolaurate are incubated at 50-60°C for 20-30 min, and stirring is performed at the same time to obtain an aqueous phase liquid;

[0127] 2. The DHA oil is mixed with the oil phase antioxidant VE and ascorbic acid palmitate at 50-60°C for 10-20 min to obtain a uniform oil phase liquid;

[0128] 3. The oil phase liquid is poured into the aqueous phase liquid, and the aqueous phase antioxidant sodium citrate is added, and shearing is performed at a speed of 5000-7000 r / min for 10-15 min to obtain an emulsion;

[0129] 4. The emulsion is subjected to two times of homogenization, the first time of homogenization is at a pressure of 20-30 MPa, and the second time of homogenization is at a pressure of 30-40 MPa, and then sterilization is performed at 65-70°C for 25-30 min;

[0130] 5. The emulsion after homogenization and sterilization is subjected to spray drying, the spray drying conditions are 170-190°C and an air outlet temperature of 80-100°C, and a DHA oil microcapsule powder with high temperature resistance and high embedding rate is obtained.

[0131] The DHA oil microcapsule powder obtained in Comparative Example 1 is a white powder, the particle size is uniform, can pass through a 60-80 mesh standard sieve, the surface oil rate of the microcapsule powder is 1.7%, and the embedding rate is 98.3%. The DHA content of the DHA algal oil microcapsule powder is 15.2%, and the peroxide value is 1.86 mmol / kg after 21 days of 60°C accelerated experiment.

[0132] In summary, according to the comparison results of Examples 1-3 and Comparative Example 1, the surface oil rates of the DHA microcapsule powders of Examples 1-3 are lower, being 0.14%, 0.17% and 0.2% respectively, and the embedding rates are higher, being 99.86%, 99.83% and 99.8% respectively, while the surface oil rate of Comparative Example 1 is higher, being 1.7%, and the embedding rate is lower, being 98.3%. Furthermore, the 21-day peroxide values of Examples 1-3 are much smaller than that of Comparative Example 1, being 0.45 mmol / kg, 0.37 mmol / kg and 0.51 mmol / kg respectively, while that of Comparative Example 1 is 1.86 mmol / kg. Therefore, compared with general DHA oil microcapsule powders, the DHA microcapsule powders of the present application have simpler formula and simpler process, and have good comparability in product indexes, good dispersing performance and sensory state, low peroxide value and surface oil rate, embedding rate as high as more than 99.8%, good smell and stability, good storage resistance, shelf life of up to 24 months, and can fully meet the special application requirements of the food industry.

[0133] The above has described various embodiments of the present application, and the above description is exemplary, not exhaustive, and is not limited to the disclosed embodiments. Many modifications and changes are obvious to those skilled in the art without departing from the scope and spirit of the described embodiments. The selection of terms used herein is intended to best explain the principles of the embodiments, practical application or improvement of technology in the market, or to enable other ordinary skilled persons in the art to understand the embodiments disclosed herein.

Claims

1. A DHA microcapsule powder, characterized in that, Comprise the following components by mass percentage: DHA oil 25-50%, edible protein 20%-40%, small molecule filler 5-25%, edible colloid 2-10%, emulsifier 0.5-8%, and antioxidant 0.1-5%; The edible protein, the small molecule filler, and the edible colloid are microcapsule wall materials in the DHA microcapsule powder, and the edible protein is an enzyme-modified edible protein obtained by a deamidation reaction using a protein glutamine enzyme. The edible colloid is curdlan.

2. The DHA microcapsule powder according to claim 1, characterized in that, The edible protein includes at least one of whey protein, sodium caseinate, soybean protein, pea protein, or walnut protein.

3. The DHA microcapsule powder according to claim 1, characterized in that, The small molecule filler includes at least one of trehalose, pullulan, soybean polysaccharide, lactose, maltose, glucose, fructose, cluster dextrin, glucose syrup, or corn syrup.

4. The DHA microcapsule powder according to claim 1, characterized in that, The emulsifier includes at least one of polyglyceryl ricinoleate, glyceryl caprylate, polyglyceryl-10-myristate, decaglyceryl monostearate, decaglyceryl pentaoleate, pentaerythritol trioleate, polyoxyethylene sorbitol monolaurate, or sodium stearoyl lactylate.

5. The DHA microcapsule powder according to any one of claims 1 to 4, characterized in that, The antioxidant includes an oil-phase antioxidant and a water-phase antioxidant.

6. The DHA microcapsule powder according to claim 5, characterized in that, The oil-phase antioxidant includes at least one of γ-glutamic acid, bamboo leaf antioxidant, licorice antioxidant, rosemary, or gallic propionic acid ester.

7. The DHA microcapsule powder according to claim 5, characterized in that, The water-phase antioxidant includes at least one of tea polyphenol, sodium ascorbate, ascorbic acid, lactic acid, malic acid, tannic acid, or citric acid and salts thereof.

8. A process for the preparation of a DHA microcapsule powder for the preparation of a DHA microcapsule powder according to any one of claims 1 to 7, characterized in that, Comprise the following preparation steps: Put the edible protein into water, add a protein glutamine enzyme, control the ratio of the protein glutamine enzyme to the substrate to be 3-20 u / g, inactivate after the reaction, cool, and obtain an enzyme-modified edible protein; Add the small molecule filler, the edible colloid, and the emulsifier to the enzyme-modified edible protein, heat under a preset condition and stir to obtain an aqueous phase liquid; Mix the DHA oil and the oil-phase antioxidant in the antioxidant to obtain an oil-phase liquid; Mix the oil-phase liquid and the aqueous phase liquid, add the water-phase antioxidant in the antioxidant, and shear to obtain an emulsion; Homogenize the emulsion twice under a preset homogenization condition, and sterilize; After sterilization, spray dry the emulsion to obtain a DHA microcapsule powder; and when spray drying, the inlet air temperature is 170-190°C, and the outlet air temperature is 80-100°C.

9. The production method according to claim 8, characterized by, The preset homogenization condition includes: The first homogenization pressure is 20-30 MPa, and the second homogenization pressure is 30-40 MPa.

Citation Information

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