A preparation method of polysaccharide-deamidated wheat protein high internal phase emulsion gel

Abstract

The present invention discloses a preparation method of a polysaccharide-deamidated wheat protein high internal phase emulsion gel, comprising the steps of preparing a polysaccharide-deamidated wheat protein solution, preparing a high internal phase Pickering emulsion, and an emulsion gel. This application uses deamidated wheat protein as a raw material, which has excellent interfacial properties after modification, and can interact with polysaccharides and vegetable oils under its structural advantages. Only by high-speed shearing and acid-heat induction methods, the cumbersome operation of a high-pressure homogenizer is avoided, thereby reducing the preparation cost of the Pickering emulsion and the emulsion gel; the oil phase volume fraction in the Pickering emulsion and the emulsion gel is greater than 75%, which can embed more fat-soluble active ingredients than the lower oil phase volume fraction in the traditional Pickering emulsion.

Description

Technical Field

[0001] The present invention relates to the field of food protein processing, and in particular to a method for preparing a polysaccharide-deamidated wheat protein high internal phase emulsion gel. Background Art

[0002] A Pickering emulsion with a high internal phase is generally defined as an emulsion with an internal phase volume fraction exceeding 74%. These emulsions are stable emulsions formed by solid particles stabilizing the interfacial layer. Food-grade Pickering emulsions are a novel type of emulsion that utilizes natural food macromolecule solid particles instead of traditional surfactants. Due to their excellent biocompatibility, they have broad application prospects in food applications such as active substance carrier transport and fat replacement. They offer advantages such as high stability, low production costs, and environmental friendliness. Currently, the natural food-grade particles used to prepare Pickering emulsions primarily include polysaccharides and proteins. The combination of polysaccharides and proteins can enhance the stability of food emulsions and gels, creating a more stable interfacial structure than simple polysaccharides and proteins. Furthermore, emulsion gels are based on emulsions and, with the aid of certain induction mechanisms, form a continuous phase that forms a spatial network structure, which is then filled with a dispersed phase. This involves encapsulating the dispersed phase within the continuous phase, forming a gel-like solid or semi-solid structure with strong water-holding and swelling capacity. Generally speaking, the preparation of emulsion gels can be divided into two steps: first, the preparation of the emulsion; second, the gelation of the continuous phase of the emulsion through a series of induction methods, thereby obtaining an emulsion gel. Common induction methods include heat induction, acid induction, salt induction, enzyme induction, and chemical crosslinking agent induction. Furthermore, the preparation of acid-induced emulsion gels typically requires heating the emulsion or the emulsion-acid mixture for a period of time after emulsification to increase gel stiffness, impart better textural and sensory properties, and more effectively prevent oxidative fission. Numerous protein-polysaccharide systems have been used to prepare emulsion gels, and protein-polysaccharide interactions have a significant impact on many aspects of complex food formulations, such as food integrity and interfacial properties. When polysaccharides adsorb at the interface, the mechanical strength and steric repulsion of the protein-coated oil droplet interface layer are enhanced, contributing to improved emulsion stability. Therefore, the synergistic acid-heat induction of high-internal-phase Pickering emulsions based on polysaccharide-deamidated wheat protein is an effective approach for preparing emulsion gels and improving their stability.

[0003] The preparation of emulsion gel in the prior art has the problems of complex operation, high equipment cost and low fat-soluble active ingredients in the obtained product. Summary of the Invention

[0004] Based on this, in order to solve the problems of complex operation, high equipment cost and low fat-soluble active ingredients in the preparation of emulsion gels in the prior art, the present invention provides an emulsion gel based on polysaccharide-deamidated wheat protein. The specific technical solution is as follows:

[0005] A method for preparing a polysaccharide-deamidated wheat protein emulsion gel, the method comprising the following steps:

[0006] Mixing deamidated wheat protein and water in a certain proportion, and stirring magnetically until the deamidated modified wheat protein is completely dispersed and dissolved to obtain a protein solution;

[0007] The polysaccharide and water are mixed in a certain proportion, and treated in a water bath under certain temperature conditions for 10 minutes to obtain a polysaccharide solution after being fully dissolved;

[0008] The protein solution and the polysaccharide solution were placed on a vortex shaker and mixed evenly, the pH was adjusted, and the mixture was stirred for 3 to 15 minutes to obtain a polysaccharide-deamidated wheat protein solution;

[0009] The polysaccharide-deamidated wheat protein solution and the vegetable oil are mixed according to a volume ratio, and high-speed shearing is performed for 1.5 minutes to 5 minutes using a high-speed shearing machine to obtain a high internal phase Pickering emulsion;

[0010] The high internal phase Pickering emulsion was heated in a water bath for 30 to 75 minutes, taken out and immediately cooled to room temperature in an ice water bath to obtain an emulsion gel.

[0011] Furthermore, the invention comprises the following ingredients in percentage by mass: 10% to 25% of deamidated wheat protein, 1% to 12% of polysaccharide and 75% to 81% of vegetable oil.

[0012] Furthermore, the polysaccharide is one or more of xanthan gum, gum arabic, carrageenan, carboxymethyl chitosan, and chitosan.

[0013] Furthermore, the vegetable oil is one or more of corn oil, soybean oil, vegetable blended oil, olive oil, linseed oil, tea oil, and coix seed oil.

[0014] Furthermore, the concentration of the protein solution is 25 mg / mL to 50 mg / mL.

[0015] Furthermore, after the polysaccharide-deamidated wheat protein solution is mixed with vegetable oil, a mixed component is obtained in which the oil phase accounts for 75% to 79% of the total volume.

[0016] Furthermore, the pH value is adjusted to 4-8.

[0017] Furthermore, one or more of citric acid, acetic acid, hydrochloric acid, malic acid or phosphoric acid is used to adjust the pH.

[0018] Furthermore, the volume fraction of the oil phase in the emulsion gel is greater than 75%.

[0019] In the above scheme, deamidated wheat protein is used as a raw material, and after surface modification, it has excellent interfacial properties. Due to its structural advantages, it can interact with polysaccharides and vegetable oils. Only high-speed shearing and simple heating methods are used, avoiding the tedious operation of using a high-pressure homogenizer, thereby reducing the preparation cost of Pickering emulsions and emulsion gels. The oil phase volume fraction in the Pickering emulsions and emulsion gels is greater than 75%, which can embed more fat-soluble active ingredients compared to the lower oil phase volume fraction in traditional Pickering emulsions. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 Picture a in the picture is a picture of whipped animal cream decoration; Figure 1 Figure b is a high internal phase Pickering emulsion decoration diagram of Example 2; Figure 1 Figure c is a decoration picture of the emulsion after centrifugation; Figure 1 Figure d is a schematic diagram of the state of Figure a after being placed at room temperature for 3 hours; Figure 1 Figure e is a schematic diagram of the state of Figure b after being placed at room temperature for 3 hours; Figure 1 Figure f is a schematic diagram of the state of Figure c after being placed at room temperature for 3 hours.

[0021] Figure 2 This is a schematic diagram of the emulsion gel obtained in Example 3 of the present application. DETAILED DESCRIPTION

[0022] In order to make the purpose, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with its embodiments. It should be understood that the specific embodiments described herein are only used to explain the present invention and do not limit the scope of protection of the present invention.

[0023] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by those skilled in the art to which this invention pertains. The terms used herein in the specification of the present invention are for the purpose of describing specific embodiments only and are not intended to limit the present invention. The term "and / or" as used herein includes any and all combinations of one or more of the associated listed items.

[0024] A method for preparing a polysaccharide-deamidated wheat protein emulsion gel in one embodiment of the present invention comprises the following steps:

[0025] Mixing deamidated wheat protein and water in a certain proportion, and stirring magnetically until the deamidated modified wheat protein is completely dispersed and dissolved to obtain a protein solution;

[0026] The polysaccharide and water are mixed in a certain proportion, and treated in a water bath under certain temperature conditions for 10 minutes to obtain a polysaccharide solution after being fully dissolved;

[0027] The protein solution and the polysaccharide solution were placed on a vortex shaker and mixed evenly, the pH was adjusted, and the mixture was stirred for 3 minutes to 15 minutes to obtain a polysaccharide-deamidated wheat protein solution;

[0028] The polysaccharide-deamidated wheat protein solution and the vegetable oil are mixed according to a volume ratio, and high-speed shearing is performed for 1.5 minutes to 5 minutes using a high-speed shearing machine to obtain a high internal phase Pickering emulsion;

[0029] The high internal phase Pickering emulsion was heated in a water bath for 30 to 75 minutes, taken out and immediately cooled to room temperature in an ice water bath to obtain an emulsion gel.

[0030] In one embodiment, the invention comprises the following ingredients in percentage by mass: 10% to 25% deamidated wheat protein, 1% to 12% polysaccharide and 75% to 81% vegetable oil.

[0031] In one embodiment, the polysaccharide is one or more of xanthan gum, gum arabic, carrageenan, carboxymethyl chitosan, and chitosan.

[0032] In one embodiment, the vegetable oil is one or more of corn oil, soybean oil, vegetable blend oil, olive oil, linseed oil, tea oil, and coix seed oil.

[0033] In one embodiment, the concentration of the protein solution is 25 mg / mL to 50 mg / mL.

[0034] In one embodiment, the polysaccharide-deamidated wheat protein solution is mixed with vegetable oil to obtain a mixed component in which the oil phase accounts for 75% to 79% of the total volume.

[0035] In one embodiment, the pH value is adjusted to 4-8.

[0036] In one embodiment, the pH is adjusted using one or more of citric acid, acetic acid, hydrochloric acid, malic acid or phosphoric acid.

[0037] In one embodiment, the volume fraction of the oil phase in the emulsion gel is greater than 75%.

[0038] In one embodiment, the preparation method of the deamidated wheat protein is:

[0039] Add citric acid, glucose, betaine, and water to a serum bottle in a volume ratio of 1:3:3:6, place the bottle in an 85°C water bath until all solid particles are dissolved to obtain a natural low eutectic solvent, then dilute the natural low eutectic solvent with distilled water, slowly add gluten, and use a magnetic stirrer to stir during the addition. Continue stirring for 1 hour after the gluten is added; after stirring, place the bottle in a water bath shaker at 35°C for 12 hours, and then place the bottle in a high-pressure vertical sterilizer for heat treatment at 121°C for 10 minutes; immediately place the bottle in ice water for cooling after treatment, pour the bottle into a centrifuge tube and balance it, place the bottle in a centrifuge and centrifuge at 9990r / min and 4°C for 10 minutes, collect the supernatant into a container and place it in a -80°C refrigerator for pre-freezing, freeze it into a solid, and then place it in a freeze dryer for freeze-drying for 3 to 5 days to obtain deamidated wheat protein.

[0040] In the above scheme, deamidated wheat protein is used as a raw material, and after surface modification, it has excellent interfacial properties. Due to its structural advantages, it can interact with polysaccharides and vegetable oils. Only high-speed shearing and simple heating methods are used, avoiding the tedious operation of using a high-pressure homogenizer, thereby reducing the preparation cost of Pickering emulsions and emulsion gels. The oil phase volume fraction in the Pickering emulsions and emulsion gels is greater than 75%, which can embed more fat-soluble active ingredients compared to the lower oil phase volume fraction in traditional Pickering emulsions.

[0041] The embodiments of the present invention will be described in detail below with reference to specific examples.

[0042] Example 1:

[0043] Preparation of deamidated wheat protein:

[0044] Add citric acid, glucose, betaine, and water to a serum bottle in a volume ratio of 1:3:3:6, place the bottle in an 85°C water bath until all solid particles are dissolved to obtain a natural low eutectic solvent, then dilute the natural low eutectic solvent with distilled water, slowly add gluten, and use a magnetic stirrer to stir during the addition. Continue stirring for 1 hour after the gluten is added; after stirring, place the bottle in a water bath shaker at 35°C for 12 hours, and then place the bottle in a high-pressure vertical sterilizer for heat treatment at 121°C for 10 minutes; immediately place the bottle in ice water for cooling after treatment, pour the bottle into a centrifuge tube and balance it, place the bottle in a centrifuge and centrifuge at 9990r / min and 4°C for 10 minutes, collect the supernatant into a container and place it in a -80°C refrigerator for pre-freezing, freeze it into a solid, and then place it in a freeze dryer for freeze-drying for 3 to 5 days to obtain deamidated wheat protein.

[0045] Example 2:

[0046] Preparation of high internal phase Pickering emulsion of carrageenan-deamidated wheat protein:

[0047] 0.35 g of freeze-dried deamidated wheat protein sample was dissolved in 10 mL of distilled water to prepare a protein solution with a concentration of 35 mg / mL; 0.1 g of carrageenan was dissolved in 10 mL of distilled water, and then 3.75 mL of corn oil and 0.25 mL of carrageenan solution were added to a serum bottle, mixed evenly using a vortex oscillator, and then 1.00 mL of protein solution was added. The mixture was sheared at a speed of 19000 r / min using a high-speed shearing machine to obtain a high internal phase Pickering emulsion.

[0048] Example 3:

[0049] Preparation of carrageenan-deamidated wheat protein emulsion gel:

[0050] The high internal phase Pickering emulsion of Example 2 was placed in an 80° C. water bath and heated for 75 min. After being taken out, it was cooled to room temperature in an ice water bath. The freshly prepared carrageenan-deamidated wheat protein high internal phase emulsion gel was stored in a refrigerator at 4° C. for later use.

[0051] The textures of the emulsion gel and cream from Example 3 were compared using the following texture analyzer parameters: pre-test speed of 1 mm / s, test speed of 1 mm / s, post-test speed of 1 mm / s, trigger force of 10 g, compression distance of 10 mm, duration of 5 seconds, and probe type P / 0.5. The gels were compared for hardness, brittleness, viscosity, elasticity, chewiness, stickiness, cohesiveness, and resilience. The measurements were repeated three times, and the average value was calculated. The results are shown in Table 1 below.

[0052] Table 1:

[0053]

[0054] Analysis of the data in Table 1 demonstrates that, after heating, the high internal phase Pickering emulsion of this application exhibits properties similar to those of butter, making it a promising alternative to vegetable butter, while also utilizing a safe raw material source. The oil phase volume fraction in the Pickering emulsion and emulsion gel is >75%, allowing for the encapsulation of more fat-soluble active ingredients compared to the lower oil phase volume fraction in traditional Pickering emulsions.

[0055] in addition, Figure 1 Picture a in the picture is a picture of whipped animal cream decoration; Figure 1 Figure b is a high internal phase Pickering emulsion decoration diagram of Example 2; Figure 1 Figure c is a decoration picture of the emulsion after centrifugation; Figure 1 Figure d is a schematic diagram of the state of Figure a after being placed at room temperature for 3 hours; Figure 1 Figure e is a schematic diagram of the state of Figure b after being placed at room temperature for 3 hours; Figure 1Figure f is a schematic diagram of the state of Figure c after being placed at room temperature for 3 hours. As can be seen from the figure, the emulsion gel prepared in this application has higher stability and higher practicality. Figure 2 This is a schematic diagram of the emulsion gel obtained in Example 3 of the present application, Figure 2 It can be seen from the results that the emulsion gel of the present application also has high stability and excellent applicability.

[0056] The technical features of the above-mentioned embodiments can be combined arbitrarily. In order to make the description concise, not all possible combinations of the technical features in the above-mentioned embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0057] The above-described embodiments merely illustrate several implementations of the present invention, and while their descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the patent. It should be noted that a person skilled in the art would be able to make numerous variations and improvements without departing from the spirit of the present invention, all of which fall within the scope of protection of the present invention. Therefore, the scope of protection of the patent for this invention shall be determined by the appended claims.

Claims

1. A method for preparing a polysaccharide-deamidated wheat protein high internal phase emulsion gel, characterized in that: The preparation method comprises the following steps: Add citric acid, glucose, betaine, and water to a serum bottle in a volume ratio of 1:3:3:6, place it in an 85°C water bath until all the solid particles are dissolved to obtain a natural low eutectic solvent, then dilute the natural low eutectic solvent with distilled water, slowly add gluten, and use a magnetic stirrer to stir during the addition. Continue stirring for 1 hour after the gluten is added; after stirring, place it in a water bath shaker at 35°C for 12 hours, and then place it in a high-pressure vertical sterilizer for heat treatment at 121°C for 10 minutes; immediately place it in ice water to cool after treatment, pour it into a centrifuge tube and balance it, place it in a centrifuge and centrifuge it at 9990r / min and 4°C for 10 minutes, collect the supernatant into a container and place it in a -80°C refrigerator for pre-freezing, freeze it into a solid, and then place it in a freeze dryer for freeze-drying for 3d to 5d to obtain deamidated wheat protein; Mixing deamidated wheat protein and water in a certain proportion, and stirring magnetically until the deamidated modified wheat protein is completely dispersed and dissolved to obtain a protein solution; The polysaccharide and water are mixed in a certain proportion, and treated in a water bath under certain temperature conditions for 10 minutes to obtain a polysaccharide solution after being fully dissolved; The protein solution and the polysaccharide solution were placed on a vortex shaker and mixed evenly, the pH was adjusted, and the mixture was stirred for 3 minutes to 15 minutes to obtain a polysaccharide-deamidated wheat protein solution; The polysaccharide-deamidated wheat protein solution and the vegetable oil are mixed according to a volume ratio, and high-speed shearing is performed for 1.5 minutes to 5 minutes using a high-speed shearing machine to obtain a high internal phase Pickering emulsion in which the oil phase accounts for 75% to 79% of the total volume ratio; The high internal phase Pickering emulsion is heated in a water bath for 30 to 75 minutes, and immediately cooled to room temperature in an ice water bath to obtain an emulsion gel; The composition comprises the following ingredients according to mass percentage: 10% to 25% deamidated wheat protein, 1% to 12% polysaccharide and 75% to 81% vegetable oil; The polysaccharide is one or more of xanthan gum, gum arabic, carrageenan, carboxymethyl chitosan, and chitosan; The concentration of the protein solution is 25 mg / mL to 50 mg / mL.

2. The preparation method according to claim 1, characterized in that The vegetable oil is one or more of corn oil, soybean oil, vegetable blended oil, olive oil, linseed oil, tea oil, and coix seed oil.

3. The preparation method according to claim 2, characterized in that The pH value is adjusted to 4-8.

4. The preparation method according to claim 3, characterized in that The pH is adjusted by using one or more of citric acid, acetic acid, hydrochloric acid, malic acid or phosphoric acid.

5. The preparation method according to claim 1, characterized in that The volume fraction of the oil phase in the emulsion gel is greater than 75%.

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