CN110710577A - Preparation method of high-oil-loading-capacity emulsion rich in fibrous polysaccharide - Google Patents
Preparation method of high-oil-loading-capacity emulsion rich in fibrous polysaccharide Download PDFInfo
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- CN110710577A CN110710577A CN201810764876.1A CN201810764876A CN110710577A CN 110710577 A CN110710577 A CN 110710577A CN 201810764876 A CN201810764876 A CN 201810764876A CN 110710577 A CN110710577 A CN 110710577A
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
- A23D9/02—Other edible oils or fats, e.g. shortenings, cooking oils characterised by the production or working-up
- A23D9/04—Working-up
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS, COOKING OILS
- A23D9/00—Other edible oils or fats, e.g. shortenings, cooking oils
- A23D9/007—Other edible oils or fats, e.g. shortenings, cooking oils characterised by ingredients other than fatty acid triglycerides
Abstract
The invention relates to a preparation method of a high oil-loading emulsion rich in fibrous polysaccharide, which comprises the steps of adding protein powder into distilled water, magnetically stirring at normal temperature to dissolve the protein powder and hydrating in a refrigerator at 4 ℃ to obtain a protein solution; mixing the protein solution and the fiber polysaccharide water dispersion powder, and adjusting the pH value of the system to obtain a protein/fiber compound; dispersing the oil phase in the protein/fiber complex, and emulsifying to prepare an oil-in-water emulsion. The invention takes protein and fibrous polysaccharide compound as an emulsion stabilizer, improves the wettability and stability of particles synergistically, and forms a stable three-dimensional network structure by being adsorbed on an oil-water interface together, thereby obtaining an emulsion rich in viscoelasticity and high stability; natural food-grade materials are adopted; the preparation process is simple and convenient, no surfactant is added, and the preparation method is green and safe; the content of the needed compound stabilizer is low and the emulsification stability is good; the prepared oil-in-water emulsion removes oil and water phases, can form a porous and stable network structure, and can be used as a porous polymer scaffold material in tissue engineering.
Description
Technical Field
The invention belongs to the fields of food science and technology and the like, and particularly relates to a preparation method of a high oil-loading-capacity emulsion rich in fiber polysaccharide.
Background
In recent years, the research related to structuring of edible oil and fat has attracted extensive attention of scholars at home and abroad. The liquid vegetable oil structuring system, namely the oleogel system, can be used as a substitute of hydrogenated vegetable oil and also as a functional factor delivery system or a porous polymer scaffold material, and has wide application prospects in the fields of foods, medicines and cosmetics. However, the construction of oleogels with gelators faces a series of challenges in food processing and commercial production, such as many low molecular weight gelling agents are not approved or limited for use as food additives in food, or are not good for human health, and processing conditions are restricted. The natural high molecular polymer prepared oil gel system has good development prospect, a plurality of natural high molecular polymers are allowed to be used in food, and the structural characteristics are clearly researched, but most of the natural food-grade high molecular polymers are hydrophilic and cannot be uniformly and stably dispersed in an oil phase to form a necessary gel network structure. Therefore, it is of great research value to take measures to introduce water-soluble polymers into the oil phase and form stable gel network structures.
The emulsion template method can introduce food-grade high molecular polymers into an oil phase to prepare oil gel, and is also one of the current research hotspots. The Pickering emulsion is an emulsion prepared by replacing the conventional surfactant with solid particles to stabilize an oil-water interface, and comprises oil-in-water, water-in-oil and multiple Pickering emulsions, so that the poison of the surfactant to an organism is reduced, the content of the used colloidal particles is low, the Pickering emulsion is green, environment-friendly and safe, the preparation is simple and easy, and the emulsion stability is good. The preparation of high oil loading Pickering emulsions using polymer colloidal particles to stabilize the dispersed phase is an effective means of forming oleogels. The high oil-loading Pickering emulsion prepared from the food-grade polymer can convert liquid vegetable oil into a solid or semi-solid state without any chemical change, and is green, safe, simple and easy to prepare and low in cost.
CN108064976A discloses a method for preparing polysaccharide emulsion gel by using Pickering emulsion, wherein a regenerated cellulose suspension with the mass fraction of 0.5-5% is used as a water phase, edible oil is used as an oil phase, and the edible oil/cellulose Pickering emulsion is obtained by homogenizing; wherein the mass fraction of the edible oil in the Pickering emulsion is 1-80%; adding the polysaccharide emulsion into Pickering emulsion, stirring, heating and cooling to obtain polysaccharide emulsion gel. But the preparation process is complex, the regenerated cellulose particles have no surface activity, and the prepared emulsion has poor stability.
CN107459661A discloses a novel preparation method of a food-grade high internal phase emulsion, which comprises mixing polysaccharide (pectin or sodium alginate) and protein (whey protein isolate or ovalbumin), adjusting pH, adding oil droplets into the solution until oil flowers are separated out, and forming the high internal phase emulsion. The preparation condition is mild, the operation is simple, but the content of the required polysaccharide and protein is high, the judgment method for preparing the emulsion by dripping oil drops until the oil flowers are separated out is not accurate enough, and the properties such as the particle size of the emulsion are not clear.
CN106040026A discloses a method for preparing Pickering emulsion by using TEMPO oxidized bacterial cellulose, which comprises oxidizing bacterial cellulose microfibrils at room temperature by using a TEMPO/NaBr/NaClO mixed oxidation system, centrifugally cleaning and dialyzing to obtain a TEMPO Oxidized Bacterial Cellulose (TOBC) suspension, wherein the prepared cellulose nanofiber can be used as a particle emulsifier to stabilize the Pickering emulsion, is green and safe, can be prepared into emulsion with good stability, and can easily form gelled emulsion. However, the oil phase with stable emulsification is limited and cannot be independently used for preparing the emulsion with high oil loading.
Disclosure of Invention
The invention aims to provide a simple, convenient and safe method aiming at the current situation; the raw materials are wide in source and low in cost; the prepared oil-in-water emulsion has high oil loading, is rich in fiber polysaccharide and low in heat, and can be used as a porous polymer scaffold material in a preparation method of the oil-in-water emulsion rich in fiber polysaccharide.
The invention aims to realize a preparation method of a high oil-loading-capacity oil-in-water emulsion rich in fiber polysaccharide, which comprises the following specific steps:
1) adding 1-5 g of protein powder into 100mL of distilled water, magnetically stirring at 500rpm at normal temperature for 30 minutes to dissolve uniformly, and placing in a refrigerator at 4 ℃ for hydration to obtain a protein solution;
the protein powder is as follows: one or two of soybean protein isolate powder, pea protein isolate powder, whey protein isolate powder, egg white protein powder and casein powder;
2) mixing the protein solution obtained in the step 1) with 0.15-0.4 g of aqueous dispersion powder of fiber polysaccharide, and adjusting the pH value of the system to 3-11 to prepare a uniformly mixed protein/fiber compound;
the fiber polysaccharide water dispersion powder is: plant cellulose powder, fungal cellulose powder or bacterial cellulose powder;
3) dispersing 100-400 mL of oil phase in the protein/fiber compound prepared in the step 2), and emulsifying to prepare an oil-in-water emulsion with high oil loading;
the oil phase is liquid edible oil, specifically soybean oil, peanut oil, corn oil, rapeseed oil or olive oil;
the method for preparing the emulsion by emulsification comprises the following steps: high speed shearing method, ultrasonic emulsification method, high pressure homogenization method or high pressure micro-jet method.
The water-soluble protein and the fibrous polysaccharide colloidal particles are blended and combined to form a protein/fiber compound, and the protein/fiber compound is added into an oil phase for emulsification to prepare the oil-in-water emulsion with high oil loading
The invention has the following advantages:
1. based on the good emulsification property of the protein and polysaccharide compound and the capability of stabilizing a high oil phase, the fiber polysaccharide colloidal particles are used for modifying protein, and are cooperated with protein particles to adsorb an oil-water interface, and the formation of an interface film with a compact network structure is promoted, so that the obtained emulsion has strong emulsibility and better viscoelasticity;
2. the prepared emulsion is rich in fibrous polysaccharide, low in or even free of trans-fatty acid, low in calorie, green, safe and free of toxic and side effects; the oil carrying capacity can reach about 80 percent, and the liquid vegetable oil can be converted into a solid or semi-solid gel-like form without any chemical change, so that the oil is green and safe;
3. the dosage of the emulsion stabilizer is small, the cost is saved, the preparation method is rapid, convenient and fast, and the method is economic and safe.
4. The preparation process is simple and convenient, no surfactant is added, and the preparation method is green and safe; the content of the needed compound stabilizer is low and the emulsification stability is good; the prepared oil-in-water emulsion removes oil and water phases, can form a porous and stable network structure, and can be used as a porous polymer scaffold material in tissue engineering.
5. The invention provides a new way for developing and researching novel functional food-grade stable Pickering emulsion with solid particles, and also provides a new idea for structuring liquid grease and researching and developing porous polymer bracket materials.
Drawings
FIG. 1 is a state diagram of a Pickering emulsion prepared in example 5,
FIG. 2 is a state diagram of a Pickering emulsion prepared in example 10,
FIG. 3 is a state diagram of a Pickering emulsion prepared in example 12,
FIG. 4 is a gel state diagram of a Pickering emulsion prepared in example 15,
FIG. 5 is a gel state diagram of a Pickering emulsion prepared in example 26.
Detailed Description
The invention takes protein powder to add into distilled water, magnetic stirring is carried out for 30 minutes under the rotation speed of 500rpm at normal temperature for uniform dissolution, and the protein solution is prepared by placing in a refrigerator for hydration at 4 ℃.
The protein powder is as follows: soy protein isolate, pea protein isolate, whey protein isolate, egg white protein or casein.
Weighing 1-5 g of soybean protein isolate powder, preferably 3 g. Added to 100mL of distilled water. Pea protein isolate powder 5g was weighed and added to 100mL of distilled water. Whey protein isolate powder 5g was weighed and added to 100mL of distilled water. 5g of egg white protein powder is weighed and added into 100mL of distilled water. Casein powder (1 g) was weighed and added to 100mL of distilled water.
Mixing the protein solution and the fiber polysaccharide water dispersion powder, and adjusting the pH value of the system to 2-4, 5-11, preferably 3; obtaining the protein/fiber compound.
Mixing the protein solution with 0.15-0.4 g of aqueous dispersion powder of fibrous polysaccharide; preferably, the protein solution is mixed with 0.24g of aqueous dispersion powder of the fibrous polysaccharide.
The plant cellulose powder, the fungus cellulose powder or the bacteria cellulose powder are respectively as follows: microcrystalline cellulose powder prepared from pure wood pulp, cellulose nanocrystalline powder prepared from needle mushroom, and bacterial cellulose nanopowder oxidized by TEMPO; the carboxyl content in the TEMPO oxidized bacterial cellulose nanopowder was 0.6 mmol/g.
For different proteins, the pH value of the adjusting system is different, the used proteins are pea protein isolate, whey protein isolate, egg albumin and casein, and the pH value is adjusted to be 7; the protein is soybean protein isolate, and the pH value is adjusted to 3-11; the pH is preferably adjusted to 3.
Dispersing 100-400 mL of oil phase in the protein/fiber compound, and emulsifying to prepare the oil-in-water emulsion.
The oil phase is liquid edible oil, specifically soybean oil, peanut oil, corn oil, rapeseed oil or olive oil. Preferred is soybean oil or rapeseed oil.
The method for preparing the emulsion by emulsification comprises the following steps: high speed shearing method, high pressure homogenizing method or ultrasonic emulsifying method.
The conditions for using high speed shearing are: rotating at 5000-12000 rpm for 5-30 min; preferably 12000rpm, and 20 minutes of shearing.
The ultrasonic emulsification method adopts a cell disruption instrument, and the conditions are as follows: carrying out ultrasonic treatment at 20kHz for 5-30 minutes under the power of 600 w; preferably, the ultrasonic treatment is carried out at a power of 600w and a frequency of 20kHz for 15 minutes.
The conditions of the high-pressure homogenization method are as follows: treating for 1-10 times under the pressure of 40-100 MPa; preferably, the treatment is carried out for 5 times under the power of 60 MPa.
The conditions of the high-pressure micro-jet method are as follows: treating for 1-10 times under the pressure of 40-80 MPa; preferably, the treatment is carried out for 5 times under the power of 50 MPa.
The present invention is described in detail below with reference to specific examples.
Example 1, 1g of casein powder was weighed, added to 100mL of distilled water, and dissolved uniformly by magnetic stirring at 500rpm at room temperature for 30 minutes, and then left to stand at 4 ℃ for hydration in a refrigerator to obtain a protein solution. The resulting protein solution was mixed with microcrystalline cellulose powder prepared from 0.2g of pure wood pulp, and the pH was adjusted to 7 to obtain a well-mixed protein/fiber complex. 100mL of soybean oil was dispersed in the prepared protein/fiber complex, and shear-dispersed in a high-speed shear at a shear revolution of 5000rpm for 30 minutes to prepare an oil-in-water Pickering emulsion.
The emulsion sample prepared by the embodiment has the advantages that an oil layer is separated out on the surface, the particle size is large and is not uniformly distributed, obvious layering occurs after standing for 24 hours, and the emulsion is easy to flow.
Example 2, 3g of ovalbumin powder was weighed, added to 100mL of distilled water, and dissolved uniformly by magnetic stirring at 500rpm at normal temperature for 30 minutes, and then placed in a refrigerator at 4 ℃ to hydrate to obtain a protein solution. The resulting protein solution was mixed with microcrystalline cellulose powder prepared from 0.15g of pure wood pulp, and the pH was adjusted to 7 to obtain a well-mixed protein/fiber complex. 100mL of soybean oil was dispersed in the prepared protein/fiber complex, and shear-dispersed in a high-speed shear at 10000rpm for 20 minutes to prepare an oil-in-water Pickering emulsion.
The emulsion prepared by the embodiment has the advantages that oil flowers are separated out on the surface, the particle size distribution is uneven, obvious layering occurs after standing for 24 hours, and the emulsion is easy to flow.
Example 3 whey protein isolate powder 5g was weighed and added to 100mL of distilled water, and the mixture was dissolved uniformly by magnetic stirring at 500rpm at room temperature for 30 minutes, and then was allowed to stand at 4 ℃ for hydration in a refrigerator to obtain a protein solution. The resulting protein solution was mixed with microcrystalline cellulose powder prepared from 0.25g of pure wood pulp, and the pH was adjusted to 7 to obtain a well-mixed protein/fiber complex. 100mL of soybean oil was dispersed in the prepared protein/fiber complex, and shear-dispersed in a high-speed shear at 12000rpm for 20 minutes to prepare an oil-in-water Pickering emulsion.
The emulsion sample prepared by the embodiment has no oil precipitation, the emulsion has large particle size and uneven distribution, obvious layering occurs after standing for 24 hours, and the emulsion is easy to flow.
Example 4, 5g of pea protein isolate powder was weighed, added to 100mL of distilled water, dissolved uniformly by magnetic stirring for 30 minutes at a normal temperature at 500rpm, and left to hydrate in a refrigerator at 4 ℃ to obtain a protein solution. The resulting protein solution was mixed with microcrystalline cellulose powder prepared from 0.25g of pure wood pulp, and the pH was adjusted to 7 to obtain a well-mixed protein/fiber complex. 100mL of soybean oil was dispersed in the prepared protein/fiber complex, and shear-dispersed in a high-speed shear at 20000rpm for 5 minutes to prepare an oil-in-water Pickering emulsion.
The emulsion sample prepared in the embodiment has no oil precipitation, the emulsion has large particle size and uneven distribution, no layering phenomenon exists after standing for 24 hours, but a micro layering phenomenon exists after standing for 14 days, and the emulsion is not easy to flow.
Example 5, 5g of isolated soy protein powder was weighed, added to 100mL of distilled water, dissolved uniformly by magnetic stirring at 500rpm at room temperature for 30 minutes, and allowed to stand at 4 ℃ for hydration in a refrigerator to obtain a protein solution. The resulting protein solution was mixed with microcrystalline cellulose powder prepared from 0.25g of pure wood pulp, and the pH was adjusted to 7 to obtain a well-mixed protein/fiber complex. 100mL of soybean oil was dispersed in the prepared protein/fiber complex, and shear-dispersed in a high-speed shear at 12000rpm for 20 minutes to prepare an oil-in-water Pickering emulsion in the state shown in FIG. 1.
The emulsion prepared by the embodiment has no oil flower precipitation on the surface, small particle size and uniform distribution, does not have the layering phenomenon after standing for 14 days, and does not flow in a gel-like state.
The results of the analysis examples 1 to 5 show that compared with other water-soluble proteins, the protein/polysaccharide complex formed by the soy protein isolate and the fibrous polysaccharide has stronger emulsification stability, smaller and uniformly distributed particle size of the emulsion with synergistic stability, the condition of phase separation of the emulsion is slower, and the viscosity of the emulsion system is enhanced and is not easy to flow.
Example 6, 3g of soy protein isolate powder was weighed, added to 100mL of distilled water, dissolved uniformly by magnetic stirring at 500rpm at room temperature for 30 minutes, and allowed to stand at 4 ℃ for hydration in a refrigerator to obtain a protein solution. Mixing the obtained protein solution with cellulose nanocrystalline powder prepared from 0.4g of pure wood pulp, and adjusting the pH value to 7 to obtain a uniformly mixed protein/fiber compound. 150mL of peanut oil was dispersed in the prepared protein/fiber complex and dispersed for 20 minutes with shear in a high speed shear at 12000rpm to prepare an oil-in-water Pickering emulsion.
A small amount of oil layer is separated out on the surface of the emulsion prepared by the embodiment, the emulsion is obviously layered after being placed for 24 hours, and the emulsion is easy to flow.
Example 7, 3g of soy protein isolate powder was weighed, added to 100mL of distilled water, dissolved uniformly by magnetic stirring at 500rpm at room temperature for 30 minutes, and allowed to stand at 4 ℃ for hydration in a refrigerator to obtain a protein solution. Mixing the obtained protein solution with cellulose nano-fiber powder prepared from 0.4g of pure wood pulp, adjusting the pH value to 7, and preparing a uniformly mixed protein/fiber compound. 150mL of peanut oil was dispersed in the prepared protein/fiber complex and dispersed for 20 minutes with shear in a high speed shear at 12000rpm to prepare an oil-in-water Pickering emulsion.
The emulsion prepared by the embodiment has no oil flower precipitation on the surface, obvious layering after being placed for 24 hours, and easy flowing of the emulsion.
Example 8, 3g of soy protein isolate powder was weighed, added to 100mL of distilled water, dissolved uniformly by magnetic stirring at 500rpm at room temperature for 30 minutes, and allowed to stand at 4 ℃ for hydration in a refrigerator to obtain a protein solution. Mixing the obtained protein solution with 0.4g of cellulose nanocrystalline powder prepared from needle mushroom, adjusting the pH value to 7, and preparing a uniformly mixed protein/fiber compound. 150mL of peanut oil was dispersed in the prepared protein/fiber complex and dispersed for 20 minutes with shear in a high speed shear at 12000rpm to prepare an oil-in-water Pickering emulsion.
The emulsion prepared in the embodiment is milky white, has no oil layer separated out, is obviously layered after being placed for 24 hours, and is easy to flow.
Example 9, 3g of soy protein isolate powder was weighed, added to 100mL of distilled water, dissolved uniformly by magnetic stirring at 500rpm at room temperature for 30 minutes, and allowed to stand at 4 ℃ for hydration in a refrigerator to obtain a protein solution. Mixing the obtained protein solution with 0.4g of cellulose nanofiber powder prepared from needle mushroom, adjusting the pH value to 7, and preparing a uniformly mixed protein/fiber compound. 150mL of peanut oil was dispersed in the prepared protein/fiber complex and dispersed for 20 minutes with shear in a high speed shear at 12000rpm to prepare an oil-in-water Pickering emulsion.
The emulsion prepared by the embodiment is milky white and has no oil layer precipitation, the particle size distribution of the emulsion is not uniform, no obvious layering phenomenon exists after the emulsion is placed for 14 days, and the emulsion has certain fluidity.
Example 10, 5g of soy protein isolate powder was weighed, added to 100mL of distilled water, dissolved uniformly by magnetic stirring at 500rpm at room temperature for 30 minutes, and allowed to stand at 4 ℃ for hydration in a refrigerator to obtain a protein solution. Mixing the obtained protein solution with 0.4g of TEMPO oxidized bacterial cellulose nano powder (the carboxyl content is 0.6mmol/g), adjusting the pH value to 7, and preparing a uniformly mixed protein/fiber compound. 150mL of peanut oil was dispersed in the prepared protein/fiber complex, and shear-dispersed in a high-speed shear at 12000rpm for 20 minutes to prepare an oil-in-water Pickering emulsion in the state shown in FIG. 2.
The emulsion prepared by the embodiment has no oil flower precipitation, small particle size and uniform distribution, no layering phenomenon after being placed for 14 days, and no flowing of the emulsion in gel-like state.
The results of the analysis examples 6 to 10 show that compared with other fibrous polysaccharides, the emulsion prepared by mixing the isolated soy protein with the TEMPO oxidized bacterial cellulose nanofibers (the carboxyl content is 0.6mmol/g) has uniform particle size distribution, no oil flowers are separated out on the surface, and no delamination phenomenon exists after the emulsion is placed for 14 days; the TEMPO oxidized bacterial cellulose nanofiber has small size, good dispersion stability and high surface charge density, can be effectively adsorbed on an oil-water interface in a synergistic way with protein particles to form a stable three-dimensional network structure system, the thickness of an interface film and the viscoelasticity of the whole emulsion are enhanced, and the prepared emulsion is in a gel-like state.
Example 11, 2g of soy protein isolate powder and 1g of pea protein isolate were weighed, added to 100mL of distilled water, magnetically stirred at 500rpm at room temperature for 30 minutes to dissolve them uniformly, and left to stand at 4 ℃ for hydration in a refrigerator to obtain a protein solution. Mixing the obtained protein solution with 0.24g of TEMPO oxidized bacterial cellulose nano powder (the carboxyl content is 0.6mmol/g), adjusting the pH value to 3, and preparing a uniformly mixed protein/fiber compound. 200mL of corn oil was dispersed in the prepared protein/fiber complex and dispersed by shearing in a high speed shear at 12000rpm for 20 minutes to prepare an oil-in-water Pickering emulsion.
The emulsion prepared by the embodiment has no oil flower on the surface, has no layering phenomenon after being placed for 14 days, and does not flow in a gel-like state.
Example 12, 2g of the isolated soy protein powder and 1g of the isolated whey protein powder were weighed and added to 100mL of distilled water, and the mixture was dissolved uniformly by magnetic stirring at 500rpm at room temperature for 30 minutes, and then was left to stand at 4 ℃ for hydration in a refrigerator to obtain a protein solution. Mixing the obtained protein solution with 0.24g of TEMPO oxidized bacterial cellulose nano powder (the carboxyl content is 0.6mmol/g), adjusting the pH value to 7, and preparing a uniformly mixed protein/fiber compound. 200mL of corn oil was dispersed in the prepared protein/fiber complex, and shear-dispersed in a high-speed shearer at a shear revolution of 12000rpm for 20 minutes to prepare an oil-in-water Pickering emulsion in a state shown in FIG. 3.
The emulsion prepared by the embodiment has no oil flower precipitation on the surface, uniform particle size distribution, no layering phenomenon after the emulsion is placed for 14 days, high viscosity and difficulty in flowing.
Example 13, 2g of soy protein isolate powder and 1g of ovalbumin powder were weighed, added to 100mL of distilled water, and dissolved uniformly by magnetic stirring at 500rpm for 30 minutes at room temperature, and then left to hydrate in a refrigerator at 4 ℃ to obtain a protein solution. Mixing the obtained protein solution with 0.24g of TEMPO oxidized bacterial cellulose nano powder (the carboxyl content is 0.6mmol/g), and adjusting the pH value to 11 to obtain a uniformly mixed protein/fiber compound. 200mL of corn oil was dispersed in the prepared protein/fiber complex and dispersed by shearing in a high speed shear at 12000rpm for 20 minutes to prepare an oil-in-water Pickering emulsion.
The emulsion prepared by the embodiment has obvious oil layer precipitation on the surface, large emulsion particle size and uneven distribution, obvious layering phenomenon occurs after standing for 24 hours, and the emulsion is not easy to flow.
Example 14, 2g of isolated soy protein powder and 1g of casein powder were weighed, added to 100mL of distilled water, and dissolved uniformly by magnetic stirring at 500rpm for 30 minutes at room temperature, and then left to stand at 4 ℃ for hydration in a refrigerator to obtain a protein solution. Mixing the obtained protein solution with 0.24g of TEMPO oxidized bacterial cellulose nano powder (the carboxyl content is 0.6mmol/g), adjusting the pH value to 7, and preparing a uniformly mixed protein/fiber compound. 200mL of corn oil was dispersed in the prepared protein/fiber complex and dispersed by shearing in a high speed shear at 12000rpm for 20 minutes to prepare an oil-in-water Pickering emulsion.
The emulsion prepared by the embodiment has no oil flower on the surface, no layering phenomenon exists after the emulsion is placed for 14 days, and the emulsion is not easy to flow.
The results of the analysis examples 11 to 14 show that when the pH value of the protein/fiber composite suspension is adjusted to 3, the pH value is lower than the isoelectric point of protein, the protein surface is positively charged, and the protein and the negatively charged cellulose are easy to generate electrostatic adsorption to form a net-shaped composite structure with good stability, the prepared emulsion has better physical stability and viscoelasticity, and the emulsion is in a gel-like state and does not flow.
Example 15, 3g of soy protein isolate powder was weighed, added to 100mL of distilled water, dissolved uniformly by magnetic stirring at 500rpm at room temperature for 30 minutes, and allowed to stand at 4 ℃ for hydration in a refrigerator to obtain a protein solution. Mixing the obtained protein solution with 0.24g of TEMPO oxidized bacterial cellulose nano powder (the carboxyl content is 0.6mmol/g), adjusting the pH value to 3, and preparing a uniformly mixed protein/fiber compound. 100mL of olive oil was dispersed in the prepared protein/fiber complex, and shear-dispersed in a high-speed shearer at a shear revolution of 12000rpm for 20 minutes, to prepare an oil-in-water Pickering emulsion in a state shown in FIG. 4.
The emulsion prepared by the embodiment has no oil bloom precipitation, the particle size distribution of the emulsion is uniform, the emulsion is not layered after being placed for 14 days, and the emulsion is in a gel-like state and is not easy to flow.
Example 16, 3g of isolated soy protein powder was weighed, added to 100mL of distilled water, dissolved uniformly by magnetic stirring at 500rpm at room temperature for 30 minutes, and allowed to stand at 4 ℃ for hydration in a refrigerator to obtain a protein solution. Mixing the obtained protein solution with 0.24g of TEMPO oxidized bacterial cellulose nano powder (the carboxyl content is 0.6mmol/g), adjusting the pH value to 3, and preparing a uniformly mixed protein/fiber compound. 100mL of olive oil was dispersed in the prepared protein/fiber complex, and sonicated with a cell disruptor at 600w power at 20kHz for 5 minutes to prepare an oil-in-water Pickering emulsion.
The emulsion prepared by the embodiment has the advantages that an oil layer is obviously separated out on the surface, the emulsion is placed and stood for 24 hours and is obviously layered, the particle size distribution of the emulsion is not uniform, the viscosity of the emulsion is low, and the emulsion is easy to flow.
Example 17, 3g of soy protein isolate powder was weighed, added to 100mL of distilled water, dissolved uniformly by magnetic stirring at 500rpm at room temperature for 30 minutes, and allowed to stand at 4 ℃ for hydration in a refrigerator to obtain a protein solution. Mixing the obtained protein solution with 0.24g of TEMPO oxidized bacterial cellulose nano powder (the carboxyl content is 0.6mmol/g), adjusting the pH value to 3, and preparing a uniformly mixed protein/fiber compound. 100mL of olive oil was dispersed in the prepared protein/fiber complex, and sonicated with a cell disruptor at 600w power at 20kHz for 15 minutes to prepare an oil-in-water Pickering emulsion.
The emulsion prepared by the embodiment has the advantages that an oil layer is separated out on the surface, the emulsion is placed and stood for 24 hours to be obviously layered, the particle size distribution of the emulsion is uniform, the viscosity of the emulsion is low, and the emulsion is easy to flow.
Example 18, 3g of soy protein isolate powder was weighed, added to 100mL of distilled water, dissolved uniformly by magnetic stirring at 500rpm at room temperature for 30 minutes, and allowed to stand at 4 ℃ for hydration in a refrigerator to obtain a protein solution. Mixing the obtained protein solution with 0.24g of TEMPO oxidized bacterial cellulose nano powder (the carboxyl content is 0.6mmol/g), adjusting the pH value to 3, and preparing a uniformly mixed protein/fiber compound. 100mL of olive oil was dispersed in the prepared protein/fiber complex, and sonicated with a cell disruptor at 600w power at 20kHz for 30 minutes to prepare an oil-in-water Pickering emulsion.
The emulsion prepared by the embodiment has the advantages that an oil layer is separated out on the surface, the emulsion is placed and stood for 24 hours to be obviously layered, the particle size distribution of the emulsion is uniform, the viscosity of the emulsion is low, and the emulsion is easy to flow.
Example 19, 3g of isolated soy protein powder was weighed, added to 100mL of distilled water, dissolved uniformly by magnetic stirring at 500rpm at room temperature for 30 minutes, and allowed to stand at 4 ℃ for hydration in a refrigerator to obtain a protein solution. Mixing the obtained protein solution with 0.24g of TEMPO oxidized bacterial cellulose nano powder (the carboxyl content is 0.6mmol/g), adjusting the pH value to 3, and preparing a uniformly mixed protein/fiber compound. 100mL of olive oil was dispersed in the prepared protein/fiber complex, and treated 10 times with a high pressure homogenizer at a pressure of 40MPa to prepare an oil-in-water Pickering emulsion.
The emulsion prepared by the embodiment has the advantages that an oil layer is obviously separated out on the surface, the grain diameter of oil drops is not uniform, the emulsion is not layered after being placed for 14 days, and the emulsion has high viscosity and is difficult to flow.
Example 20, 3g of soy protein isolate powder was weighed, added to 100mL of distilled water, dissolved uniformly by magnetic stirring at 500rpm at room temperature for 30 minutes, and allowed to stand at 4 ℃ for hydration in a refrigerator to obtain a protein solution. Mixing the obtained protein solution with 0.24g of TEMPO oxidized bacterial cellulose nano powder (the carboxyl content is 0.6mmol/g), adjusting the pH value to 3, and preparing a uniformly mixed protein/fiber compound. 100mL of olive oil was dispersed in the prepared protein/fiber complex, and treated 5 times with a high pressure homogenizer at a pressure of 60MPa to prepare an oil-in-water Pickering emulsion.
The emulsion prepared by the embodiment has no oil flower on the surface, small oil drop particle size and uniform distribution, no layering phenomenon after the emulsion is placed for 14 days, and high viscosity and difficult flowing.
Example 21, 3g of isolated soy protein powder was weighed, added to 100mL of distilled water, dissolved uniformly by magnetic stirring at 500rpm at room temperature for 30 minutes, and allowed to stand at 4 ℃ for hydration in a refrigerator to obtain a protein solution. Mixing the obtained protein solution with 0.24g of TEMPO oxidized bacterial cellulose nano powder (the carboxyl content is 0.6mmol/g), adjusting the pH value to 3, and preparing a uniformly mixed protein/fiber compound. 100mL of olive oil was dispersed in the prepared protein/fiber complex, and treated 1 time with a high pressure homogenizer at a pressure of 100MPa to prepare an oil-in-water Pickering emulsion.
The emulsion prepared by the embodiment has no oil flower precipitation on the surface, large oil drop particle size and uneven distribution, and the emulsion has a micro layering phenomenon after being placed for 14 days, has high viscosity and is difficult to flow.
Example 22, 3g of isolated soy protein powder was weighed and added to 100mL of distilled water, and the mixture was dissolved uniformly by magnetic stirring at 500rpm at room temperature for 30 minutes, and then the mixture was allowed to stand at 4 ℃ for hydration in a refrigerator to obtain a protein solution. Mixing the obtained protein solution with 0.24g of TEMPO oxidized bacterial cellulose nano powder (the carboxyl content is 0.6mmol/g), adjusting the pH value to 3, and preparing a uniformly mixed protein/fiber compound. 100mL of olive oil was dispersed in the prepared protein/fiber complex and treated 10 times with a high pressure microfluidizer at 40MPa to prepare an oil-in-water Pickering emulsion.
The emulsion prepared by the embodiment has no oil flower on the surface, larger oil drop particle size and uneven distribution, no layering phenomenon after the emulsion is placed for 14 days, and high viscosity and no flowing.
Example 23, 3g of isolated soy protein powder was weighed and added to 100mL of distilled water, and the mixture was dissolved uniformly by magnetic stirring at 500rpm at room temperature for 30 minutes, and then the mixture was allowed to stand at 4 ℃ for hydration in a refrigerator to obtain a protein solution. Mixing the obtained protein solution with 0.24g of TEMPO oxidized bacterial cellulose nano powder (the carboxyl content is 0.6mmol/g), adjusting the pH value to 3, and preparing a uniformly mixed protein/fiber compound. 100mL of olive oil was dispersed in the prepared protein/fiber complex and treated 5 times with a high pressure microfluidizer at a pressure of 50MPa to prepare an oil-in-water Pickering emulsion.
The emulsion prepared by the embodiment has no oil flower on the surface, small oil drop particle size and uniform distribution, no layering phenomenon after the emulsion is placed for 14 days, and high viscosity and no flowing.
Example 24, 3g of isolated soy protein powder was weighed, added to 100mL of distilled water, dissolved uniformly by magnetic stirring at 500rpm at room temperature for 30 minutes, and allowed to stand at 4 ℃ for hydration in a refrigerator to obtain a protein solution. Mixing the obtained protein solution with 0.24g of TEMPO oxidized bacterial cellulose nano powder (the carboxyl content is 0.6mmol/g), adjusting the pH value to 3, and preparing a uniformly mixed protein/fiber compound. 100mL of olive oil was dispersed in the prepared protein/fiber complex and treated 1 time with a high pressure microfluidizer at 80MPa to prepare an oil-in-water Pickering emulsion.
A small amount of oil layer is separated out on the surface of the emulsion prepared by the embodiment, the oil drop particle size is large and is not uniformly distributed, the emulsion is not layered after being placed for 14 days, and the viscosity of the emulsion is large and does not flow.
The analysis examples 15 to 24 show that the emulsion obtained by different emulsification methods has different particle sizes and distributions, compared with ultrasonic emulsification, the emulsion treated by high-speed shearing, high-pressure homogenization and high-pressure microjet has smaller and uniform particle sizes, the emulsion treated by high-pressure microjet has smaller particle sizes, but the emulsified oil phase is limited, and the high-speed shearing and high-pressure homogenization emulsification effects are better.
Example 25A protein solution was prepared by weighing 3g of soybean protein isolate powder, adding to 100mL of distilled water, magnetically stirring at 500rpm at room temperature for 30 minutes to dissolve the powder uniformly, and then placing the solution in a refrigerator at 4 ℃. Mixing the obtained protein solution with 0.24g of TEMPO oxidized bacterial cellulose nano powder (the carboxyl content is 0.6mmol/g), adjusting the pH value to 3, and preparing a uniformly mixed protein/fiber compound. 200mL of rapeseed oil was dispersed in the prepared protein/fiber complex, and shear-dispersed in a high-speed shear at 12000rpm for 20 minutes to prepare an oil-in-water Pickering emulsion.
The emulsion prepared by the embodiment has no oil flower precipitation on the surface, small oil drop particle size and uniform distribution, no layering phenomenon after being placed for 14 days, and the emulsion is in a gel-like state and has certain fluidity.
Example 26, 3g of isolated soy protein powder was weighed and added to 100mL of distilled water, and the mixture was dissolved uniformly by magnetic stirring at 500rpm at room temperature for 30 minutes, and then the mixture was allowed to stand at 4 ℃ for hydration in a refrigerator to obtain a protein solution. Mixing the obtained protein solution with 0.24g of TEMPO oxidized bacterial cellulose nano powder (the carboxyl content is 0.6mmol/g), adjusting the pH value to 3, and preparing a uniformly mixed protein/fiber compound. 300mL of rapeseed oil was dispersed in the prepared protein/fiber complex, and shear-dispersed in a high-speed shear at 12000rpm for 20 minutes to prepare an oil-in-water Pickering emulsion in the state shown in FIG. 5.
The emulsion prepared by the embodiment has no oil flower on the surface, small oil drop particle size and uniform distribution, no layering phenomenon after being placed for 14 days, no flowing of the emulsion in a gel-like state and good viscoelasticity.
Example 27, 3g of isolated soy protein powder was weighed and added to 100mL of distilled water, and the mixture was dissolved uniformly by magnetic stirring at 500rpm at room temperature for 30 minutes, and then the mixture was allowed to stand at 4 ℃ for hydration in a refrigerator to obtain a protein solution. Mixing the obtained protein solution with 0.24g of TEMPO oxidized bacterial cellulose nano powder (the carboxyl content is 0.6mmol/g), adjusting the pH value to 3, and preparing a uniformly mixed protein/fiber compound. 400mL of rapeseed oil was dispersed in the prepared protein/fiber complex, and shear-dispersed in a high-speed shear at 12000rpm for 20 minutes to prepare an oil-in-water Pickering emulsion.
A small amount of oil stains are separated out on the surface of the emulsion prepared by the embodiment, the particle size distribution of oil drops is uneven, the emulsion is not layered after being placed for 14 days, and the emulsion is in a gel-like state and does not flow.
The results of the analysis examples 25 to 27 show that 300mL of rapeseed oil is added as an oil phase to be added into 100mL of protein/fiber composite suspension, and the prepared Pickering emulsion is emulsified, has the oil loading of 75%, is good in stability, does not have the phenomenon of layering, does not have the phenomenon of oil flower precipitation, does not flow in a gel-like state, and has strong viscoelasticity.
Claims (9)
1. A preparation method of a high oil-loading emulsion rich in fibrous polysaccharide is characterized by comprising the following steps: the method comprises the following specific steps:
1) adding 1-5 g of protein powder into 100mL of distilled water, magnetically stirring at 500rpm at normal temperature for 30 minutes to dissolve uniformly, and placing in a refrigerator at 4 ℃ for hydration to obtain a protein solution;
the protein powder is as follows: one or two of soybean protein isolate powder, pea protein isolate powder, whey protein isolate powder, egg white protein powder and casein powder;
2) mixing the protein solution obtained in the step 1) with 0.15-0.4 g of aqueous dispersion powder of fiber polysaccharide, and adjusting the pH value of the system to 3-11 to prepare a uniformly mixed protein/fiber compound;
the fiber polysaccharide water dispersion powder is: plant cellulose powder, fungal cellulose powder or bacterial cellulose powder;
3) dispersing 100-400 mL of oil phase in the protein/fiber compound prepared in the step 2), and emulsifying to prepare an oil-in-water emulsion with high oil loading;
the oil phase is liquid edible oil, specifically soybean oil, peanut oil, corn oil, rapeseed oil or olive oil;
the method for preparing the emulsion by emulsification comprises the following steps: high speed shearing method, ultrasonic emulsification method, high pressure homogenization method or high pressure micro-jet method.
2. The method for preparing the oil-in-water emulsion with high oil loading and rich fiber polysaccharide according to claim 1, wherein the method comprises the following steps: weighing 1-5 g of soybean protein isolate powder in the step 1), and adding into 100mL of distilled water; weighing 5g of pea protein isolate powder, and adding the pea protein isolate powder into 100mL of distilled water; weighing 5g of whey protein isolate powder, and adding into 100mL of distilled water; weighing 5g of egg white protein powder, and adding the egg white protein powder into 100mL of distilled water; casein powder (1 g) was weighed and added to 100mL of distilled water.
3. The method for preparing the high oil-loading oil-in-water emulsion rich in fiber polysaccharide according to claim 2, characterized in that: 3g of soybean protein isolate powder is weighed in the step 1) and added into 100mL of distilled water.
4. The method for preparing the oil-in-water emulsion with high oil loading and rich fiber polysaccharide according to claim 1, wherein the method comprises the following steps: in step 2), the protein solution obtained in step 1) was mixed with 0.24g of aqueous dispersion powder of a fibrous polysaccharide.
5. The method for preparing the oil-in-water emulsion with high oil loading and rich fiber polysaccharide according to claim 1, wherein the method comprises the following steps: the aqueous dispersion powder of the fibrous polysaccharide used in the step 2) is plant cellulose powder, fungal cellulose powder or bacterial cellulose powder, and the aqueous dispersion powder of the fibrous polysaccharide is respectively: microcrystalline cellulose powder prepared from pure wood pulp, cellulose nanocrystalline powder prepared from needle mushroom, and bacterial cellulose nanopowder oxidized by TEMPO; the carboxyl content in the TEMPO oxidized bacterial cellulose nano powder is 0.6 mmol/g.
6. The method for preparing the high oil-loading oil-in-water emulsion rich in fiber polysaccharide according to claim 5, wherein the method comprises the following steps: mixing the pea protein isolate solution, the whey protein isolate solution, the egg albumin solution and the casein protein solution used in the step 2) with the aqueous dispersion powder of the fibrous polysaccharide, and adjusting the pH value to 7; the soybean protein isolate solution and the fiber polysaccharide water dispersion powder are mixed, and the pH value is adjusted to be 3-11.
7. The method for preparing the high oil-loading oil-in-water emulsion rich in fiber polysaccharide according to claim 5, wherein the method comprises the following steps: mixing the soybean protein isolate used in the step 2) with the aqueous dispersion powder of the fibrous polysaccharide, and adjusting the pH value to 3.
8. The method for preparing the oil-in-water emulsion with high oil loading and rich fiber polysaccharide according to claim 1, wherein the method comprises the following steps: the conditions of high-speed shearing adopted in the step 3) are as follows: the rotating speed is 5000-20000 rpm, the time is 5-30 minutes, the preferred rotating speed is 12000rpm, and the shearing time is 20 minutes;
the conditions of the ultrasonic emulsification method are as follows: carrying out ultrasonic treatment at 20kHz for 5-30 minutes under the power of 600 w;
the conditions of the high-pressure homogenization method are as follows: treating for 1-10 times under the pressure of 40-100 MPa;
the conditions of the high-pressure micro-jet method are as follows: treating for 1-10 times under the pressure of 40-80 MPa.
9. The method for preparing the oil-in-water emulsion with high oil loading and rich fiber polysaccharide according to claim 1, wherein the method comprises the following steps: the conditions of high-speed shearing adopted in the step 3) are as follows: rotating at 12000rpm, and shearing for 20 minutes;
the conditions of the ultrasonic emulsification method are as follows: ultrasonic treatment is carried out for 15 minutes at 20kHz under the power of 600 w;
the conditions of the high-pressure homogenization method are as follows: processing for 5 times under the power of 60 MPa;
the conditions of the high-pressure micro-jet method are as follows: treating for 5 times under the power of 50 MPa.
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