CN115104722A - High internal phase pickering emulsion capable of reducing fat digestion/inhibiting fat digestion and preparation method thereof - Google Patents
High internal phase pickering emulsion capable of reducing fat digestion/inhibiting fat digestion and preparation method thereof Download PDFInfo
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- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
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- A23G9/00—Frozen sweets, e.g. ice confectionery, ice-cream; Mixtures therefor
- A23G9/32—Frozen sweets, e.g. ice confectionery, ice-cream; Mixtures therefor characterised by the composition containing organic or inorganic compounds
- A23G9/327—Frozen sweets, e.g. ice confectionery, ice-cream; Mixtures therefor characterised by the composition containing organic or inorganic compounds characterised by the fatty product used, e.g. fat, fatty acid, fatty alcohol, their esters, lecithin, glycerides
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- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
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Abstract
The application relates to the technical field of emulsion material preparation methods and food processing, in particular to a high internal phase pickering emulsion capable of reducing fat digestion/inhibiting fat digestion and a preparation method thereof. The high internal phase pickering emulsion provided by the application comprises an oil phase and composite nano particles adsorbed on an oil-water interface of the oil phase, wherein the material of the composite nano particles comprises whey protein isolate and sodium alginate, and the concentration of the composite nano particles is at least 2.4 w/v%. The high internal phase pickering emulsion provided by the application uses special composite nano particles as an emulsifier, can effectively embed hydrophobic oil phase to form stable high internal phase emulsion, can obviously inhibit the digestion of fat, and has the advantages of initial digestion rate shearing and overall fat digestion rate reduction. The high internal phase pickering emulsion has good application prospect in the field of food.
Description
Technical Field
The application belongs to the technical field of emulsion material preparation and food processing, and particularly relates to a high internal phase pickering emulsion capable of reducing fat digestion/inhibiting fat digestion and a preparation method thereof.
Background
Emulsions are classified into low internal phase emulsions (lips) and High Internal Phase Emulsions (HIPEs) based on the volume fraction of the dispersed phase, whereas emulsions with a volume fraction of internal phase greater than 74% are referred to as high internal phase emulsions. Along with the increase of the volume fraction of the internal phase of the emulsion, the emulsion is subjected to phase transformation, the emulsion droplets are accumulated and deformed into a multi-area geometric shape, and the macroscopic angle emulsion realizes the transformation from liquid oil to solid, so that the solid property of the liquid oil is endowed with great application value. In recent years, high internal phase emulsions have shown great potential applications in the food, chemical and biomedical fields, such as site-directed delivery of functional nutrients or drugs, which can replace partially hydrogenated oils to reduce the intake of trans fatty acids in the human body. Although some high internal phase emulsions such as mayonnaise, ice cream and the like are popular with consumers, the use of these emulsions greatly increases the fat content, particularly with high internal phase emulsions where the oil phase ratio is very high and excessive fat intake can lead to a range of health problems such as cardiovascular and cerebrovascular disease and obesity.
Pickering emulsion is an emulsion formed by irreversible adsorption of solid particles on an oil-water interface, and has excellent stability. The current research on pickering emulsions focuses on the development of novel emulsifiers or the delivery of functional nutrients, and there are relatively few reports on the digestion of fat by the body, while the research on high internal phase pickering emulsions that inhibit fat digestion is more recent. Most of the solid particles used in pickering emulsions are inorganic particles or synthetic polymers, such as graphene and silica, which have excellent stabilizing effects on emulsions, but have problems of low biosafety and difficulty in degradation. The food industry and the pharmaceutical sector are more inclined to the use of colloidal particles based on biomacromolecules as stabilizers for pickering emulsions. Polysaccharide particles can produce greater steric stability, but in many cases surface hydrophobicization modification is still required to improve their emulsifying properties. Although protein particles have good emulsibility, the structural stability is greatly influenced by external environmental factors, and the protein particles are easy to be structurally dissociated when adsorbed on a two-phase interface.
Therefore, on the premise of being based on biomacromolecules, how to construct pickering emulsion which has good stability and can reduce the digestion and absorption of fat in vivo is a problem to be solved urgently at present,
disclosure of Invention
The application aims to provide a high internal phase pickering emulsion capable of reducing fat digestion/inhibiting fat digestion and a preparation method thereof, and aims to form pickering emulsion which is safe, good in stability and capable of reducing lipid digestion.
In order to achieve the purpose of the application, the technical scheme adopted by the application is as follows:
in a first aspect, the present application provides a high internal phase pickering emulsion comprising an oil phase and composite nanoparticles adsorbed at the oil-water interface of the oil phase, the material of the composite nanoparticles comprising whey protein isolate and sodium alginate, the concentration of the composite nanoparticles being at least 2.4 w/v%.
In one embodiment, the concentration of the composite nanoparticles is 2.4-4.0 w/v%.
In one embodiment, the mass ratio of the whey protein isolate to the sodium alginate is 1: 1-5: 1; and/or the presence of a gas in the gas,
the particle size of the composite nano-particles is 200-300 nm.
In one embodiment, the oil phase of the high internal phase pickering emulsion is 75 to 80 volume percent.
In one embodiment, the oil phase consists of medium chain triglycerides.
In one embodiment, the medium chain triglyceride is a medium chain fatty acid triglyceride formed by esterification of saturated fatty acids having 6 to 12 carbon atoms and glycerol.
In a second aspect, the present application also provides a method of preparing a high internal phase pickering emulsion comprising the steps of:
preparing an aqueous solution of composite nano particles;
and mixing the aqueous solution of the composite nano particles with the oil phase material, and then carrying out shearing emulsification treatment to obtain the high internal phase pickering emulsion.
In one embodiment, the step of formulating the aqueous solution of composite nanoparticles comprises:
preparing whey protein isolate water solution and sodium alginate water solution;
mixing the whey protein isolate aqueous solution and the sodium alginate aqueous solution with sodium chloride to obtain a mixed solution;
the mixed solution is adjusted to be acidic and then stirred.
In one embodiment, the concentration of sodium chloride in the mixed solution is 10-200 mM; and/or the presence of a gas in the gas,
in the step of adjusting the mixed solution to be acidic, the pH value of the acidity is 4.0-6.0; and/or the presence of a gas in the gas,
the stirring treatment comprises the following steps: stirring at a rotation speed of 400-600 r/min for 20-40 min.
In one embodiment, the shear emulsification treatment comprises: emulsifying at 20000-21000 r/min for 1-3 min.
The high internal phase pickering emulsion provided by the application uses the unique composite nano particles as an emulsifier, and can effectively embed hydrophobic oil phase to form stable high internal phase emulsion, the composite nano particles comprise whey protein isolate and sodium alginate, wherein the sodium alginate interacts with the whey protein isolate through electrostatic interaction to form hydrophilic composite nano particles with good acid-heat stability, the whey protein isolate and the sodium alginate of the composite nano particles have wide sources and low cost, and have various beneficial effects on human bodies, high biocompatibility and degradability, so the high internal phase pickering emulsion is safe to use, and the high internal phase pickering emulsion can obviously inhibit fat digestion after the composite nano particles are used as the emulsifier to embed the oil phase, so the fat digestion rate of the whole oil phase is reduced, and the health risk caused by introducing excessive grease into the high internal phase pickering emulsion is reduced, therefore, the high internal phase pickering emulsion has good application prospect in the field of food.
According to the preparation method of the high internal phase pickering emulsion, the water solution of the specific composite nano particles is mixed with the oil phase material for shearing and emulsifying treatment, so that the high internal phase pickering emulsion which is high in biocompatibility, good in stability and capable of effectively inhibiting lipid digestion is obtained.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings needed to be used in the description of the embodiments are briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a graph of the appearance of high internal phase pickering emulsions of various concentrations of composite nanoparticles provided in the examples herein;
FIG. 2 is a comparative graph of a high internal phase pickering emulsion of 2.4% concentration composite nanoparticles provided in the examples herein before and after 75 days of storage; a is a high internal phase pickering emulsion made on the same day, B is a high internal phase pickering emulsion after 75 days of storage;
FIG. 3 is a graph of the apparent viscosity of a high internal phase pickering emulsion of composite nanoparticles at a concentration of 2.4% as provided in the examples herein;
FIG. 4 is a plot of the modulus of a high internal phase pickering emulsion of 2.4% concentration composite nanoparticles provided in the examples herein;
fig. 5 is a comparative graph of lipid digestion of a high internal phase pickering emulsion of 2.4% concentration of composite nanoparticles provided in the examples of the present application.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present application more clearly apparent, the present application is further described in detail below with reference to the embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the present application and are not intended to limit the present application.
In this application, the term "and/or" describes an association relationship of associated objects, meaning that there may be three relationships, e.g., a and/or B, which may mean: a is present alone, A and B are present simultaneously, and B is present alone. Wherein A and B can be singular or plural. The character "/" generally indicates that the former and latter associated objects are in an "or" relationship.
It should be understood that, in various embodiments of the present application, the sequence numbers of the above-mentioned processes do not mean the execution sequence, some or all of the steps may be executed in parallel or executed sequentially, and the execution sequence of each process should be determined by its function and inherent logic, and should not constitute any limitation to the implementation process of the embodiments of the present application.
The terminology used in the embodiments of the present application is for the purpose of describing particular embodiments only and is not intended to be limiting of the application. As used in the examples of this application and the appended claims, the singular forms "a", "an", and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
The weight of the related components mentioned in the description of the embodiments of the present application may not only refer to the specific content of each component, but also represent the proportional relationship of the weight among the components, and therefore, the content of the related components is scaled up or down within the scope disclosed in the description of the embodiments of the present application as long as it is scaled up or down according to the description of the embodiments of the present application. Specifically, the mass described in the specification of the embodiments of the present application may be a mass unit known in the chemical industry field such as μ g, mg, g, kg, etc.
The terms "first" and "second" are used for descriptive purposes only and are used for distinguishing purposes such as substances from one another, and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. For example, a first XX may also be referred to as a second XX, and similarly, a second XX may also be referred to as a first XX, without departing from the scope of embodiments of the present application. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature.
In a first aspect, the embodiments of the present application provide a high internal phase pickering emulsion, the high internal phase pickering emulsion comprising an oil phase and composite nanoparticles adsorbed at the oil-water interface of the oil phase, the material of the composite nanoparticles comprising whey protein isolate and sodium alginate, the concentration of the composite nanoparticles being at least 2.4 w/v%.
The high internal phase pickering emulsion provided by the embodiment of the application uses the specific composite nano particles as the emulsifier, can effectively embed the hydrophobic oil phase to form the stable high internal phase emulsion, the composite nano particles comprise whey protein isolate and sodium alginate, wherein the sodium alginate is adsorbed with the whey protein isolate through electrostatic action to form the hydrophilic composite nano particles with good acid-heat stability, the whey protein isolate and the sodium alginate raw materials of the composite nano particles are not only wide in source and low in cost, but also have various beneficial effects on human bodies, high in biocompatibility and degradable, so that the use is safe, and meanwhile, after the composite nano particles are used as the emulsifier to embed the oil phase, the high internal phase pickering emulsion can obviously inhibit the digestion of fat, the fat digestion rate of the whole oil phase is reduced, so that the health risk caused by introducing excessive fat into the high internal phase pickering emulsion is reduced, therefore, the high internal phase pickering emulsion has good application prospect in the field of food.
Based on the polysaccharide particles alone, better emulsifying performance is difficult to generate, and the protein particles alone have poor structural stability and are difficult to be stably adsorbed on a two-phase interface. Therefore, the composite nanoparticle with good spatial stability and emulsibility is formed by compounding Whey Protein Isolate (WPI) and sodium Alginate (ALG), specifically, the composite nanoparticle comprises Whey protein isolate and sodium alginate, wherein the sodium alginate and the Whey protein isolate form hydrophilic composite nanoparticle with good acid-heat stability through electrostatic interaction, the Whey protein isolate is high in purity and rich in nutritional value, the sodium alginate is a natural polysaccharide, and the sodium alginate and the Whey protein isolate form a compound through electrostatic interaction, so that the nanoparticle with both stability and emulsibility can be obtained, and the composite nanoparticle has wide prospects in the fields of food industry and medicine. The sodium alginate and the whey protein isolate raw materials both meet the generally accepted safety (GRAS) standard, the construction materials are biological macromolecules which widely exist in nature, the raw materials are wide in source, economical and practical, the preparation method is green and convenient, and the raw materials are good in biocompatibility and degradable, so that the high internal phase pickering emulsion is low in cost.
In the examples of the present application, it was demonstrated by experiments that a stable high internal phase pickering emulsion was formed only when the concentration of the composite nanoparticles in the high internal phase pickering emulsion was at least 2.4 w/v%, i.e. how many grams of solute were contained in 100ml of liquid (total volume of solute and solvent), and 1 w/v% was 10 g/L. Specifically, the concentration of the composite nanoparticles is 2.4-4 w/v%, and the volume ratio of the internal phase in the high internal phase pickering emulsion can reach 75-80%; the high internal phase pickering emulsion can have a high internal phase volume ratio of up to 80% by emulsification of the composite nanoparticles at the above concentrations. The high internal phase pickering emulsion which can be applied to a food system and has a function of inhibiting fat digestion is limited at present, and the composite nanoparticles are emulsified at a concentration of at least 2.4 w/v% to enable the oil phase proportion of the high internal phase pickering emulsion to reach 80%, the lipid digestion rate is uniform, the release rate of free fatty acid in intestinal tract is lower than 50%, and on the premise of meeting the emulsion stability and solid gel structure, the high internal phase pickering emulsion can inhibit fat digestion, increase satiety and reduce health risks caused by excessive fat ingestion.
In one embodiment, the mass ratio of the whey protein isolate to the sodium alginate is 1: 1-5: 1; for example, whey protein isolate and sodium alginate are combined into composite nano particles through electrostatic interaction at a mass ratio of 1: 1-5: 1 and are used as an emulsifier, wherein the mass ratio of whey protein isolate to sodium alginate can be 1:1, 2:1, 3:1, 4:1, 5:1 and the like, and the composite nano particles formed under the conditions of the above ratios have better comprehensive effects of acid-heat stability and emulsibility.
In one embodiment, the composite nanoparticles have a particle size of 200 to 300nm, such as 200nm, 220nm, 240nm, 260nm, 280nm, 300nm, and the like. The composite nano-particles with the particle sizes are spherical and uniform in size, can be better divided, and can form uniform high internal phase pickering emulsion when being used as an emulsifier.
In one embodiment, the high internal phase pickering emulsion has uniform droplet size distribution of about 30-40 microns, has a permeable 3D network structure, and can effectively embed triglyceride hydrophobic substances by enabling the oil phase loading to be as high as 80% through composite nanoparticles.
In one embodiment, the oil phase is composed of medium chain triglycerides, specifically, medium chain triglycerides are medium chain fatty acid triglycerides (MCT) formed by esterification of saturated fatty acids containing 6-12 carbon atoms and glycerol.
The present application also provides, in a second aspect, a method of preparing a high internal phase pickering emulsion comprising the steps of:
s01: preparing an aqueous solution of composite nano particles;
s02: and mixing the aqueous solution of the composite nano particles with the oil phase material, and then carrying out shearing emulsification treatment to obtain the high internal phase pickering emulsion.
According to the preparation method of the high internal phase pickering emulsion, the specific water solution of the composite nano particles and the oil phase material are mixed for shearing and emulsifying treatment, so that the high internal phase pickering emulsion which is high in biocompatibility, good in stability and capable of effectively inhibiting lipid digestion is obtained.
In one embodiment, the step of preparing the aqueous solution of composite nanoparticles comprises:
s011: preparing whey protein isolate water solution and sodium alginate water solution;
s012: mixing the whey protein isolate aqueous solution and the sodium alginate aqueous solution with sodium chloride to obtain a mixed solution;
s013: and adjusting the mixed solution to be acidic, and then stirring to obtain the aqueous solution of the composite nano particles.
According to the embodiment of the application, whey protein isolate aqueous solution and sodium alginate aqueous solution are mixed with sodium chloride, then the mixed solution is adjusted to be acidic, and the whey protein isolate and the sodium alginate are compounded to form the composite nano-particles through electrostatic adsorption. The preparation method has the advantages of wide raw material sources and simple preparation process, and can obtain the degradable composite nano-particles with uniform particle size, stable structure, good emulsibility and high biocompatibility only under the acidic condition.
In one embodiment, the aqueous whey protein isolate solution of step S011 may be obtained by dissolving whey protein isolate in water, and the aqueous sodium alginate solution may be obtained by dissolving sodium alginate in water. Specifically, the prepared whey protein isolate aqueous solution can be 0.8-1.2 (w/v)% whey protein isolate aqueous solution, and the prepared sodium alginate aqueous solution can be 0.8-1.2 (w/v)% sodium alginate aqueous solution.
In one embodiment, step S012 mixes the whey protein isolate aqueous solution and the sodium alginate aqueous solution with sodium chloride to obtain a mixed solution, wherein the concentration of sodium chloride is 10-200 mM, such as 10mM, 50mM, 150mM, 180mM, 200mM, and the like. The sodium chloride is dissolved in the mixed solution to form sodium ions and chloride ions, so that an environment is provided for the whey protein isolate and the sodium alginate to generate electrostatic interaction, and the sodium chloride under the concentration condition can enable the whey protein isolate and the sodium alginate to be better electrostatically adsorbed.
In one embodiment, in the step of adjusting the mixed solution to be acidic in step S013, the pH of the acidity is 4.0 to 6.0. Under the acidic condition, the sodium alginate can be stably compounded with the whey protein isolate, so that hydrophilic composite nano-particles with good acid-heat stability are formed. Specifically, under the acidic condition, the mixed solution is stirred at the speed of 400-600 r/min for 20-40 min, and the sodium alginate and the whey protein isolate are fully compounded. Specifically, acid adjustment may be performed with an acid solution such as hydrochloric acid, acetic acid, or the like.
In one embodiment, the obtained aqueous solution of the composite nano-particles can be further removed from the aqueous solvent, so as to obtain solid composite nano-particles, and of course, the solid composite nano-particles can also be directly used as an emulsifier in the form of the composite nano-particle solution.
Furthermore, in the step of the shearing emulsification treatment, the shearing emulsification rotating speed can be 20000 to 21000r/min, and the time can be 1 to 3 min. According to the embodiment of the application, the high internal phase pickering emulsion is constructed through high-speed shearing, the liquid oil is converted into the viscoelastic solid gel, a trans-fat solidification mode is not needed, and the preparation method of the high internal phase pickering emulsion can be applied to the field of food and has the advantages of nutrition, health, safety and the like.
In one embodiment, the high internal phase pickering emulsions of the present application are constructed by the steps of:
(1) accurately weighing whey protein isolate, adding the whey protein isolate into deionized water, fully dissolving the whey protein isolate by using a magnetic stirrer to obtain whey protein isolate aqueous solution, and storing the whey protein isolate aqueous solution at 4 ℃ for later use.
Accurately weighing sodium alginate, adding into deionized water, stirring to obtain transparent colloidal solution, and storing at 4 deg.C.
(2) Protein isolation according to whey: mixing a whey protein isolate aqueous solution and a sodium alginate aqueous solution according to the mass ratio of 1: 1-5: 1, simultaneously adding sodium chloride to obtain a mixed solution, adjusting the pH value to be within the range of 4.0-6.0, setting the NaCl concentration to be 10-200 mM, fully stirring for a certain time to fully compound the whey protein isolate and the sodium alginate, and centrifuging to remove insoluble substances to obtain a composite nanoparticle aqueous solution.
(3) Mixing the aqueous solution of the composite nano-particles with triglyceride, and then carrying out shearing emulsification treatment: emulsifying at the rotating speed of 20000-21000 r/min for 1-3 min to obtain the high internal phase pickering emulsion.
In one embodiment, experiments prove that the high internal phase pickering emulsion has excellent storage stability, the appearance does not change remarkably after being stored for 75 days at normal temperature (25-27 ℃), no oil phase is separated out, the high internal phase pickering emulsion is in a solid gel state, and the high internal phase pickering emulsion can meet the preparation requirement of food and cosmetics, and particularly can replace part of hydrogenated oil. Meanwhile, experiments in the embodiment of the application prove that the high internal phase pickering emulsion has a good inhibition effect on lipid digestion, and the release rate of free fatty acid in the digestion process (2h) of the emulsion in the intestinal tract is monitored by adopting a pH-stat method, so that only about 45% of release rate is finally found. The fat digestion rate is reduced, so that the fat absorption of the body can be effectively reduced, the obesity can be prevented, secondly, the intestinal tract movement can be reduced because a large amount of oil is not digested in the small intestine, the satiety is increased, the appetite is controlled, and the food intake is reduced, and the beneficial effects can be beneficial to the popularization and the application of the high internal phase pickering emulsion in products such as ice cream, peanut butter, mayonnaise and the like.
The following description will be given with reference to specific examples.
Example 1
A method of preparing a high internal phase pickering emulsion comprising the steps of:
(1) the preparation method of the WPI-ALG composite nanoparticle comprises the following steps:
accurately weighing 1.0g whey protein isolate (Davisco Foods International Inc) and adding into 100mL deionized water, stirring with magnetic stirrer for 1 hr/min, dissolving sufficiently to obtain whey protein isolate solution, and storing at 4 deg.C for use.
Accurately weighing 1.0g of sodium alginate, adding into 100mL of deionized water, stirring at 500r/min for 4h to obtain transparent colloidal liquid, obtaining sodium alginate solution, and storing at 4 ℃ for later use.
Protein isolation according to whey: mixing whey protein isolate solution and sodium alginate solution at a mass ratio of 5:1, fixing the concentration of whey protein isolate to 0.5% (w/v), adding NaCl to 200mM, adjusting pH to 4.0, stirring at 500r/min for 30min, and centrifuging at 1600r/min for 20min to remove insoluble substances.
The WPI-ALG composite nano-particles with the particle size of 268nm are obtained, and are spherical and uniform in size.
(2) A shearing and emulsifying step:
weighing the obtained WPI-ALG composite nano-particle solution according to the mass ratio, mixing with medium-chain fatty acid triglyceride (formed by esterification of saturated fatty acid with 12 carbon atoms and glycerol), and shearing and emulsifying at a high speed, wherein the rotating speed is 20600r/min, and the time is 2min, so as to obtain the high internal phase Pickering emulsion with the final oil phase volume ratio of up to 80%.
Example 2
A method of preparing a high internal phase pickering emulsion comprising the steps of:
(1) the preparation method of the WPI-ALG composite nanoparticle comprises the following steps:
accurately weighing 1.0g whey protein isolate (Davisco Foods International Inc) and adding into 100mL deionized water, stirring with magnetic stirrer for 1 hr/min, dissolving sufficiently to obtain whey protein isolate solution, and storing at 4 deg.C for use.
Accurately weighing 1.0g of sodium alginate, adding into 100mL of deionized water, stirring at 500r/min for 4h to obtain transparent colloidal liquid, obtaining sodium alginate solution, and storing at 4 ℃ for later use.
Protein isolation according to whey: mixing whey protein isolate solution and sodium alginate solution at a mass ratio of 1:1, fixing the concentration of whey protein isolate to 0.5% (w/v), adding NaCl to make the concentration to 100mM, adjusting pH to 6.0, stirring at 500r/min for 30min, and centrifuging at 1600r/min for 20min to remove insoluble substances.
The WPI-ALG composite nano-particles with the particle size of 240nm are obtained, and are spherical and uniform in size.
(2) A shearing and emulsifying step:
weighing the obtained WPI-ALG composite nano-particle solution according to the mass ratio, mixing with medium-chain fatty acid triglyceride (formed by esterification of saturated fatty acid with 6 carbon atoms and glycerol), and performing high-speed shearing emulsification at the rotating speed of 20000r/min for 1min to obtain the high-internal-phase Pickering emulsion with the final oil phase volume ratio of up to 78%.
Performance testing
Stability of
Fig. 1 is an appearance diagram of high internal phase pickering emulsion of WPI-ALG composite nanoparticles of example 1 with different concentrations, when the WPI-ALG composite nanoparticles in the high internal phase pickering emulsion are less than 2.4 w/v% of low concentration, it is difficult to form the high internal phase pickering emulsion stably, when the concentration of the WPI-ALG composite nanoparticles is increased to 2.4% w/v%, it is possible to form the high internal phase pickering emulsion with about 80% of oil phase volume ratio stably, and as shown in fig. 1, the high internal phase pickering emulsion of WPI-ALG composite nanoparticles with 2.4% w/v% of concentration is like paste, and can be inverted to realize the liquid oil to solid state transition. When the volume ratio of the oil phase is increased to 70%, demulsification and oil leakage occur after the oil phase is placed for a certain time, and a stable high-internal-phase pickering emulsion is difficult to form.
Figure 2 is an appearance and microscopy image of a high internal phase pickering emulsion of 2.4% w/v% concentration WPI-ALG composite nanoparticles of example 1 compared before and after 75 days. It can be seen from B of fig. 2 that after being left for 75 days, the high internal phase pickering emulsion can still be inverted, indicating that the high internal phase pickering emulsion forms a gel and is transformed from a liquid state to a solid state, which shows that the high internal phase pickering emulsion has no significant change in appearance after being stored for 75 days, and no oil phase is precipitated, no demulsification phenomenon, and can be inverted, indicating that the high internal phase pickering emulsion has good storage stability, and can effectively prevent unstable phenomena such as flocculation precipitation, austenite ripening, and the like.
Apparent viscosity and modulus
Figure 3 is a graph of the results of steady state flow tests of a high internal phase pickering emulsion of WPI-ALG composite nanoparticles at a concentration of 2.4% w/v% of example 1 showing Shear thinning as the Viscosity (Viscosity) decreases with increasing Shear rate (Shear rate) and the high internal phase pickering emulsion is a non-newtonian fluid. The reduction in interactions between the droplets results in the formation of a lubricating layer and a decrease in viscosity, resulting in an increase in the fluidity of the high internal phase pickering emulsion. Figure 4 is a graph of the modulus test of a high internal phase pickering emulsion of WPI-ALG composite nanoparticles of example 1 at a concentration of 2.4% w/v% with a G' (storage modulus) greater than G "(loss modulus) indicating that the emulsion is a gel emulsion exhibiting gel properties dominated by viscoelasticity under dynamic oscillation conditions at a certain Angular frequency (Angular frequency). The formation of this structure may be due to the thick particle layer formed at the oil-water interface, as well as the formation of a 3D network of particles in the continuous phase.
The rheological data further confirm that the high internal phase pickering emulsion of the examples is supported by the network structure formed by the high internal phase pickering emulsion in appearance and storage stability, the interface structure plays a key role in the formation of the viscoelastic property of the high internal phase pickering emulsion, and the WPI-ALG composite nanoparticle coated and penetrated network structure formed by the interaction between droplets is helpful for forming a solid material with certain rigidity.
Lipid digestion
The high internal phase pickering emulsion of WPI-ALG composite nanoparticles at a concentration of 2.4% w/v of example 1 simulates intestinal digestion, as the lipase hydrolysis of the encapsulated medium chain fatty acid triglycerides increases, the pH immediately drops, and the pH is maintained at 7.0 by titration with 0.5M NaOH. Simulated Intestinal Fluid (SIF) was maintained at 37 ℃ and pH 7.0 and digestion continued for 120min, and NaOH consumption was recorded during digestion at different time points to calculate free fatty acid release (FFA,%), as follows:
FFA(％)＝100×(V NaOH ×m NaOH ×M LipId )/2W LipId
in the formula, V NaOH Represents the volume of NaOH (L), m consumed to neutralize free fatty acids NaOH Represents the NaOH concentration (mol. L) -1 ，0.5)，M LipId Represents the molecular weight (g.mol) of the triglyceride -1 )，W LipId Represents the total mass (g) of medium-chain fatty acid triglycerides.
As shown in fig. 5, the titration kinetics of the high internal phase pickering emulsion samples of the examples of the present application proceed at a much faster rate than bulk oil samples (i.e., bulk medium chain fatty acid triglycerides). According to the Free Fatty Acid (FFA) release versus time curve, the rate of digestion of most lipids in the high internal phase pickering emulsion system is relatively uniform, FFA only reaches about 43% at the end of digestion, while FFA reaches 90% at the end of digestion in normal emulsions (emulsions with medium chain fatty acid triglyceride oil phase in 60% by volume). The digestion kinetics of the oil phase in the high internal phase pickering emulsion samples of the examples herein are faster compared to bulk oil, since the high internal phase pickering emulsions of the examples herein have a larger surface area than the bulk oil phase, but the release rate of free fatty acids from the high internal phase pickering emulsions prepared in the examples herein is reduced by half compared to conventional emulsions.
The above description is only exemplary of the present application and should not be taken as limiting the present application, as any modification, equivalent replacement, or improvement made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (10)
1. A high internal phase pickering emulsion comprising an oil phase and composite nanoparticles adsorbed to the oil-water interface of the oil phase, the material of the composite nanoparticles comprising whey protein isolate and sodium alginate, the concentration of the composite nanoparticles being at least 2.4 w/v%.
2. The high internal phase pickering emulsion of claim 1, wherein the concentration of the composite nanoparticles is from 2.4 to 4.0 w/v%.
3. The high internal phase pickering emulsion of claim 1, wherein the mass ratio of whey protein isolate to sodium alginate is 1:1 to 5: 1; and/or the presence of a gas in the gas,
the particle size of the composite nano-particles is 200-300 nm.
4. The high internal phase pickering emulsion of claim 1, wherein the volume percent of the oil phase in the high internal phase pickering emulsion is from 75 to 80%.
5. The high internal phase pickering emulsion of any one of claims 1-4, wherein the oil phase is comprised of medium chain triglycerides.
6. The high internal phase pickering emulsion of claim 5, wherein the medium chain triglyceride is a medium chain fatty acid triglyceride formed by esterification of a saturated fatty acid having from 6 to 12 carbon atoms and glycerol.
7. A method of preparing a high internal phase pickering emulsion according to any one of claims 1 to 6, comprising the steps of:
preparing an aqueous solution of the composite nanoparticles;
and mixing the aqueous solution of the composite nano particles with an oil phase material, and then carrying out shearing emulsification treatment to obtain the high internal phase pickering emulsion.
8. The method of claim 7, wherein the step of formulating the aqueous solution of composite nanoparticles comprises:
preparing whey protein isolate water solution and sodium alginate water solution;
mixing the whey protein isolate aqueous solution and the sodium alginate aqueous solution with sodium chloride to obtain a mixed solution;
and adjusting the mixed solution to be acidic, and then stirring.
9. The method according to claim 8, wherein the concentration of sodium chloride in the mixed solution is 10 to 200 mM; and/or the presence of a gas in the gas,
in the step of adjusting the mixed solution to be acidic, the pH value of the acidity is 4.0-6.0; and/or the presence of a gas in the gas,
the stirring treatment comprises: stirring at a rotation speed of 400-600 r/min for 20-40 min.
10. The method of claim 7, wherein the shear emulsification process comprises: emulsifying at 20000-21000 r/min for 1-3 min.
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