CN115444124B - Food-grade lipid Pickering particle-stabilized oil-in-water type high internal phase emulsion, and preparation method and application thereof - Google Patents
Food-grade lipid Pickering particle-stabilized oil-in-water type high internal phase emulsion, and preparation method and application thereof Download PDFInfo
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- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
- A61K8/04—Dispersions; Emulsions
- A61K8/06—Emulsions
- A61K8/062—Oil-in-water emulsions
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- 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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Abstract
The invention belongs to the technical field of food processing, and discloses an oil-in-water type high internal phase emulsion with stable food-grade lipid Pickering particles, and a preparation method and application thereof. The preparation method comprises the following steps: (1) Heating and mixing the high-melting-point lipid-fixing and emulsifying agent with distilled water, then shearing at high speed, performing ultrasonic dispersion, and then cooling to obtain lipid pickering particle dispersion liquid; (2) And mixing the lipid pickering particle dispersion liquid with vegetable oil, shearing at a high speed, and cooling to obtain the food-grade lipid pickering particle stable oil-in-water type high internal phase emulsion. The preparation method is simple, green and environment-friendly, and the prepared food-grade lipid pickering particles have an interface structure with obvious lipid pickering particle adsorption at an oil/water interface; the oil-in-water type high internal phase Pickering emulsion system prepared by the method has good stability, uniform emulsion droplet distribution, good stability within 1 month, and wide application prospect in the fields of food, medicine and cosmetics.
Description
Technical Field
The invention belongs to the technical field of food processing, and particularly relates to an oil-in-water type high internal phase emulsion with stable food-grade lipid Pickering particles, and a preparation method and application thereof.
Background
High internal phase emulsions, typically emulsions having an internal phase volume fraction in excess of 74%, have droplets in the internal dispersed phase intimately associated with each other and squeeze each other until the polygons are dispersed in the continuous phase, and the system assumes a non-flowable semi-solid texture. The high internal phase emulsion stabilized by the surfactant and the high internal phase emulsion stabilized by the solid active particles, i.e., the high internal phase pickering emulsion, can be classified according to the colloidal particles of the stable high internal phase emulsion. Compared with the common high internal phase emulsion which can be stabilized by adding a large amount of surfactant (5-50%), the high internal phase pickering emulsion can be stabilized by hardly adding or adding a small amount of surfactant, has enhanced interfacial stability, has better physical stability for resisting coagulation and milk out, and can better protect functional components. Based on this, the high internal phase pickering emulsion is widely used in the fields of foods, medicines, cosmetics, and the like.
Compared with inorganic particles, the pickering emulsion is prepared by adopting stable and safe natural food-grade particles in the food field. Research shows that the fat crystal particles have good interface wettability, are easy to diffuse from bulk phase to interface adsorption and assembly to form an interface film, and generate a large number of emulsion drops; the formed interfacial film has proper mechanical strength, and can avoid coagulation and oil precipitation when a large amount of emulsion drops coexist. The fat crystal particles determine the internal phase content, stability and processability of the emulsion system. The research on solid lipid-stabilized food grade pickering low internal phase emulsions is increasingly mature, but the construction and stabilization of oil-in-water type high internal phase emulsions by using lipid-based pickering particles is not realized at present.
How to prepare food-grade oil-in-water type high internal phase emulsion with green safety and good stability through lipid Pickering particles is one of the problems to be solved at present.
Disclosure of Invention
In order to overcome the defects and shortcomings of the prior art, the primary purpose of the invention is to provide a preparation method of an oil-in-water type high internal phase emulsion with stable food grade lipid Pickering particles, which has simple process, good stability of the prepared oil-in-water type high internal phase emulsion and green and safe.
The second object of the invention is to provide an oil-in-water type high internal phase emulsion with stable food grade lipid Pickering particles, which is prepared by the preparation method.
A third object of the present invention is to provide the use of an oil-in-water high internal phase emulsion with stable food grade lipid pickering particles.
The primary purpose of the invention is realized by the following technical scheme:
a method for preparing a food grade lipid pickering particle stable oil-in-water high internal phase emulsion comprising the steps of:
(1) Preparing lipid pickering particle dispersion liquid: heating and mixing high-melting-point solid fat, an emulsifying agent and distilled water to form a mixed solution, then shearing at high speed, dispersing by ultrasonic, rapidly cooling and storing, and standing to obtain lipid pickering particle dispersion liquid;
(2) Mixing the lipid Pickering particle dispersion liquid with vegetable oil, shearing at high speed, and rapidly cooling and storing to obtain the food-grade oil-in-water type high internal phase emulsion with stable lipid Pickering particles;
The mass concentration of the high melting point solid fat in the mixed solution in the step (1) is 0.5-5 wt%; the mass concentration of the emulsifier in the mixed solution is 0.1-3wt.%;
the high-melting-point solid lipid in the step (1) is lipid with a melting point of more than or equal to 42 ℃;
the volume ratio of the lipid pickering particle dispersion liquid to the vegetable oil in the step (2) is 10-30:70-90.
Preferably, the high melting point lipid is at least one of beeswax and palm stearin high melting point lipid; the emulsifier is at least one of sodium caseinate, tween 80 and Tween 40; the vegetable oil is at least one of rapeseed oil, corn oil and soybean oil low-melting-point edible vegetable oil.
Preferably, the high-melting-point fat fixing agent is beeswax, the emulsifying agent is sodium caseinate, and the vegetable oil is rapeseed oil.
Preferably, in the step (1), the heating and mixing means that the high-melting-point solid fat is melted first, and then the high-melting-point solid fat is mixed with the distilled water mixed with the emulsifying agent after being heated; the melting temperature is 70-85 ℃ and the melting time is 20-40min; the temperature of the heated distilled water is 70-85 ℃.
Preferably, the mixing in step (1) is stirring mixing; the stirring speed is 300-700rpm, and the stirring time is 20-30min; preferably, the high-speed shearing in the step (1) has a rotating speed of 10000-14000rpm and a shearing time of 30-90s.
Preferably, the power of the ultrasonic dispersion in the step (1) is 300-450W, and the ultrasonic time is 5-10min.
Preferably, the time of standing in the step (1) is more than or equal to 24 hours.
Preferably, the mass concentration of the high melting point solid fat in the mixed solution in the step (1) is 1-2wt.%, and the mass concentration of the emulsifier in the mixed solution is 0.5-2wt.%.
Preferably, the high-speed shearing in the step (2) has a rotating speed of 10000-14000rpm and a shearing time of 1-3min.
Preferably, the rapid cooling and storage temperatures in step (1) and step (2) are 4 ℃.
The second object of the invention is achieved by the following technical scheme:
an oil-in-water type high internal phase emulsion with stable food grade lipid Pickering granule is prepared by the above preparation method.
The third object of the invention is achieved by the following technical scheme:
use of food grade lipid pickering particles stable oil-in-water high internal phase emulsion is provided.
Preferably, the application is in particular in the fields of food, cosmetics and pharmaceuticals.
Compared with the prior art, the invention has the following advantages:
(1) The oil-in-water type high internal phase emulsion with stable food-grade lipid Pickering particles can be controllably self-assembled to oil/water surface to form single-layer or multi-layer fat crystallization interface film stable liquid drops by adopting solid lipid particles prepared by high melting point solid fat; the high internal phase emulsion with stable food-grade lipid pickering particles has an obvious interface structure for adsorbing the lipid pickering particles at an oil/water interface, and the prepared high internal phase emulsion has good stability within 1 month, is little influenced by environmental factors, and has wide application prospect in the fields of foods, medicines and cosmetics.
(2) The lipid pickering particles are formed by using the lipid serving as a natural food-grade ingredient, the preparation method is simple and mild in condition, the formula is green and safe, no toxic or harmful reagent is involved, the pickering particle stable high internal phase emulsion system is expanded, and large-scale production is easy to realize.
(3) The lipid pickering particles are formed by using the beeswax which is a natural food-grade ingredient, and the prepared food-grade lipid-based oil water-in-water type high internal phase pickering emulsion has good stability and high safety, and has wide application prospect in the food field.
Drawings
FIG. 1 is a process flow diagram of the preparation of the food grade lipid pickering particle stabilized oil-in-water high internal phase emulsion of the present invention;
FIG. 2 is a graph showing the appearance of the food grade lipid pickering particle stabilized oil-in-water high internal phase emulsions prepared in examples 1 to 6;
FIG. 3 is a graph showing the appearance of the food-grade lipid pickering particle-stabilized oil-in-water high internal phase emulsions prepared in examples 1 to 6 after standing at 4℃for 7 days;
FIG. 4 is a graph showing the appearance of the food-grade lipid pickering particle-stabilized oil-in-water high internal phase emulsions prepared in examples 1 to 6 after standing at 4℃for 1 month;
FIG. 5 is a micrograph of a food grade lipid Pickering particle stabilized oil-in-water high internal phase emulsion prepared in example 3 and example 4;
FIG. 6 is a micrograph and polarized view of a food grade lipid Pickering particle stabilized oil-in-water high internal phase emulsion prepared in example 2;
FIG. 7 is a micrograph and polarized view of a food grade lipid Pickering particle stabilized oil-in-water high internal phase emulsion prepared in example 4;
FIG. 8 is a micrograph and polarized view of a food grade lipid Pickering particle stabilized oil-in-water high internal phase emulsion prepared in example 5;
FIG. 9 is a graph showing the appearance effect of the food grade lipid pickering particle stabilized oil-in-water high internal phase emulsions prepared in comparative examples 1 to 4;
FIG. 10 is a micrograph and polarized view of a food grade lipid Pickering particle stabilized oil-in-water high internal phase emulsion prepared in comparative example 1;
FIG. 11 is a micrograph and polarized view of an oil-in-water type high internal phase emulsion stabilized with food grade lipid Pickering particles prepared in comparative example 4.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but embodiments of the present invention are not limited thereto. Unless otherwise indicated, the materials and instruments used in the examples below are commercially available, and a process flow diagram for preparing the food-grade lipid pickering particle-stabilized oil-in-water high internal phase emulsion of the present invention is shown in FIG. 1.
Example 1
A method for preparing a stable oil-in-water high internal phase emulsion of food grade lipid pickering particles, comprising the steps of:
(1) Preparation of a food-grade lipid pickering particle dispersion: mixing 1 part by mass of sodium caseinate and 17 parts by mass of distilled water, heating (heating and stirring at 80 ℃ for 30 min), mixing with 2 parts by mass of beeswax heated to be completely melted, heating and stirring at 80 ℃ for 30min, shearing at 14000rpm for 1min by a high-speed shearing machine, finally performing ultrasonic treatment at 350W for 7min by an ultrasonic device, rapidly cooling, and standing at 4 ℃ for 24h in a refrigerator to obtain a food-grade lipid pickering particle dispersion;
(2) Preparation of food-grade lipid pickering particle-stabilized oil-in-water high internal phase emulsion: 80 parts by volume of rapeseed oil was added to 20 parts by volume of lipid pickering particle dispersion, sheared at high speed at 14000rpm for 3min with a high speed shearing machine, then cooled rapidly and stored at 4 ℃ in a refrigerator to obtain lipid pickering particle stabilized oil-in-water type high internal phase emulsion.
The high internal phase emulsion prepared in this example was stored in a refrigerator at 4 ℃ for 24 hours, the whole system was semi-solid, and the emulsion could be inverted in the container without flowing, see fig. 2. Fig. 3 and 4 are graphs showing the appearance effects of the oil-in-water type high internal phase emulsion stabilized with the food-grade lipid pickering particles of this example after standing at 4 ℃ for 7 days and 1 month, respectively. The high internal phase emulsion prepared in this example was observed under a polarizing microscope, and as a control, the high internal phase emulsion (i.e., comparative example 1) with the added amount of beeswax of 1 was added to each oil droplet of the high internal phase emulsion with 2.0wt.% beeswax being completely encapsulated by the lipid particle. Stabilization of the high internal phase pickering emulsion requires that the particles adsorb to the surface of the droplets and form a dense interfacial film, and that the oil droplets are completely covered with a sufficient number of particles. The emulsion liquid drops are uniformly distributed, no coalescence phenomenon exists, and the system stability is good.
Example 2
A method for preparing a stable oil-in-water high internal phase emulsion of food grade lipid pickering particles, comprising the steps of:
(1) Preparation of a food-grade lipid pickering particle dispersion: mixing 2 parts by mass of sodium caseinate and 16 parts by mass of distilled water, heating (heating and stirring at 80 ℃ for 30 min), mixing the mixture with 2 parts by mass of beeswax heated to be completely melted, heating and stirring at 80 ℃ for 30min, shearing at 14000rpm for 1min by a high-speed shearing machine, finally performing ultrasonic treatment at 350W for 7min by an ultrasonic device, rapidly cooling, and standing at 4 ℃ for 24h in a refrigerator to obtain a food-grade lipid pickering particle dispersion;
(2) Preparation of food-grade lipid pickering particle-stabilized oil-in-water high internal phase emulsion: 80 parts by volume of rapeseed oil was added to 20 parts by volume of lipid pickering particle dispersion, sheared at high speed at 14000rpm for 3min with a high speed shearing machine, then cooled rapidly and stored at 4 ℃ in a refrigerator to obtain lipid pickering particle stabilized oil-in-water type high internal phase emulsion.
The high internal phase emulsion prepared in this example was stored in a refrigerator at 4 ℃ for 24 hours, the whole system was semi-solid, and the emulsion could be inverted in the container without flowing, see fig. 2. Fig. 3 and 4 are graphs showing the appearance effects of the oil-in-water type high internal phase emulsion stabilized with the food-grade lipid pickering particles of this example after standing at 4 ℃ for 7 days and 1 month, respectively. The high internal phase emulsion prepared in this example was observed under a polarizing microscope, and fig. 6 is a microscopic and polarizing image of the oil-in-water type high internal phase emulsion with stable food-grade lipid pickering particles prepared in this example; by contrast with the high internal phase emulsion with a beeswax addition of 1 (i.e. comparative example 1), the droplets of the high internal phase emulsion with 2.0wt.% beeswax and 2.0wt.% sodium caseinate were evenly distributed, more lipid pickering particles adsorbed at the oil/water interface, and strong interactions between the particles caused the emulsion to form a 3D network gel structure to effectively buffer the contact between droplets, preventing coalescence destabilization between droplets, while the excess particles increased the viscosity of the continuous phase in the continuous phase, enhancing system stability.
Example 3
A method for preparing a stable oil-in-water high internal phase emulsion of food grade lipid pickering particles, comprising the steps of:
(1) Preparation of a food-grade lipid pickering particle dispersion: mixing 2 parts by mass of sodium caseinate and 17 parts by mass of distilled water, heating (heating and stirring at 80 ℃ for 30 min), mixing with 1 part by mass of beeswax heated to be completely melted, heating and stirring at 80 ℃ for 30min, shearing at 14000rpm for 1min by a high-speed shearing machine, finally performing ultrasonic treatment at 350W for 7min by an ultrasonic device, rapidly cooling, and storing at 4 ℃ for 24h to obtain a food-grade lipid pickering particle dispersion;
(2) Preparation of food-grade lipid pickering particle-stabilized oil-in-water high internal phase emulsion: 80 parts by volume of rapeseed oil was added to 20 parts by volume of lipid pickering particle dispersion, sheared at high speed at 14000rpm for 3min with a high speed shearing machine, then cooled rapidly and stored at 4 ℃ in a refrigerator to obtain lipid pickering particle stabilized oil-in-water type high internal phase emulsion.
The high internal phase emulsion prepared in this example was stored in a refrigerator at 4 ℃ for 24 hours, the whole system was semi-solid, and the emulsion could be inverted in the container without flowing, see fig. 2. Fig. 3 and 4 are graphs showing the appearance effects of the oil-in-water type high internal phase emulsion stabilized with the food-grade lipid pickering particles of this example after standing at 4 ℃ for 7 days and 1 month, respectively. The high internal phase emulsion prepared in this example was observed under a polarizing microscope, and referring specifically to fig. 3 and 4, the high internal phase emulsion with 1 added sodium caseinate (i.e. comparative example 1) was used as a control, droplets of the high internal phase emulsion with 2.0wt.% sodium caseinate were closely packed with each other, and the typical bridging flocculation of pickering emulsions was also reflected, thus providing closer association between oil droplets in the microscopic aspect, resulting in a firmer network structure of the emulsion in the macroscopic aspect, and a more uniform whole emulsion.
Example 4
A method for preparing a stable oil-in-water high internal phase emulsion of food grade lipid pickering particles, comprising the steps of:
(1) Preparation of a food-grade lipid pickering particle dispersion: mixing 1 part by mass of sodium caseinate and 21 parts by mass of distilled water, heating (heating and stirring at 80 ℃ for 30 min), then mixing with 3 parts by mass of beeswax heated to be completely melted, heating and stirring at 80 ℃ for 30min, shearing at 14000rpm for 1min by a high-speed shearing machine, finally performing ultrasonic treatment at 350W power for 7min by an ultrasonic device, then performing rapid cooling and storing at 4 ℃ for 24h to obtain a food-grade lipid pickering particle dispersion;
(2) Preparation of food-grade lipid pickering particle-stabilized oil-in-water high internal phase emulsion: 75 parts by volume of rapeseed oil was added to 25 parts by volume of lipid pickering particle dispersion, sheared at high speed at 14000rpm for 3min with a high speed shearing machine, then cooled rapidly and stored at 4 ℃ in a refrigerator to obtain lipid pickering particle stabilized oil-in-water type high internal phase emulsion.
The high internal phase emulsion prepared in this example was stored in a refrigerator at 4 ℃ for 24 hours, the whole system was semi-solid, and the emulsion could be inverted in the container without flowing, see fig. 2. Fig. 3 and 4 are graphs showing the appearance effects of the oil-in-water type high internal phase emulsion stabilized with the food-grade lipid pickering particles of this example after standing at 4 ℃ for 7 days and 1 month, respectively. The high internal phase emulsion prepared in this example was observed under a polarizing microscope, and referring specifically to fig. 7, with reference to the high internal phase emulsion (i.e., comparative example 2) having an oil phase volume of 80%, droplets of the high internal phase emulsion having an oil phase volume of 75% were closely packed with each other, and each oil droplet was completely encapsulated with lipid particles.
Example 5
A method for preparing a stable oil-in-water high internal phase emulsion of food grade lipid pickering particles, comprising the steps of:
(1) Preparation of a food-grade lipid pickering particle dispersion: mixing 1 part by mass of sodium caseinate and 21 parts by mass of distilled water, heating (heating and stirring at 80 ℃ for 30 min), then mixing with 3 parts by mass of palm stearin which is heated to be completely melted, heating and stirring at 80 ℃ for 30min, shearing at 14000rpm for 1min by a high-speed shearing machine, finally performing ultrasonic treatment at 350W power for 7min by an ultrasonic device, then rapidly cooling and storing at 4 ℃ for 24h to obtain a food-grade lipid Pickering particle dispersion;
(2) Preparation of food-grade lipid pickering particle-stabilized oil-in-water high internal phase emulsion: 75 parts by volume of rapeseed oil was added to 25 parts by volume of lipid pickering particle dispersion, sheared at high speed at 14000rpm for 3min with a high speed shearing machine, then cooled rapidly and stored at 4 ℃ in a refrigerator to obtain lipid pickering particle stabilized oil-in-water type high internal phase emulsion.
The high internal phase emulsion prepared in this example was stored in a refrigerator at 4 ℃ for 24 hours, the whole system was semi-solid, and the emulsion could be inverted in the container without flowing, see fig. 2. Fig. 3 and 4 are graphs showing the appearance effects of the oil-in-water type high internal phase emulsion stabilized with the food-grade lipid pickering particles of this example after standing at 4 ℃ for 7 days and 1 month, respectively. The high internal phase emulsion prepared in this example was observed under a polarizing microscope, and referring specifically to fig. 8, the high internal phase emulsion (i.e. comparative example 1) with the beeswax added in an amount of 3.0wt.% was used as a control, and the droplets of the high internal phase emulsion with 3.0wt.% palm stearin were closely packed with each other, and the typical bridging flocculation of pickering emulsion was also reflected, thus providing closer bonding between the oil droplets in the microscopic aspect, resulting in a firmer network structure of the emulsion and a more uniform overall emulsion.
Example 6
A method for preparing a stable oil-in-water high internal phase emulsion of food grade lipid pickering particles, comprising the steps of:
(1) Preparation of a food-grade lipid pickering particle dispersion: mixing 2 parts by mass of sodium caseinate and 16 parts by mass of distilled water, heating (heating and stirring at 80 ℃ for 30 min), then mixing with 2 parts by mass of palm stearin which is heated to be completely melted, heating and stirring at 80 ℃ for 30min, shearing at 14000rpm for 1min by a high-speed shearing machine, finally carrying out ultrasonic treatment at 350W for 7min by an ultrasonic device, then rapidly cooling and standing at 4 ℃ for 24h in a refrigerator to obtain a food-grade lipid Pickering particle dispersion;
(2) Preparation of food-grade lipid pickering particle-stabilized oil-in-water high internal phase emulsion: 80 parts by volume of rapeseed oil was added to 20 parts by volume of lipid pickering particle dispersion, sheared at high speed at 14000rpm for 3min with a high speed shearing machine, then cooled rapidly and stored at 4 ℃ in a refrigerator to obtain lipid pickering particle stabilized oil-in-water type high internal phase emulsion.
The high internal phase emulsion prepared in this example was stored in a refrigerator at 4 ℃ for 24 hours, the whole system was semi-solid, and the emulsion could be inverted in the container without flowing, see fig. 2. Fig. 3 and 4 are graphs showing the appearance effects of the oil-in-water type high internal phase emulsion stabilized with the food-grade lipid pickering particles of this example after standing at 4 ℃ for 7 days and 1 month, respectively. The high internal phase emulsion prepared in this example was observed under a polarizing microscope, and the high internal phase emulsion (i.e., comparative example 3) with a beeswax addition of 1 was used as a control, and the high internal phase emulsion with 2.0wt.% of palm stearin and 2.0wt.% of sodium caseinate was added to have a uniform droplet distribution, more lipid pickering particles were adsorbed at the oil/water interface, and the strong interactions between the particles caused the emulsion to form a 3D network gel structure to effectively buffer the contact between the droplets, preventing coalescence destabilization between the droplets, while the excess particles increased the viscosity of the continuous phase in the continuous phase, enhancing the system stability.
Comparative example 1
An oil-in-water high internal phase emulsion stabilized by unstable food grade lipid pickering particles is prepared by:
(1) Preparation of a food-grade lipid pickering particle dispersion: mixing 1 part by mass of sodium caseinate and 18 parts by mass of distilled water, heating (heating and stirring at 80 ℃ for 30 min), then mixing with 1 part by mass of beeswax heated to be completely melted, heating and stirring at 80 ℃ for 30min, shearing at 14000rpm for 1min by a high-speed shearing machine, finally performing ultrasonic treatment at 350W power for 7min by an ultrasonic device, then performing rapid cooling and storing at 4 ℃ for 24h to obtain a food-grade lipid pickering particle dispersion;
(2) Preparation of food-grade lipid pickering particle-stabilized oil-in-water high internal phase emulsion: 80 parts by volume of rapeseed oil was added to 20 parts by volume of lipid pickering particle dispersion, sheared at high speed at 14000rpm for 3min with a high speed shearing machine, then cooled rapidly and stored at 4 ℃ in a refrigerator to obtain lipid pickering particle stabilized oil-in-water type high internal phase emulsion.
The high internal phase emulsion prepared in this comparative example was stored in a refrigerator at 4 ℃ for 24 hours, and the oil phase was precipitated in a small amount, and could not be in a semi-solid state of the high internal phase emulsion, as shown in fig. 9. The high internal phase emulsion prepared in this comparative example was observed under a polarizing microscope, and referring specifically to fig. 10, the lipid pickering particles with lower concentration were not in demand, the particles could not encapsulate the whole oil phase, and under the same shearing conditions, the oil phase could not be uniformly mixed into the system, so that the high internal phase emulsion could not exist stably.
Comparative example 2
An oil-in-water high internal phase emulsion stabilized by unstable food grade lipid pickering particles is prepared by:
(1) Preparation of a food-grade lipid pickering particle dispersion: mixing 1 part by mass of sodium caseinate and 16 parts by mass of distilled water, heating (heating and stirring at 80 ℃ for 30 min), then mixing with 3 parts by mass of beeswax heated to be completely melted, heating and stirring at 80 ℃ for 30min, shearing at 14000rpm for 1min by a high-speed shearing machine, finally performing ultrasonic treatment at 350W power for 7min by an ultrasonic device, then performing rapid cooling and storing at 4 ℃ for 24h to obtain a food-grade lipid pickering particle dispersion;
(2) Preparation of food-grade lipid pickering particle-stabilized oil-in-water high internal phase emulsion: 80 parts by volume of rapeseed oil was added to 20 parts by volume of lipid pickering particle dispersion, sheared at high speed at 14000rpm for 3min with a high speed shearing machine, then cooled rapidly and stored at 4 ℃ in a refrigerator to obtain lipid pickering particle stabilized oil-in-water type high internal phase emulsion.
The high internal phase emulsion prepared in this comparative example was stored in a refrigerator at 4 ℃ for 24 hours, and the emulsion was unstable. The high internal phase emulsion prepared in this comparative example was observed under a polarizing microscope, and the lipid pickering particles with higher concentration did not better encapsulate the droplets, but rather because of severe molecular agglomeration, the interfacial area occupied by its individual molecules was large, resulting in low interfacial adsorption, failure to form an effective barrier film, and failure to stabilize the emulsion, as shown in fig. 9. It can be seen that the higher the concentration of lipid pickering particles is not, the better the effect of stabilizing the high internal phase emulsion.
Comparative example 3
An oil-in-water high internal phase emulsion stabilized by unstable food grade lipid pickering particles is prepared by:
(1) Preparation of a food-grade lipid pickering particle dispersion: mixing 1 mass of sodium caseinate and 17 mass parts of distilled water, heating (heating and stirring at 80 ℃ for 30 min), then mixing with 2 mass parts of palm stearin which is heated to be completely melted, heating and stirring at 80 ℃ for 30min, shearing at 14000rpm for 1min by a high-speed shearing machine, finally performing ultrasonic treatment at 350W power for 7min by an ultrasonic device, then rapidly cooling and storing at 4 ℃ for 24h to obtain a food-grade lipid Pickering particle dispersion;
(2) Preparation of food-grade lipid pickering particle-stabilized oil-in-water high internal phase emulsion: 80 parts by volume of rapeseed oil was added to 20 parts by volume of lipid pickering particle dispersion, sheared at high speed at 14000rpm for 3min with a high speed shearing machine, then cooled rapidly and stored at 4 ℃ in a refrigerator to obtain lipid pickering particle stabilized oil-in-water type high internal phase emulsion.
The high internal phase emulsion prepared in this comparative example was stored in a refrigerator at 4 ℃ for 24 hours, and the emulsion was unstable, see fig. 9.
Comparative example 4
An oil-in-water high internal phase emulsion stabilized by unstable food grade lipid pickering particles is prepared by:
(1) Preparation of a food-grade lipid pickering particle dispersion: mixing and heating 2 parts by mass of Tween 80 and 16 parts by mass of distilled water (heating and stirring at 80 ℃ for 30 min), then mixing with 2 parts by mass of beeswax heated to be completely melted, heating and stirring at 80 ℃ for 30min, shearing at 14000rpm for 1min by a high-speed shearing machine, finally performing ultrasonic treatment at 350W power for 7min by an ultrasonic device, then performing rapid cooling and storing at 4 ℃ for 24h to obtain a food-grade lipid pickering particle dispersion;
(2) Preparation of food-grade lipid pickering particle-stabilized oil-in-water high internal phase emulsion: 80 parts by volume of rapeseed oil was added to 20 parts by volume of lipid pickering particle dispersion, sheared at high speed at 14000rpm for 3min with a high speed shearing machine, then cooled rapidly and stored at 4 ℃ in a refrigerator to obtain lipid pickering particle stabilized oil-in-water type high internal phase emulsion.
The high internal phase emulsion prepared in this comparative example was stored in a refrigerator at 4 ℃ for 24 hours, the emulsion was unstable, and the high internal phase emulsion prepared in this comparative example was observed under a polarizing microscope, see fig. 11.
From the above, from examples 1 to 6, comparative examples 1 to 4, it is known that the crystal form, morphology, size, concentration of the lipid pickering particles are several main factors affecting the stability of the high internal phase emulsion; the lipid Pickering particles with lower concentration are in short supply, the particles cannot wrap all the oil phase, and under the same shearing condition, the oil phase cannot be uniformly mixed into the system, so that the high internal phase emulsion cannot exist stably; the lipid Pickering particles with higher concentration do not better encapsulate the liquid drops, but because of the serious aggregation of molecules, the interface area occupied by single molecules is large, so that the interface adsorption is low, an effective barrier film cannot be formed, and the emulsion cannot be stabilized. It can be seen that the higher the concentration of lipid pickering particles is not, the better the effect of stabilizing the high internal phase emulsion.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principles of the present invention are equivalent.
Claims (5)
1. A method for preparing an oil-in-water type high internal phase emulsion with stable food grade lipid Pickering particles is characterized by comprising the following steps,
(1) Preparing lipid pickering particle dispersion liquid: heating and mixing high-melting-point solid fat, an emulsifying agent and distilled water to form a mixed solution, then shearing at high speed, dispersing by ultrasonic, rapidly cooling and storing, and standing to obtain lipid pickering particle dispersion liquid;
(2) Mixing the lipid Pickering particle dispersion liquid with vegetable oil, shearing at high speed, and rapidly cooling and storing to obtain the food-grade oil-in-water type high internal phase emulsion with stable lipid Pickering particles;
The mass concentration of the high melting point solid fat in the mixed solution in the step (1) is 0.5-5 wt%; the mass concentration of the emulsifier in the mixed solution is 0.1-3 wt%; the high melting point solid lipid is a lipid with a melting point of more than or equal to 42 ℃; the high melting point lipid is at least one of beeswax and palm stearin high melting point lipid;
In the step (1), the heating and mixing means that the high-melting-point solid fat is melted firstly, and then the high-melting-point solid fat is mixed with distilled water mixed with an emulsifying agent after being heated; the melting temperature is 70-85 ℃ and the melting time is 20-40 min; the temperature of the heated distilled water is 70-85 ℃;
The mixing in the step (1) is stirring mixing; the stirring speed is 300-700 rpm, and the stirring time is 20-30 min; the rotation speed of the high-speed shearing in the step (1) is 10000-14000 rpm, and the shearing time is 30-90 s;
The standing time in the step (1) is more than or equal to 24 h;
the volume ratio of the lipid pickering particle dispersion liquid to the vegetable oil in the step (2) is 10-30:70-90;
The emulsifier is sodium caseinate; the vegetable oil is rapeseed oil;
The rotation speed of the high-speed shearing in the step (2) is 10000-14000 rpm, and the shearing time is 1-3 min.
2. A process for the preparation of a food grade lipid pickering particle stable oil-in-water high internal phase emulsion according to claim 1, characterized in that: the power of the ultrasonic dispersion in the step (1) is 300-450W, and the ultrasonic time is 5-10 min.
3. A process for the preparation of a food grade lipid pickering particle stable oil-in-water high internal phase emulsion according to claim 1, characterized in that: the rapid cooling and storage temperatures in step (1) and step (2) were 4 ℃.
4. A food grade lipid pickering particle stable oil-in-water high internal phase emulsion prepared according to the method of any one of claims 1 to 3.
5. Use of the food grade lipid pickering particle stabilized oil-in-water high internal phase emulsion according to claim 4, characterized in that the food grade lipid pickering particle stabilized oil-in-water high internal phase emulsion is used in the food, cosmetic and pharmaceutical fields.
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