CN113892632B - Method for preparing Pickering emulsion by using modified glycinin micelles - Google Patents
Method for preparing Pickering emulsion by using modified glycinin micelles Download PDFInfo
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- 239000000839 emulsion Substances 0.000 title claims abstract description 89
- 239000000693 micelle Substances 0.000 title claims abstract description 65
- 108010083391 glycinin Proteins 0.000 title claims abstract description 58
- 238000000034 method Methods 0.000 title claims abstract description 33
- 230000004048 modification Effects 0.000 claims abstract description 35
- 238000012986 modification Methods 0.000 claims abstract description 35
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- 239000003921 oil Substances 0.000 claims abstract description 24
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- 239000002285 corn oil Substances 0.000 claims abstract description 14
- 235000005687 corn oil Nutrition 0.000 claims abstract description 14
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 14
- 239000000843 powder Substances 0.000 claims description 83
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 83
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 72
- 239000000523 sample Substances 0.000 claims description 39
- 238000003756 stirring Methods 0.000 claims description 35
- 239000012153 distilled water Substances 0.000 claims description 22
- 244000046052 Phaseolus vulgaris Species 0.000 claims description 21
- 235000010627 Phaseolus vulgaris Nutrition 0.000 claims description 21
- 230000008569 process Effects 0.000 claims description 18
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- 230000001105 regulatory effect Effects 0.000 claims description 15
- 239000006228 supernatant Substances 0.000 claims description 14
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- 229910021641 deionized water Inorganic materials 0.000 claims description 13
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- 230000001276 controlling effect Effects 0.000 claims description 12
- 238000007710 freezing Methods 0.000 claims description 12
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- HVYWMOMLDIMFJA-DPAQBDIFSA-N cholesterol Chemical compound C1C=C2C[C@@H](O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@H]([C@H](C)CCCC(C)C)[C@@]1(C)CC2 HVYWMOMLDIMFJA-DPAQBDIFSA-N 0.000 description 4
- 230000003247 decreasing effect Effects 0.000 description 4
- 108010044091 Globulins Proteins 0.000 description 3
- 102000006395 Globulins Human genes 0.000 description 3
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- 108010082495 Dietary Plant Proteins Proteins 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
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- 101710102211 11S globulin Proteins 0.000 description 1
- 206010003210 Arteriosclerosis Diseases 0.000 description 1
- 101710190853 Cruciferin Proteins 0.000 description 1
- DWAQJAXMDSEUJJ-UHFFFAOYSA-M Sodium bisulfite Chemical compound [Na+].OS([O-])=O DWAQJAXMDSEUJJ-UHFFFAOYSA-M 0.000 description 1
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Classifications
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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
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/03—Organic compounds
- A23L29/035—Organic compounds containing oxygen as heteroatom
- A23L29/04—Fatty acids or derivatives
-
- 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
- A23L11/00—Pulses, i.e. fruits of leguminous plants, for production of food; Products from legumes; Preparation or treatment thereof
- A23L11/05—Mashed or comminuted pulses or legumes; Products made therefrom
- A23L11/07—Soya beans, e.g. oil-extracted soya bean flakes
-
- 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
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/015—Inorganic compounds
-
- 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
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/03—Organic compounds
- A23L29/045—Organic compounds containing nitrogen as heteroatom
-
- 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
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
- A23L5/30—Physical treatment, e.g. electrical or magnetic means, wave energy or irradiation
-
- 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
- A23L5/00—Preparation or treatment of foods or foodstuffs, in general; Food or foodstuffs obtained thereby; Materials therefor
- A23L5/30—Physical treatment, e.g. electrical or magnetic means, wave energy or irradiation
- A23L5/32—Physical treatment, e.g. electrical or magnetic means, wave energy or irradiation using phonon wave energy, e.g. sound or ultrasonic waves
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
- Y02A40/90—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in food processing or handling, e.g. food conservation
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Inorganic Chemistry (AREA)
- Agronomy & Crop Science (AREA)
- Botany (AREA)
- Colloid Chemistry (AREA)
- Peptides Or Proteins (AREA)
Abstract
The invention discloses a method for preparing Pickering emulsion by using modified glycinin micelles, which combines heat treatment, ultrasonic treatment and pH shift treatment to prepare the modified glycinin micelles; corn oil and modified glycinin micelles were mixed according to an oil ratio of 80% to prepare a high internal phase Pickering emulsion. Compared with the prior art, the invention adopts a heating-ultrasonic-pH shift combined technology to modify glycinin, combines physical modification and chemical modification, so that the glycinin obtains nano-scale particle size, improves surface hydrophobicity and enhances emulsifying capacity; the high internal phase Pickering emulsion prepared from the particles and corn oil is stable to salt ions, heat treatment and polar acid and polar alkali environments (pH=2 and 8-10), has good edible safety and environmental compatibility, can be maintained for more than 180 days in an environment of 4 ℃, is a food-grade emulsion, and has a good prospect in the fields of carrying and embedding active substances, fat substitute production and the like.
Description
Technical Field
The invention relates to the technical field of Pickering emulsion preparation, in particular to a method for preparing Pickering emulsion by using modified glycinin micelles.
Background
Pickering emulsions refer to emulsions that are stabilized by solid particles adsorbed onto the interface of two mutually immiscible liquids by altering the steric hindrance or the rheological properties of the interface and the continuous phase. Compared with the traditional emulsion, the Pickering emulsion has the remarkable advantages that: (1) Using natural stabilizers of biological origin instead of inorganic surfactants; (2) Fluid properties can be altered by altering the oil phase composition or particle type; (3) The influence of temperature, ionic strength, acid-base, oil phase composition and the like on the emulsion is slowed down; (4) Excellent performance in carrying and releasing active substances, improving food quality, reducing calories, etc.; (5) has better environmental compatibility and edible safety.
Pickering emulsion with oil phase ratio more than or equal to 74% is called high internal phase Pickering emulsion (HIPEs), or super-concentrated emulsion or gel emulsion, has the property of solid-like, and has great application value in the fields of functional food production and the like. The HIPEs have lower water content, and can effectively inhibit bacterial growth, thereby obtaining longer shelf life.
Glycinin (SG), also known as 11S globulin, is a major vegetable protein and is widely used in the food industry. The acidic polypeptide and the alkaline polypeptide of the SG are connected through disulfide bonds, so that the SG has lower molecular flexibility, better thermal stability and emulsibility; the emulsion can be promoted to be formed by reducing the water-oil interfacial tension, and meanwhile, a film structure is formed at the water-oil interface, so that the emulsion is prevented from aggregation and flocculation; the subunits have high structural integrity and strong intramolecular interaction in the natural state, so the subunits are ideal raw materials for preparing Pickering emulsion.
SG has a compact molecular structure in a natural state, and most active groups are wrapped in the spherical structure, so that the application of SG in foods is limited. And proper heat treatment can destroy the structure of the protein, so that the protein conformation is stretched, and the aggregation state and the functional property of SG are improved. The cavitation effect and the microbeam effect of the ultrasound can break peptide bonds of the SG heat aggregate, expose hydrophilic groups and increase hydration between protein molecules and water molecules, so that the heat-induced gel property, the emulsifying property and the solubility of the SG heat aggregate are further improved. The pH shift treatment is typically performed at a pH of 12 for 1 hour, so that the secondary structure of the protein is maintained and a part of the tertiary structure is developed, exhibiting a Molten Globular (MG) structure; the protein is then refolded by adjusting the pH back to neutral. During this process the SG subunit dissociates and the specific group is further exposed. When heat, ultrasound and pH shift are combined, some desirable structural and functional properties are also produced.
In summary, the invention combines physical modification and chemical modification methods by taking the soybean globulin with rich nutrition as a raw material, and develops a method for preparing Pickering emulsion by using modified soybean globulin micelles, and the prepared emulsion has the characteristics of long stability period and edible safety.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a method for preparing a high-internal-phase Pickering emulsion with high stability by using modified glycinin micelles.
In order to achieve the above purpose, the invention is implemented according to the following technical scheme:
a first object of the present invention is to provide a method for preparing a Pickering emulsion using modified glycinin micelles, comprising the steps of:
s1, extracting glycinin and preparing modified glycinin micelles;
s2, mixing corn oil with modified glycinin micelles to prepare the high internal phase Pickering emulsion.
Further, the step S1 specifically includes:
s11, preparing glycinin powder by taking soybean meal as a raw material; firstly, grinding soybean meal into soybean meal powder, and sieving the soybean meal powder with a 100-mesh sieve to obtain fine powder; thoroughly mixing soybean meal powder with distilled water according to a ratio of 1g to 15mL, adjusting the pH of the suspension to 7.5 by using 1mol/L NaOH, and stirring for 2h at room temperature; centrifuging to obtain supernatant;adding NaHSO with a final concentration of 1.04g/L into the supernatant 3 Stirring uniformly, standing for 30min, and regulating the pH to 6.4; hydrating in a refrigerator at 4deg.C for 16 hr, centrifuging for 20min, dissolving the precipitate in distilled water, regulating pH to 7.5, dialyzing for 48 hr, and controlling ambient temperature below 4deg.C by ice box; pre-freezing at-80deg.C, and lyophilizing for 48 hr to obtain glycinin powder;
s12, adding the glycinin powder into deionized water, stirring for 2 hours at room temperature, and placing into a refrigerator at 4 ℃ for hydration overnight to enable the glycinin powder to be fully dissolved; centrifuging to remove the incompletely dissolved part to obtain glycinin solution, and respectively carrying out combined modification on the glycinin solution through heating treatment, ultrasonic treatment and pH deviation treatment to obtain modified glycinin micelles; the heating treatment process comprises the following steps: heating glycinin solution in 95deg.C water bath for 5-30min, immediately taking out, placing in ice box, and cooling to room temperature; the ultrasonic treatment process comprises the following steps: the probe of the ultrasonic cell disruption instrument is stretched into the central depth of the glycinin solution, and is treated for 0-12min with 0-70% amplitude under the conditions of rated power of 750W and output frequency of 20kHz, and the temperature of a sample is controlled below 25 ℃ by using an ice bath in the whole ultrasonic process; the pH shift treatment comprises the following steps: the pH of the glycinin solution was adjusted to 12 with 1mol/L NaOH, stirred slowly at room temperature for 1h, and then the pH of the glycinin solution was adjusted back to 7.0 with 1mol/L HCl and maintained for 1h.
Further, the step S2 specifically includes:
mixing corn oil and modified glycinin micro-particles with the concentration of 1-5% according to 65-85% of the oil, placing under an IKA homogenizer probe for high-speed dispersion treatment, homogenizing at 12800rpm for 2min for 15s, and obtaining Pickering emulsion.
Preferably, the modification sequence of the glycinin solution in the step S12 is as follows: heating, then ultrasonic treatment and finally pH shift treatment.
Preferably, the heating time for the combined modification of the glycinin solution in the step S12 is 20min 19S.
Preferably, the ultrasonic amplitude of the combined modification of the glycinin solution in the step S12 is 43%.
Preferably, the ultrasonic time for the combined modification of the glycinin solution in the step S12 is 5min 17S.
Preferably, the protein concentration used in step S2 to prepare the Pickering emulsion by combining the modified glycinin micelles with corn oil is 4%.
Preferably, the oil used to prepare the Pickering emulsion in step S2 in combination with the modified glycinin micelles is 80% oil.
A second object of the present invention is to provide an edible Pickering emulsion that is stable to salt ions, heat treatment, polar acid and polar base (ph=2/8-10) prepared by the method of preparing Pickering emulsion using modified glycinin micelles.
Compared with the prior art, the invention has the following advantages:
1. the invention adopts a heating-ultrasonic-pH shift combined technology to modify glycinin, and combines physical modification and chemical modification. The glycinin obtains nano-scale particle size, and the surface hydrophobicity is enhanced, so that the glycinin is more suitable for the production of Pickering emulsion.
2. The glycinin used in the invention is an important vegetable protein source, has high nutritive value, good amphipathy and strong emulsifying capacity, and can replace a surfactant to prepare edible high internal phase Pickering emulsion. The content of unsaturated fatty acid in the corn oil is up to 80% -85%. Does not contain cholesterol, has dissolving effect on accumulation of cholesterol in blood, and has positive preventing and treating effects on senile diseases such as arteriosclerosis, diabetes, etc.
3. The invention provides a preparation method of food-grade internal phase Pickering emulsion, which is simple and convenient to operate, environment-friendly, nontoxic and low in cost, and is suitable for industrial production.
4. The soybean globulin micelles modified by the combination of heat treatment, ultrasonic treatment and pH shift treatment have the characteristics of high nutritive value, strong emulsifying capacity and the like, and the high internal phase Pickering emulsion prepared from the particles and corn oil has good edible safety and environmental compatibility, can be maintained for more than 180 days in an environment of 4 ℃, is a food-grade emulsion, and has a prospect in the fields of carrying and embedding active substances, fat substitute production and the like.
Drawings
FIG. 1 is a graph showing the effect of different modification sequences provided in example 1 of the present invention on particle size of SG micelles modified by heat-ultrasonic-pH shift combination.
FIG. 2 is a graph showing the effect of different modification sequences provided in example 1 of the present invention on the potential of SG micelles modified by a combination of heat-ultrasonic-pH shift.
FIG. 3 is a graph showing the effect of different modification sequences provided in example 1 of the present invention on the hydrophobicity of the surface of SG micelles by heat-ultrasonic-pH shift combined modification.
FIG. 4 is a graph showing the effect of different modification sequences provided in example 1 of the present invention on the change in appearance of heat-ultrasonic-pH shift combined modified SG micelles.
FIG. 5 is a graph showing the effect of different heating times on particle size of SG micelles modified by a combination of heat-ultrasonic-pH shift, as provided in example 2 of the present invention.
FIG. 6 is a graph showing the effect of different heating times on the potential of heat-ultrasonic-pH shift combined modified SG micelles provided in example 2 of the present invention.
FIG. 7 is a graph showing the effect of different heating times on the hydrophobicity of the surface of SG micelles modified by the combination of heat-ultrasonic-pH shift, as provided in example 2 of the present invention.
FIG. 8 is a graph showing the effect of different heating times on the change in appearance of heat-ultrasonic-pH shift combined modified SG micelles provided in example 2 of the present invention.
FIG. 9 is a graph showing the effect of different ultrasonic amplitudes on particle size of SG micelles modified by a combination of heat-ultrasonic-pH shift, as provided in example 3 of the present invention.
FIG. 10 is a graph showing the effect of different ultrasonic amplitudes on the potential of heat-ultrasonic-pH shift combined modified SG micelles provided in example 3 of the present invention.
FIG. 11 is a graph showing the effect of different ultrasonic amplitudes on the hydrophobicity of the surface of SG micelles modified by the combination of heat-ultrasonic-pH shift, provided in example 3 of the present invention.
FIG. 12 is a graph showing the effect of different ultrasonic amplitudes on the change in appearance of heat-ultrasonic-pH shift combined modified SG micelles provided in example 3 of the present invention.
FIG. 13 is a graph showing the effect of different ultrasonic times on particle size of SG micelles modified by a combination of heat-ultrasonic-pH shift, as provided in example 4 of the present invention.
FIG. 14 is a graph showing the effect of different ultrasonic time on the potential of heat-ultrasonic-pH shift combined modified SG micelles provided in example 4 of the present invention.
FIG. 15 is a graph showing the effect of different ultrasonic times on the hydrophobicity of the surface of SG micelles modified by the combination of heat-ultrasonic-pH shift, provided in example 4 of the present invention.
FIG. 16 is a graph showing the effect of different ultrasonic times on the change in appearance of heat-ultrasonic-pH shift combined modified SG micelles provided in example 4 of the present invention.
FIG. 17 is a graph showing the effect of different protein concentrations on the particle size of a high internal phase Pickering emulsion prepared from heat-ultrasonic-pH shift combined modified SG micelles provided in example 5 of the present invention.
FIG. 18 is a graph showing the effect of different protein concentrations on the emulsifying activity of a high internal phase Pickering emulsion prepared from heat-ultrasonic-pH shift combined modified SG micelles according to example 5 of the present invention.
FIG. 19 is a graph showing the effect of different protein concentrations on the emulsion stability of a high internal phase Pickering emulsion prepared from heat-ultrasonic-pH shift combined modified SG micelles provided in example 5 of the present invention.
FIG. 20 is a graph showing the effect of different protein concentrations on the storage modulus and loss modulus of a high internal phase Pickering emulsion prepared from heat-ultrasonic-pH shift combined modified SG micelles provided in example 5 of the present invention.
FIG. 21 is a graph showing the effect of different protein concentrations on the viscosity of a high internal phase Pickering emulsion prepared from heat-ultrasonic-pH shift-modified SG micelles in accordance with example 6 of the present invention.
FIG. 22 is a graph showing the effect of different protein concentrations on the change in appearance of a high internal phase Pickering emulsion prepared from heat-ultrasonic-pH shift-modified SG micelles in accordance with example 6 of the present invention.
Fig. 23 is a graph showing the effect of different oil phases provided in example 7 of the present invention on the particle size of a high internal phase Pickering emulsion prepared from heat-ultrasonic-pH shift combined modified SG micelles.
Fig. 24 is a graph showing the effect of different oil phases provided in example 7 of the present invention on the emulsification activity of a high internal phase Pickering emulsion prepared from heat-ultrasonic-pH shift combined modified SG micelles.
Fig. 25 is a graph showing the effect of different oil phases provided in example 7 of the present invention on the emulsion stability of a high internal phase Pickering emulsion prepared from heat-ultrasonic-pH shift combined modified SG micelles.
FIG. 26 is a graph showing the effect of different oil phases provided in example 7 of the present invention on the storage modulus and loss modulus of a high internal phase Pickering emulsion prepared from heat-ultrasonic-pH shift combined modified SG micelles.
FIG. 27 is a graph showing the effect of different oil phases provided in example 7 of the present invention on the viscosity of a high internal phase Pickering emulsion prepared from heat-ultrasonic-pH shift-modified SG micelles.
Fig. 28 is a graph showing the effect of different oil phases provided in example 7 of the present invention on the change in appearance of a high internal phase Pickering emulsion prepared from heat-ultrasonic-pH shift combined modified SG micelles.
Fig. 29 is a graph showing the effect of different pH on the change in appearance of a high internal phase Pickering emulsion prepared from heat-ultrasonic-pH shift combined modified SG micelles provided in example 8 of the present invention.
FIG. 30 is a graph showing the effect of different ion concentrations on the change in appearance of a high internal phase Pickering emulsion prepared from heat-ultrasonic-pH shift combined modified SG micelles provided in example 9 of the present invention.
FIG. 31 is a graph showing the effect of different temperatures on the change in appearance of a high internal phase Pickering emulsion prepared from heat-ultrasonic-pH shift-modified SG micelles in accordance with example 10 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. The specific embodiments described herein are for purposes of illustration only and are not intended to limit the invention.
Example 1
Firstly, grinding bean pulp into powder, sieving with 100 mesh sieveObtaining fine powder; thoroughly mixing bean powder with distilled water at a ratio of 1:15 (g/mL), adjusting the pH of the suspension to 7.5 with 1mol/L NaOH, and stirring at room temperature for 2h; centrifuging for 30min (9000 g, 4deg.C), and keeping supernatant; naHSO with a final concentration of 1.04g/L was added 3 Stirring uniformly, standing for 30min, and regulating the pH to 6.4; hydrating in a refrigerator at 4deg.C for 16 hr, centrifuging for 20min (6500 g, 4deg.C), dissolving the precipitate in distilled water completely, adjusting pH to 7.5, dialyzing for 48 hr, and controlling ambient temperature below 4deg.C by ice box; pre-freezing at-80 deg.c, and freeze drying for 48 hr to obtain SG powder.
Adding deionized water into appropriate amount of SG powder, stirring at room temperature for 2h, and placing into a refrigerator at 4 ℃ for hydration overnight to enable the SG powder to be fully dissolved; the insoluble fraction was removed by centrifugation for 20min (8000 g,4 ℃) and the protein content was determined by the Bradford method, diluted appropriately to a final concentration of 2mg/mL. First, treatment conditions of Heating (H), ultrasonic treatment (U), pH shift treatment (pH, P) are set to be: 95-30 min, 750W-20kHz-40% amplitude-6 min, pH=12 for 1h, and setting 6 different modification sequences (HUP, HPU, UHP, UPH, PHU, PUH) to respectively carry out joint modification. Notice that: immediately taking out the sample after the heating treatment, placing the sample in an ice box, and cooling the sample to room temperature; in the ultrasonic process, an ultrasonic cell breaker probe extends into the central depth of SG solution, and in the whole ultrasonic process, the temperature of a sample is controlled below 25 ℃ by using an ice bath; the SG solution was adjusted to pH 12 with 1mol/L NaOH, stirred slowly at room temperature for 1h, and the pH of the system was adjusted back to 7.0 with 1mol/L HCl and maintained for 1h.
As shown in fig. 1-4, under the same modification conditions, different modification sequences can have certain influence on the average particle size, potential, surface hydrophobicity and appearance change of the combined modified SG micelles; the HUP sample has the best storage stability and the greatest surface hydrophobicity.
Example 2
Firstly, grinding bean pulp into powder, and sieving the powder with a 100-mesh sieve to obtain fine powder; thoroughly mixing bean powder with distilled water at a ratio of 1:15 (g/mL), adjusting the pH of the suspension to 7.5 with 1mol/L NaOH, and stirring at room temperature for 2h; centrifuging for 30min (9000 g, 4deg.C), and keeping supernatant; naHSO with a final concentration of 1.04g/L was added 3 Stirring uniformly, standing for 30min, and regulating the pH to 6.4; hydrating in a refrigerator at 4deg.C for 16 hr, centrifuging for 20min (6500 g, 4deg.C), dissolving the precipitate in distilled water completely, adjusting pH to 7.5, dialyzing for 48 hr, and controlling ambient temperature below 4deg.C by ice box; pre-freezing at-80 deg.c, and freeze drying for 48 hr to obtain SG powder.
Adding deionized water into appropriate amount of SG powder, stirring at room temperature for 2h, and placing into a refrigerator at 4 ℃ for hydration overnight to enable the SG powder to be fully dissolved; the insoluble fraction was removed by centrifugation for 20min (8000 g,4 ℃) and the protein content was determined by the Bradford method, diluted appropriately to a final concentration of 2mg/mL. The preferred modification sequence HUP is selected for joint modification. Firstly, the SG solution is heated in a water bath at 95 ℃ for 5-30min, and is immediately taken out and placed in an ice box to be cooled to room temperature after finishing. The ultrasonic cell disruption instrument probe is extended into the central depth of SG solution, and is processed for 6min at 40% amplitude under the condition of rated power of 750W and output frequency of 20 kHz; in the whole ultrasonic process, the temperature of the sample is controlled below 25 ℃ by using an ice bath. The SG solution was adjusted to pH 12 with 1mol/L NaOH, stirred slowly at room temperature for 1h, the pH of the system was adjusted back to 7.0 with 1mol/L HCl, and maintained for 1h.
As shown in fig. 5 to 8, the particle size, the absolute value of the electric potential and the surface hydrophobicity of the combined modified SG micelles all show a tendency to increase and decrease with the increase of the heating time, and the particle size of the sample is minimum, the electric potential and the surface hydrophobicity are maximum and the storage stability is the best when the heating time is 20 min.
Example 3
Firstly, grinding bean pulp into powder, and sieving the powder with a 100-mesh sieve to obtain fine powder; thoroughly mixing bean powder with distilled water at a ratio of 1:15 (g/mL), adjusting the pH of the suspension to 7.5 with 1mol/L NaOH, and stirring at room temperature for 2h; centrifuging for 30min (9000 g, 4deg.C), and keeping supernatant; naHSO with a final concentration of 1.04g/L was added 3 Stirring uniformly, standing for 30min, and regulating the pH to 6.4; hydrating in a refrigerator at 4deg.C for 16 hr, centrifuging for 20min (6500 g, 4deg.C), dissolving the precipitate in distilled water completely, adjusting pH to 7.5, dialyzing for 48 hr, and controlling ambient temperature below 4deg.C by ice box; pre-freezing at-80 deg.c, and freeze drying for 48 hr to obtain SG powder.
Adding deionized water into appropriate amount of SG powder, stirring at room temperature for 2h, and placing into a refrigerator at 4 ℃ for hydration overnight to enable the SG powder to be fully dissolved; the insoluble fraction was removed by centrifugation for 20min (8000 g,4 ℃) and the protein content was determined by the Bradford method, diluted appropriately to a final concentration of 2mg/mL. The preferred modification sequence HUP and the preferred heating time of 20min are selected for the combined modification. The SG solution was first heated in a 95℃water bath for 20min, immediately after the end, taken out and placed in an ice box to cool to room temperature. The ultrasonic cell disruption instrument probe is extended into the central depth of SG solution, and is processed for 6min with 0-70% amplitude under the condition of rated power 750W and output frequency 20 kHz; in the whole ultrasonic process, the temperature of the sample is controlled below 25 ℃ by using an ice bath. The SG solution was adjusted to pH 12 with 1mol/LNaOH, stirred slowly at room temperature for 1h, the pH of the system was adjusted back to 7.0 with 1mol/L HCl, and maintained for 1h.
As shown in fig. 9-12, the lower amplitude ultrasonic treatment (40%) significantly reduced SG particle size, probably due to cavitation caused by ultrasonic waves and physical effects caused by microbeam effects breaking the noncovalent interactions between protein molecules, and as the ultrasonic power increases, SG particle size increases again, indicating that SG re-aggregates to form small polymers; the effective surface charge of SG can be changed by ultrasonic treatment, the potential absolute value of a sample shows a trend of increasing and then decreasing along with the increase of ultrasonic power, namely electrostatic repulsive force is increased and then decreased, because the charged groups of SG are exposed on the surface of molecules under the action of ultrasonic waves, the potential absolute value is increased, and as the ultrasonic power is increased, proteins are excessively denatured and aggregated, and the charged groups are hidden in the protein molecules; the relative fluorescence intensity of SG micelles increases and decreases with increasing ultrasonic power, and the fluorescence intensity reaches the maximum when the ultrasonic amplitude is 40%, because many hydrophobic groups of SG are embedded inside the molecules, so that the hydrophobicity of proteins is low, hydrophobic groups of SG are exposed and hydrophobicity increases when the SG is subjected to ultrasonic treatment, but as the ultrasonic power increases further, high-energy ultrasonic waves cause part of protein molecules to aggregate, so that the hydrophobicity decreases. At an ultrasonic amplitude of 40%, the particle size of the sample is smallest, the absolute value of the electric potential and the surface hydrophobicity are largest, and the storage stability is best.
Example 4
Firstly, grinding bean pulp into powder, and sieving the powder with a 100-mesh sieve to obtain fine powder; thoroughly mixing bean powder with distilled water at a ratio of 1:15 (g/mL), adjusting the pH of the suspension to 7.5 with 1mol/L NaOH, and stirring at room temperature for 2h; centrifuging for 30min (9000 g, 4deg.C), and keeping supernatant; adding NaHSO3 with the final concentration of 1.04g/L, uniformly stirring, standing for 30min, and regulating the pH value to 6.4; hydrating in a refrigerator at 4deg.C for 16 hr, centrifuging for 20min (6500 g, 4deg.C), dissolving the precipitate in distilled water completely, adjusting pH to 7.5, dialyzing for 48 hr, and controlling ambient temperature below 4deg.C by ice box; pre-freezing at-80 deg.c, and freeze drying for 48 hr to obtain SG powder.
Adding deionized water into appropriate amount of SG powder, stirring at room temperature for 2h, and placing into a refrigerator at 4 ℃ for hydration overnight to enable the SG powder to be fully dissolved; the insoluble fraction was removed by centrifugation for 20min (8000 g,4 ℃) and the protein content was determined by the Bradford method, diluted appropriately to a final concentration of 2mg/mL. The preferred modification sequence HUP, the preferred heating time of 20min, and the preferred ultrasonic amplitude of 40% are selected for joint modification. The SG solution was first heated in a 95℃water bath for 20min, immediately after the end, taken out and placed in an ice box to cool to room temperature. The ultrasonic cell disruption instrument probe is extended into the central depth of SG solution, and is processed for 0-12min at the rated power of 750W and the output frequency of 20kHz and with the amplitude of 40%; in the whole ultrasonic process, the temperature of the sample is controlled below 25 ℃ by using an ice bath. The SG solution was adjusted to pH 12 with 1mol/L NaOH, stirred slowly at room temperature for 1h, the pH of the system was adjusted back to 7.0 with 1mol/L HCl, and maintained for 1h.
As shown in fig. 13 to 16, the particle size of SG micelles tends to decrease and then increase with the increase of the ultrasonic time, and the phenomenon that the particle size increases due to the long-time ultrasonic treatment is called "oversreatment", similar to the influence of ultrasonic power on the particle size of SG; the absolute value of the potential of SG micelles tends to increase and decrease with the increase of ultrasound time. When the ultrasonic time is 6min, the particle size of the sample is minimum, the absolute value of the potential and the surface hydrophobicity are maximum, and the storage stability is best.
Example 5
Firstly, grinding bean pulp into powder, and sieving the powder with a 100-mesh sieve to obtain fine powder; bean flour is added into the mixtureDistilled water 1:15 (g/mL) was thoroughly mixed, the pH of the suspension was adjusted to 7.5 with 1mol/L NaOH, and stirred at room temperature for 2h; centrifuging for 30min (9000 g, 4deg.C), and keeping supernatant; naHSO with a final concentration of 1.04g/L was added 3 Stirring uniformly, standing for 30min, and regulating the pH to 6.4; hydrating in a refrigerator at 4deg.C for 16 hr, centrifuging for 20min (6500 g, 4deg.C), dissolving the precipitate in distilled water completely, adjusting pH to 7.5, dialyzing for 48 hr, and controlling ambient temperature below 4deg.C by ice box; pre-freezing at-80 deg.c, and freeze drying for 48 hr to obtain SG powder.
Adding deionized water into appropriate amount of SG powder, stirring at room temperature for 2h, and placing into a refrigerator at 4 ℃ for hydration overnight to enable the SG powder to be fully dissolved; the insoluble fraction was removed by centrifugation for 20min (8000 g,4 ℃) and the protein content was determined by the Bradford method, diluted appropriately to a final concentration of 2mg/mL. The modification conditions of the joint modification were optimized by using a response surface analysis method, the response surface design factors and levels are shown in table 1, and the response values of the response surface test design and the surface hydrophobicity are shown in table 2. The SG solution is heated in a water bath at 95 ℃ for 15-30min, immediately taken out and placed in an ice box to be cooled to room temperature. The ultrasonic cell disruption instrument probe is extended into the central depth of SG solution, and is processed for 3-9min with 30-50% amplitude under the condition of rated power 750W and output frequency 20 kHz; in the whole ultrasonic process, the temperature of the sample is controlled below 25 ℃ by using an ice bath. The SG solution was adjusted to pH 12 with 1mol/L NaOH, stirred slowly at room temperature for 1h, the pH of the system was adjusted back to 7.0 with 1mol/L HCl, and maintained for 1h.
TABLE 1
TABLE 2
In table 2, a represents heating time, B represents ultrasonic amplitude, C represents ultrasonic power, and Y represents a surface hydrophobicity response value of a corresponding number of samples.
Performing multiple regression fitting on the test result and each factor to obtain a final regression equation: y= 3458.95-168.61a+143.37b-108.12C-14.06AB-65.12ac+75.77bc-269.36a 2 -230.90B 2 -143.58C 2 。
The combined modification conditions of the heating treatment, the ultrasonic treatment and the pH shift treatment obtained by the response surface analysis method are as follows: heating for 95-20 min 19s; ultrasonic 750W-20kHz-43% amplitude-5 min 17s; ph=12 treatment for 1h.
Example 6
Firstly, grinding bean pulp into powder, and sieving the powder with a 100-mesh sieve to obtain fine powder; thoroughly mixing bean powder with distilled water at a ratio of 1:15 (g/mL), adjusting the pH of the suspension to 7.5 with 1mol/L NaOH, and stirring at room temperature for 2h; centrifuging for 30min (9000 g, 4deg.C), and keeping supernatant; naHSO with a final concentration of 1.04g/L was added 3 Stirring uniformly, standing for 30min, and regulating the pH to 6.4; hydrating in a refrigerator at 4deg.C for 16 hr, centrifuging for 20min (6500 g, 4deg.C), dissolving the precipitate in distilled water completely, adjusting pH to 7.5, dialyzing for 48 hr, and controlling ambient temperature below 4deg.C by ice box; pre-freezing at-80 deg.c, and freeze drying for 48 hr to obtain SG powder.
Adding deionized water into appropriate amount of the SG powder, stirring at room temperature for 2h, and placing into a refrigerator at 4 ℃ for hydration overnight to enable the SG powder to be fully dissolved. The SG solution of 1% -5% was subjected to a joint modification by selecting the preferred modification sequence HUP, preferably heating time 20min 19s, preferably ultrasonic amplitude 43% and preferably ultrasonic time 5min 17s. The SG solution was first heated in a 95℃water bath for 20min 19s, immediately after the end, removed and placed in an ice box to cool to room temperature. The ultrasonic cell disruption instrument probe is extended into the central depth of SG solution, and is processed for 5min 17s at the rated power of 750W and the output frequency of 20kHz with the amplitude of 43 percent; in the whole ultrasonic process, the temperature of the sample is controlled below 25 ℃ by using an ice bath. The SG solution was adjusted to pH 12 with 1mol/L NaOH, stirred slowly at room temperature for 1h, the pH of the system was adjusted back to 7.0 with 1mol/L HCl, and maintained for 1h.
And (3) treating the SG solution with the protein concentration of 1% -5%, obtaining modified SG micelles by using the heating-ultrasonic-pH shift combined modification method, adding corn oil with the oil phase ratio of 75% as a fixed value, placing the oil-water mixed solution under an IKA homogenizer probe for high-speed dispersion treatment, homogenizing for 2min 15s at 12800rpm, and preparing the Pickering emulsion.
17-22, pickering emulsion particle size showed a decreasing trend with increasing protein concentration, which also reflects that increasing particle concentration can stabilize larger interfacial area; emulsion stability tends to increase with increasing protein concentration, indicating that the ability of the emulsion to remain stable is also enhanced; as the protein concentration increases, the storage modulus of Pickering emulsion increases with it and each storage modulus is much greater than the loss modulus; the viscosity of Pickering emulsion increases with increasing protein concentration; the Pickering emulsion has no obvious change after 180 days of storage, which indicates that the emulsion is stable in coagulation during storage, and the emulsion has high coagulation stability. The protein concentration was chosen to be 4% by comprehensive consideration.
Example 7
Firstly, grinding bean pulp into powder, and sieving the powder with a 100-mesh sieve to obtain fine powder; thoroughly mixing bean powder with distilled water (1:15) (g/mL), regulating pH of the suspension to 7.5 with 1mol/L NaOH, and stirring at room temperature for 2h; centrifuging for 30min (9000 g, 4deg.C), and keeping supernatant; naHSO with a final concentration of 1.04g/L was added 3 Stirring uniformly, standing for 30min, and regulating the pH to 6.4; hydrating in a refrigerator at 4deg.C for 16 hr, centrifuging for 20min (6500 g, 4deg.C), dissolving the precipitate in distilled water completely, adjusting pH to 7.5, dialyzing for 48 hr, and controlling ambient temperature below 4deg.C by ice box; pre-freezing at-80 deg.c, and freeze drying for 48 hr to obtain SG powder.
Adding deionized water into appropriate amount of the SG powder, stirring at room temperature for 2h, and placing into a refrigerator at 4 ℃ for hydration overnight to enable the SG powder to be fully dissolved. The preferred modification sequence HUP, the preferred heating time of 20min 19s, the preferred ultrasound amplitude of 43%, the preferred ultrasound time of 5min 17s, the preferred protein concentration of 4% were chosen. The SG solution was first heated in a 95℃water bath for 20min 19s, immediately after the end, removed and placed in an ice box to cool to room temperature. The ultrasonic cell disruption instrument probe is extended into the central depth of SG solution, and is processed for 5min 17s at the rated power of 750W and the output frequency of 20kHz with the amplitude of 43 percent; in the whole ultrasonic process, the temperature of the sample is controlled below 25 ℃ by using an ice bath. The SG solution was adjusted to pH 12 with 1mol/L NaOH, stirred slowly at room temperature for 1h, the pH of the system was adjusted back to 7.0 with 1mol/L HCl, and maintained for 1h.
Selecting SG solution with optimal protein concentration of 4%, treating by using the heating-ultrasonic-pH shift combined modification method to obtain modified SG micelles, adding corn oil with oil content of 65-85%, placing the oil-water mixed solution under an IKA homogenizer probe for high-speed dispersion treatment, homogenizing at 12800rpm for 2min for 15s, and preparing Pickering emulsion.
As shown in fig. 23-28, with the increase of the oil phase ratio, the particle size, the emulsifying activity, the emulsifying stability, the viscosity and the storage modulus of the Pickering emulsion all show a trend of decreasing first and then increasing, and no obvious change occurs after 180 days of storage, which indicates that the Pickering emulsion is stable in coagulation during storage, and the emulsion has good stability. When the oil phase ratio is 80%, the Pickering emulsion has the advantages of minimum particle size, highest emulsion stability, highest viscosity and maximum storage modulus.
Example 8
Firstly, grinding bean pulp into powder, and sieving the powder with a 100-mesh sieve to obtain fine powder; thoroughly mixing bean powder with distilled water at a ratio of 1:15 (g/mL), adjusting the pH of the suspension to 7.5 with 1mol/L NaOH, and stirring at room temperature for 2h; centrifuging for 30min (9000 g, 4deg.C), and keeping supernatant; naHSO with a final concentration of 1.04g/L was added 3 Stirring uniformly, standing for 30min, and regulating the pH to 6.4; hydrating in a refrigerator at 4deg.C for 16 hr, centrifuging for 20min (6500 g, 4deg.C), dissolving the precipitate in distilled water completely, adjusting pH to 7.5, dialyzing for 48 hr, and controlling ambient temperature below 4deg.C by ice box; pre-freezing at-80 deg.c, and freeze drying for 48 hr to obtain SG powder.
Adding deionized water into appropriate amount of the SG powder, stirring at room temperature for 2h, and placing into a refrigerator at 4 ℃ for hydration overnight to enable the SG powder to be fully dissolved. The preferred modification sequence HUP, the preferred heating time of 20min 19s, the preferred ultrasound amplitude of 43%, the preferred ultrasound time of 5min 17s, the preferred protein concentration of 4% were chosen. The SG solution was first heated in a 95℃water bath for 20min 19s, immediately after the end, removed and placed in an ice box to cool to room temperature. The ultrasonic cell disruption instrument probe is extended into the central depth of SG solution, and is processed for 5min 17s at the rated power of 750W and the output frequency of 20kHz with the amplitude of 43 percent; in the whole ultrasonic process, the temperature of the sample is controlled below 25 ℃ by using an ice bath. The SG solution was adjusted to pH 12 with 1mol/L NaOH, stirred slowly at room temperature for 1h, the pH of the system was adjusted back to 7.0 with 1mol/L HCl, and maintained for 1h. The pH of the modified SG solution was adjusted to 2, 4, 6, 8, 10 with 1mol/L NaOH, and the solution was stirred slowly at room temperature for 1 hour.
Selecting SG solution with optimal protein concentration of 4%, treating by using the heating-ultrasonic-pH shift combined modification method to obtain modified SG micelles, adding corn oil with oil content of 80%, placing the oil-water mixed solution under an IKA homogenizer probe for high-speed dispersion treatment, homogenizing at 12800rpm for 2min for 15s, and preparing Pickering emulsion.
As shown in fig. 29, on day 1, the Pickering emulsion was in good condition at pH 2, 4, 6, 8, 10; the Pickering emulsion with pH of 4 and 6 has emulsion breaking and emulsion separating phenomena at 60 days, and the Pickering emulsion with pH of 2, 8 and 10 has no obvious change and still has good stability; at 180 days, the pH of the Pickering emulsion with pH values of 2, 8 and 10 is not changed obviously, and the emulsion still has good stability. Can be used for controlled release of active substances, including environmentally responsive release and gastrointestinal tract.
Example 9
Firstly, grinding bean pulp into powder, and sieving the powder with a 100-mesh sieve to obtain fine powder; thoroughly mixing bean powder with distilled water at a ratio of 1:15 (g/mL), adjusting the pH of the suspension to 7.5 with 1mol/L NaOH, and stirring at room temperature for 2h; centrifuging for 30min (9000 g, 4deg.C), and keeping supernatant; naHSO with a final concentration of 1.04g/L was added 3 Stirring uniformly, standing for 30min, and regulating the pH to 6.4; hydrating in a refrigerator at 4deg.C for 16 hr, centrifuging for 20min (6500 g, 4deg.C), dissolving the precipitate in distilled water completely, adjusting pH to 7.5, dialyzing for 48 hr, and controlling ambient temperature below 4deg.C by ice box; pre-freezing at-80 deg.c, and freeze drying for 48 hr to obtain SG powder.
Adding deionized water into appropriate amount of the SG powder, stirring at room temperature for 2h, and placing into a refrigerator at 4 ℃ for hydration overnight to enable the SG powder to be fully dissolved. The preferred modification sequence HUP, the preferred heating time of 20min 19s, the preferred ultrasound amplitude of 43%, the preferred ultrasound time of 5min 17s, the preferred protein concentration of 4% were chosen. The SG solution was first heated in a 95℃water bath for 20min 19s, immediately after the end, removed and placed in an ice box to cool to room temperature. The ultrasonic cell disruption instrument probe is extended into the central depth of SG solution, and is processed for 5min 17s at the rated power of 750W and the output frequency of 20kHz with the amplitude of 43 percent; in the whole ultrasonic process, the temperature of the sample is controlled below 25 ℃ by using an ice bath. The SG solution was adjusted to pH 12 with 1mol/L NaOH, stirred slowly at room temperature for 1h, the pH of the system was adjusted back to 7.0 with 1mol/L HCl, and maintained for 1h. NaCl was placed in the above-mentioned modified SG solution at 0.1mol/L, 0.2mol/L, 0.3mol/L, 0.4mol/L, 0.5mol/L, and 0.6mol/L, respectively.
Selecting SG solution with optimal protein concentration of 4%, treating by using the heating-ultrasonic-pH shift combined modification method to obtain modified SG micelles, adding corn oil with oil content of 80%, placing the oil-water mixed solution under an IKA homogenizer probe for high-speed dispersion treatment, homogenizing at 12800rpm for 2min for 15s, and preparing Pickering emulsion.
As shown in figure 30, the appearance of Pickering emulsion is not changed obviously within 1-180 days, and the Pickering emulsion has good stability under low-high ionic strength and can be applied to low-salt and high-salt foods.
Example 10
Firstly, grinding bean pulp into powder, and sieving the powder with a 100-mesh sieve to obtain fine powder; thoroughly mixing bean powder with distilled water at a ratio of 1:15 (g/mL), adjusting the pH of the suspension to 7.5 with 1mol/L NaOH, and stirring at room temperature for 2h; centrifuging for 30min (9000 g, 4deg.C), and keeping supernatant; naHSO with a final concentration of 1.04g/L was added 3 Stirring uniformly, standing for 30min, and regulating the pH to 6.4; hydrating in a refrigerator at 4deg.C for 16 hr, centrifuging for 20min (6500 g, 4deg.C), dissolving the precipitate in distilled water completely, adjusting pH to 7.5, dialyzing for 48 hr, and controlling ambient temperature below 4deg.C by ice box; pre-freezing at-80 deg.c, and freeze drying for 48 hr to obtain SG powder.
Adding deionized water into appropriate amount of the SG powder, stirring at room temperature for 2h, and placing into a refrigerator at 4 ℃ for hydration overnight to enable the SG powder to be fully dissolved. The preferred modification sequence HUP, the preferred heating time of 20min 19s, the preferred ultrasound amplitude of 43%, the preferred ultrasound time of 5min 17s, the preferred protein concentration of 4% were chosen. The SG solution was first heated in a 95℃water bath for 20min 19s, immediately after the end, removed and placed in an ice box to cool to room temperature. The ultrasonic cell disruption instrument probe is extended into the central depth of SG solution, and is processed for 5min 17s at the rated power of 750W and the output frequency of 20kHz with the amplitude of 43 percent; in the whole ultrasonic process, the temperature of the sample is controlled below 25 ℃ by using an ice bath. The SG solution was adjusted to pH 12 with 1mol/L NaOH, stirred slowly at room temperature for 1h, the pH of the system was adjusted back to 7.0 with 1mol/L HCl, and maintained for 1h.
Selecting SG solution with optimal protein concentration of 4%, treating by using the heating-ultrasonic-pH shift combined modification method to obtain modified SG micelles, adding corn oil with oil content of 80%, placing the oil-water mixed solution under an IKA homogenizer probe for high-speed dispersion treatment, homogenizing at 12800rpm for 2min for 15s, and preparing Pickering emulsion. Heating the Pickering emulsion at 100deg.C for 5min, 10min, 20min, 30min, and 60min respectively.
As shown in FIG. 31, the appearance of Pickering emulsion is not changed obviously within 1-180 days, and the Pickering emulsion has good heat stability and can be applied to heat sterilization food.
The technical scheme of the invention is not limited to the specific embodiment, and all technical modifications made according to the technical scheme of the invention fall within the protection scope of the invention.
Claims (4)
1. A method for preparing Pickering emulsion by using modified glycinin micelles, which is characterized by comprising the following steps:
s1, extracting glycinin and preparing modified glycinin micelles;
s2, mixing corn oil with modified glycinin micelles to prepare a high internal phase Pickering emulsion;
the step S1 specifically includes:
s11, preparing glycinin powder by taking soybean meal as a raw material: firstly, grinding bean pulp into beansSieving the meal powder with a 100-mesh sieve to obtain fine powder; thoroughly mixing soybean meal powder and distilled water according to the ratio of 1g to 15mL, regulating the pH of the suspension to 7.5 by using 1mol/L NaOH, and stirring at room temperature for 2h; centrifuging to obtain supernatant; adding NaHSO with a final concentration of 1.04g/L into the supernatant 3 Stirring, standing for 30min, and regulating pH to 6.4; hydrating in a refrigerator at 4deg.C for 16 and h, centrifuging for 20min, dissolving the precipitate in deionized water, adjusting pH to 7.5, dialyzing for 48 hr, and controlling ambient temperature below 4deg.C by ice box; pre-freezing at-80deg.C, and lyophilizing 48h to obtain glycinin powder;
s12, adding the glycinin powder into deionized water, stirring at room temperature for 2h, and placing into a refrigerator at 4 ℃ for hydration overnight to enable the glycinin powder to be fully dissolved; centrifuging to remove the incompletely dissolved part to obtain a glycinin solution, and carrying out combined modification on the glycinin solution through heating treatment, ultrasonic treatment and pH shift treatment to obtain modified glycinin micelles; the heating treatment process comprises the following steps: heating glycinin solution in 95deg.C water bath for 5-30min, immediately taking out, placing in ice box, and cooling to room temperature; the ultrasonic treatment process comprises the following steps: the probe of an ultrasonic cell disruption instrument is stretched into the central depth of the glycinin solution, and is treated for 1-9 min at the rated power of 750W and the output frequency of 20kHz with the amplitude of 30-70%, and the temperature of a sample is controlled below 25 ℃ by using an ice bath in the whole ultrasonic process; the pH shift treatment comprises the following steps: the pH of the glycinin solution was adjusted to 12 with 1mol/L NaOH, slowly stirred at room temperature for 1h, then the pH of the glycinin solution was adjusted back to 7.0 with 1mol/L HCl and maintained at 1 h;
the step S2 specifically includes:
mixing corn oil and modified glycinin micro-particles with the concentration of 1-5% according to the ratio of 75-85% of the oil, placing under an IKA homogenizer probe for high-speed dispersion treatment, homogenizing at 12800rpm for 2min 15s, and obtaining Pickering emulsion.
2. The method for preparing Pickering emulsion using modified glycinin micelles as in claim 1, wherein the modification sequence of the glycinin solution in step S12 is as follows: heating, then carrying out ultrasonic treatment, and finally carrying out pH shift treatment; heating for 20min 19s; the ultrasonic amplitude was 43%; the ultrasonic time was 5min 17s.
3. The method for preparing Pickering emulsion using modified glycinin micelles as in claim 1, wherein the modified glycinin micelle concentration in step S2 is 4% and the oil phase ratio is 80%.
4. A Pickering emulsion prepared by the method of preparing a Pickering emulsion using modified glycinin micelles of any one of claims 1-3.
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