CN110615900A - Preparation method and application of novel large-size Pickering emulsion - Google Patents
Preparation method and application of novel large-size Pickering emulsion Download PDFInfo
- Publication number
- CN110615900A CN110615900A CN201910947270.6A CN201910947270A CN110615900A CN 110615900 A CN110615900 A CN 110615900A CN 201910947270 A CN201910947270 A CN 201910947270A CN 110615900 A CN110615900 A CN 110615900A
- Authority
- CN
- China
- Prior art keywords
- starch
- pickering emulsion
- preparing
- solution
- water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000839 emulsion Substances 0.000 title claims abstract description 79
- 238000002360 preparation method Methods 0.000 title claims abstract description 29
- 229920002472 Starch Polymers 0.000 claims abstract description 87
- 235000019698 starch Nutrition 0.000 claims abstract description 79
- 239000008107 starch Substances 0.000 claims abstract description 77
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000002245 particle Substances 0.000 claims abstract description 29
- 239000011258 core-shell material Substances 0.000 claims abstract description 26
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 21
- 238000010008 shearing Methods 0.000 claims abstract description 11
- 240000008415 Lactuca sativa Species 0.000 claims abstract description 7
- 239000008268 mayonnaise Substances 0.000 claims abstract description 7
- 235000010746 mayonnaise Nutrition 0.000 claims abstract description 7
- 235000012045 salad Nutrition 0.000 claims abstract description 7
- 235000011389 fruit/vegetable juice Nutrition 0.000 claims abstract description 6
- 239000011259 mixed solution Substances 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 36
- 229920002494 Zein Polymers 0.000 claims description 27
- 239000005019 zein Substances 0.000 claims description 27
- 229940093612 zein Drugs 0.000 claims description 27
- 238000000034 method Methods 0.000 claims description 22
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 13
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 10
- 235000010983 sucrose acetate isobutyrate Nutrition 0.000 claims description 10
- UVGUPMLLGBCFEJ-SWTLDUCYSA-N sucrose acetate isobutyrate Chemical compound CC(C)C(=O)O[C@H]1[C@H](OC(=O)C(C)C)[C@@H](COC(=O)C(C)C)O[C@@]1(COC(C)=O)O[C@@H]1[C@H](OC(=O)C(C)C)[C@@H](OC(=O)C(C)C)[C@H](OC(=O)C(C)C)[C@@H](COC(C)=O)O1 UVGUPMLLGBCFEJ-SWTLDUCYSA-N 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 9
- 239000001797 sucrose acetate isobutyrate Substances 0.000 claims description 8
- UFTFJSFQGQCHQW-UHFFFAOYSA-N triformin Chemical compound O=COCC(OC=O)COC=O UFTFJSFQGQCHQW-UHFFFAOYSA-N 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 5
- 229910021641 deionized water Inorganic materials 0.000 claims description 5
- 238000004108 freeze drying Methods 0.000 claims description 4
- 239000012488 sample solution Substances 0.000 claims description 3
- 238000001338 self-assembly Methods 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 claims description 2
- 229930006000 Sucrose Natural products 0.000 claims description 2
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 2
- 238000001556 precipitation Methods 0.000 claims description 2
- 239000005720 sucrose Substances 0.000 claims description 2
- 235000013305 food Nutrition 0.000 abstract description 14
- 239000000463 material Substances 0.000 abstract description 4
- 230000001105 regulatory effect Effects 0.000 abstract description 3
- 230000001276 controlling effect Effects 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 33
- 235000019198 oils Nutrition 0.000 description 32
- 229920002261 Corn starch Polymers 0.000 description 23
- 239000008120 corn starch Substances 0.000 description 23
- 240000003183 Manihot esculenta Species 0.000 description 14
- 235000016735 Manihot esculenta subsp esculenta Nutrition 0.000 description 14
- 239000008187 granular material Substances 0.000 description 13
- 229920001592 potato starch Polymers 0.000 description 9
- 229940100486 rice starch Drugs 0.000 description 8
- 229940100445 wheat starch Drugs 0.000 description 8
- 240000008042 Zea mays Species 0.000 description 7
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 7
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 7
- 235000005822 corn Nutrition 0.000 description 7
- 239000011248 coating agent Substances 0.000 description 4
- 239000004519 grease Substances 0.000 description 4
- 239000012296 anti-solvent Substances 0.000 description 3
- 238000000576 coating method Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 238000004806 packaging method and process Methods 0.000 description 3
- 102000004169 proteins and genes Human genes 0.000 description 3
- 108090000623 proteins and genes Proteins 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 239000004094 surface-active agent Substances 0.000 description 3
- 235000019483 Peanut oil Nutrition 0.000 description 2
- 235000019484 Rapeseed oil Nutrition 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000000975 bioactive effect Effects 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 239000000346 nonvolatile oil Substances 0.000 description 2
- 239000000312 peanut oil Substances 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000003549 soybean oil Substances 0.000 description 2
- 235000012424 soybean oil Nutrition 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 244000017020 Ipomoea batatas Species 0.000 description 1
- 235000002678 Ipomoea batatas Nutrition 0.000 description 1
- 229920002752 Konjac Polymers 0.000 description 1
- 229920000881 Modified starch Polymers 0.000 description 1
- 239000004368 Modified starch Substances 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 150000001720 carbohydrates Chemical class 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- 238000007385 chemical modification Methods 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- FLISWPFVWWWNNP-BQYQJAHWSA-N dihydro-3-(1-octenyl)-2,5-furandione Chemical compound CCCCCC\C=C\C1CC(=O)OC1=O FLISWPFVWWWNNP-BQYQJAHWSA-N 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 229940095686 granule product Drugs 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- 235000010485 konjac Nutrition 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 229940057917 medium chain triglycerides Drugs 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 235000019426 modified starch Nutrition 0.000 description 1
- 235000014593 oils and fats Nutrition 0.000 description 1
- 238000012803 optimization experiment Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000002572 peristaltic effect Effects 0.000 description 1
- 239000000825 pharmaceutical preparation Substances 0.000 description 1
- 230000000379 polymerizing effect Effects 0.000 description 1
- 235000021067 refined food Nutrition 0.000 description 1
- 239000000523 sample Substances 0.000 description 1
- 235000015067 sauces Nutrition 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
Classifications
-
- 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
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/125—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives containing carbohydrate syrups; containing sugars; containing sugar alcohols; containing starch hydrolysates
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/12—Powdering or granulating
- C08J3/126—Polymer particles coated by polymer, e.g. core shell structures
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2303/00—Characterised by the use of starch, amylose or amylopectin or of their derivatives or degradation products
- C08J2303/02—Starch; Degradation products thereof, e.g. dextrin
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2489/00—Characterised by the use of proteins; Derivatives thereof
Abstract
The invention discloses a preparation method of a novel large-size pickering emulsion, and belongs to the technical field of pickering emulsion preparation. The invention selects the starch with a core-shell structure prepared by different types of starch, then the starch is used as an emulsifier to be added into the oil-water mixed solution, and the Pickering emulsion can reach different particle sizes and can be stable for a long time at high oil content (70% oil content) by regulating and controlling the oil density, the oil content, the emulsifier concentration, the shearing rate and the like. In addition, the invention can save the shearing step required in the preparation of the emulsion, and can form stable pickering emulsion in a short time only by shaking the oil-water mixed solution containing the starch with the shell-core structure by hand. The materials used in the invention are all natural edible materials, the preparation method is simple, the formed pickering emulsion can be stable for a long time, and the pickering emulsion can be used for preparing novel mouthfeel foods, such as instant salad juice and mayonnaise.
Description
Technical Field
The invention relates to the technical field of Pickering emulsion preparation, in particular to a preparation method and application of large-size Pickering emulsion based on core-shell structure starch.
Background
Many of the processed foods we prefer, personal care products to moisturize and beautify the skin, agricultural chemical products to protect crops, and pharmaceutical preparations we rely on are made based on emulsions. Emulsions can exist in either oil-in-water or water-in-oil form, but in both cases very stable droplets are required to prevent breaking of the emulsion leading to deterioration of the product. The stabilization of emulsion droplets is usually achieved by the addition of amphiphilic molecules (such as surfactants or emulsifiers) which act by lowering the interfacial tension between the phases, increasing steric hindrance or electrostatic repulsion between the droplets. In addition to small molecular weight surfactants, soluble proteins and polymeric emulsifiers, solid particles with double wettability can be used to stabilize emulsions, which are named Pickering emulsions (Pickering). Since its discovery by human in 1903, it has been widely used in various fields such as food, medicine, cosmetics, etc. The type, ratio of oil and water phases combined with the particles having dual wetting properties gives the Pickering emulsion many of the formulation characteristics of practical value and the ability to produce highly stable droplets. The types of particles currently in common use include inorganic or synthetic particles such as silica, alumina, titanium oxide, latex, clay, and the like, but they are not used in the food industry. Therefore, finding some natural food particles or making particles that have double wettability and are capable of stabilizing pickering emulsions using food materials entirely has been a difficult problem in the food industry.
On the other hand, the particles in a pickering emulsion need to do some work if they move from the equilibrium position of the interface to either volume phase. When it is completely out of the interface, there are many large variations in the surface free energy of the system. The free energy of desorption for a 10 nm particle leaving the interface is several thousand kT, compared to only 10kT for a surfactant of similar particle size. The stability of pickering emulsions is much higher than that of conventional emulsions. Whereas the separation of a single particle can be linearly increased with respect to its radius squared. Thus, particles with larger particle sizes are more difficult to stabilize the pickering emulsion, and once it is successfully stabilized, its stability will be better than that of smaller particle sizes.
The chemical formula of the starch is C6H12O6Is formed by polymerizing glucose molecules. It is the most common storage form of carbohydrates in cells and one of the most important sources of energy for humans. Native starch is not hydrophobic in nature, but its hydrophobicity can be increased by chemical modification and coating with a hydrophobic shell, and its double wettability is increased. Zein (zein) is a protein which is extracted from corn for the first time in 1821 by Gorhamin and can be dissolved in ethanol, has good film forming property, adhesiveness, water resistance and moisture resistance, has the characteristics of acid resistance, oil resistance and the like, and can be widely applied to other industries such as medicine, food, chemical industry and the like. In the food industry, the alcohol soluble protein can be used as a coating agent, namely a coating is formed on the surface of food in a spraying mode, and the coating can prevent moisture and oxidation, thereby prolonging the shelf life of the food, and can also increase the luster when being sprayed on fruits. Sucrose acetate isobutyrate is a stabilizer and a relative density regulator, has certain viscosity, and can increase the density of grease after being mixed with the grease.
The method modifies common starch by using octenyl succinic anhydride soluble modified starch (OSA starch), separates out zein by an anti-solvent method, and forms a starch-zein core-shell structure on the surface of starch granules in a self-assembly manner, and the starch with the core-shell structure and the grease with well-mixed density are used for preparing Pickering emulsion.
The invention content is as follows:
the invention aims to solve the technical problem of providing a preparation method of a large-size Pickering emulsion stabilized by starch with a shell-core structure, so that the large-size Pickering emulsion has a larger structure than the traditional Pickering emulsion and has better stability under the normal temperature condition, and the method is suitable for most of the conventional oil on the market.
The inventors continuously make efforts to finally obtain a preparation method of a novel large-size Pickering emulsion, which takes starch with a shell-core structure as a stable emulsifier, takes mixed oil of medium-chain triglyceride and sucrose acetate isobutyrate as an oil phase and deionized water as a water phase, and the preparation method comprises the following steps:
(1) preparation of a sample solution: preparing ethanol-water solution, continuously preparing zein solution with the ethanol-water solution, shaking up, placing in a water bath ultrasonic device, and performing ultrasonic treatment for 15min to obtain a solution for later use; preparing an OSA starch solution with a certain concentration, magnetically stirring for 2 hours, and standing for later use; preparing sucrose acetate isobutyrate-medium chain triglyceride (SAIB-MCT) mixed oil, wherein the mixing volume ratio of the medium chain triglyceride to the sucrose acetate isobutyrate is 3:2, and after mixing, placing the mixture in a water bath at 70 ℃ and stirring the mixture for 2 hours at constant temperature to uniformly mix the mixture;
(2) preparing a core-shell structure starch emulsifier: adding starch into a zein solution, placing the zein solution on a magnetic stirrer for stirring at 200-400rpm, and simultaneously dropping an OSA starch solution at a constant speed to reduce the concentration of ethanol in the solution so as to separate out zein, and forming a shell layer on the surface of a starch particle by self-assembly to finally form starch particles with a shell-core structure of starch-zein; standing for precipitation, repeatedly washing with water for 3-4 times, removing residual ethanol and zein particles in the solution, and freeze drying;
(3) preparation of pickering emulsion: preparing the oil phase and the water phase in the step (1) into an oil-water mixed solution, adding the starch with the shell-core structure in the step (2), shearing the mixture for 30s by using a high-speed shearing instrument, wherein the shearing rate is 5000rpm/min-20000rm/min, and standing the mixture to finally form the large-size Pickering emulsion taking the starch with the shell-core structure as an emulsifier.
Preferably, in the preparation method of the novel large-size pickering emulsion, the ethanol-water solution of zein in the step (1) has a volume concentration of 70% and a mass concentration of zein of 1.0-3.0%.
Preferably, in the preparation method of the novel large-size pickering emulsion, the mass concentration of the OSA starch in the OSA starch solution in the step (1) is 1-3%, preferably 2%.
Preferably, in the preparation method of the novel large-size pickering emulsion, the volume concentration of ethanol in the ethanol-water solution in the step (2) is reduced from 70% to 30%, preferably 45%.
Preferably, in the method for preparing the novel large-size pickering emulsion, the mass content of the starch added into the zein solution in the step (2) is 2.5% w/w-7.5%, preferably 4.5%.
Preferably, in the preparation method of the novel large-size Pickering emulsion, as described above, the adding rate of the OSA starch solution in the step (2) is controlled to be 0.1-0.5ml/min, preferably 0.2 ml/min.
Preferably, in the preparation method of the novel large-size pickering emulsion, the SAIB content in the mixed oil phase prepared in the step (3) is 20% -50%, preferably 40%.
Preferably, in the preparation method of the novel large-size pickering emulsion, the added core-shell structure starch in the step (3) accounts for 1% -5%, preferably 3% of the mass of the oil-water mixed solution.
Preferably, in the method for preparing the novel large-size pickering emulsion, as described above, the mixing volume ratio of the oil phase and the water phase in the step (3) is 10-70%, preferably 50-60%.
Preferably, the shear rate in step (3) is 5000rpm/min, and the time is preferably 30 s.
Preferably, the preparation method of the novel large-size pickering emulsion comprises the steps of preparing the starch with the shell-core structure from wheat starch, corn starch, waxy corn starch, cassava starch, potato starch and rice starch.
The application of the novel large-size Pickering emulsion comprises the following steps: the Pickering emulsion can be used for preparing food-grade salad juice, and can be used for preparing products such as food-grade mayonnaise and the like after heating and pasting.
Compared with the prior art, the invention has the advantages that:
1. the invention uses the starch with a shell-core structure prepared by an anti-solvent method as an emulsifier, and has the advantages of simple and easy method, low preparation components and food-grade materials.
2. The size of the Pickering emulsion can be effectively regulated and controlled by simply changing the content of the starch with the shell-core structure, the shearing rate and the proportion of oil and water phases.
3. The prepared Pickering emulsion can be stable for a long time at normal temperature and other severe environments, and can be used for packaging sensitive bioactive components in foods and local formulas, and making portable mayonnaise or salad juice.
4. The core-shell structure starch granules have good surface activity and double wettability, can form Pickering emulsion with high grease content, can form large-size Pickering emulsion of hundreds of microns or even millimeter level, can be used for preparing novel mouthfeel food such as instant salad juice and mayonnaise, and has excellent stability, packaging performance and freeze-thaw stability which prove to be suitable for packaging sensitive bioactive components in food and local formulas and the like.
5. The core-shell structure starch granules have good surface activity, can form large-granule Pickering emulsion by simple manual shaking, can be used for preparing food-grade salad juice, and can be used for preparing products such as food-grade mayonnaise and the like after being heated and gelatinized.
Drawings
FIG. 1 is a picture of a core-shell structure starch emulsifier product prepared from corn starch by an anti-solvent method.
FIG. 2 is a microscope photograph of Pickering granules formed by core-shell structure granules of corn starch, potato starch, tapioca starch, wheat starch, waxy corn starch and rice starch at 5000rpm for 30s, respectively, wherein the oil phase content is 50%.
FIG. 3 is a fluorescent microscope photograph of Pickering granules formed by core-shell structure granules of corn starch, potato starch, tapioca starch, wheat starch, waxy corn starch and rice starch at 5000rpm for 30s, respectively, with the oil phase content being 50%.
FIG. 4 is a laser confocal microscope photograph of Pickering granules formed by core-shell structure granules of corn starch, potato starch, tapioca starch, wheat starch, waxy corn starch and rice starch at 5000rpm for 30s, wherein the oil phase content is 50%.
FIG. 5 shows scanning electron micrographs of Pickering granules formed from core-shell structure granules of corn starch, potato starch, tapioca starch, wheat starch, waxy corn starch and rice starch at 5000rpm for 30s, respectively, with the oil phase content being 30%.
FIG. 6 is a photograph of the three-phase contact angles of corn starch, potato starch, tapioca starch, wheat starch, waxy corn starch and rice starch, respectively, and core-shell structured particles thereof.
FIG. 7 shows Pickering emulsions prepared with different emulsifier (cassava core-shell structure starch) concentrations at a fixed rotation speed of 10000rpm and a fixed oil phase concentration of 30%, wherein the emulsifier concentrations are respectively 1%, 2%, 3% and 4%.
FIG. 8 shows Pickering emulsions prepared at different rotation speeds after the concentration of the fixed emulsifier (cassava core-shell structure starch) is 3% and the concentration of the fixed oil phase is 30%, wherein the rotation speeds are respectively 5000rpm, 10000rpm, 15000rpm, 20000rpm and 25000 rpm.
FIG. 9 shows Pickering emulsions prepared at different oil phase concentrations with a fixed rotation speed of 10000rpm and a fixed emulsifier (cassava core-shell structure starch) concentration of 3%, wherein the oil phase concentrations are respectively selected from 30%, 40%, 50% and 60%. 70 percent.
FIG. 10 is a Pickering emulsion made by shaking by hand for 5 seconds using 2% and 3% tapioca kernel structure starch and 50% oil phase.
The specific implementation mode is as follows:
in order to clearly illustrate the technical features of the scheme of the invention, the invention is explained below with reference to specific embodiments. The scope of protection of the invention is not limited to these examples. All changes, modifications and equivalents that do not depart from the spirit of the invention are intended to be included within the scope thereof.
The starch of the present invention is not limited to corn starch, potato starch, tapioca starch, wheat starch, waxy corn starch, rice starch, and other common starches.
The choice of oil in the present invention is not limited to medium chain triglycerides, and other common oils are suitable for use in the present invention, such as soybean oil, peanut oil, rapeseed oil, and the like.
In particular, the choice of the emulsification process of the present invention is not limited to the use of high shear, and large-size pickering emulsions can also be formed by simple manual shaking.
Example 1:
the invention is suitable for the preparation of starch with a shell-core structure and various oils and fats made of various common starches, and the preparation method of the novel large-size Pickering emulsion comprises the following steps:
(1) preparation of a sample solution: preparing an OSA solution: an aqueous solution containing 2% OSA starch (type GUM-1773) in 100g (w/w) was prepared with deionized water and stirred at 400rpm for 2h to dissolve it thoroughly. Preparing zein solution: preparing 70% (v/v) ethanol-water solution, mixing uniformly for later use, preparing 0.25% -1% (w/w) zein in the 70% (v/v) ethanol-water solution, and carrying out ultrasonic treatment for 15 min. ③ putting the sucrose acetate isobutyrate into a 70 ℃ water bath kettle to heat for 2h to ensure that the sucrose acetate isobutyrate has fluidity, weighing 20g of sucrose acetate isobutyrate to mix with 30g of medium chain triglyceride, and heating and stirring for 2h in the 70 ℃ water bath kettle to uniformly mix.
(2) Preparing the core-shell structure starch: weighing 1.5g of corn starch in a 100ml beaker, adding the zein solution prepared in the step (1) into the beaker to 40g, adding stirring magnetons, and stirring at the rotating speed of 200rpm for 10 minutes to uniformly disperse the starch. And (2) slowly dripping the OSA starch solution prepared in the step (1) into the starch dispersion liquid through a peristaltic pump. The dropping speed is controlled to be 0.2ml/min, the dropping amount is controlled to be 22.22ml, and the ethanol concentration of the starch-zein solution is reduced from 70% (v/v) to 45% (v/v). Standing to precipitate starch after the dropwise addition is completed, repeatedly washing the starch for 3-4 times by using deionized water, and freeze-drying to obtain the corn starch with the shell-core structure. FIG. 1 shows a diagram of a corn husk-core structure starch granule product prepared by the method.
(3) Preparation of pickering emulsion: 0.3g of freeze-dried starch with a shell-core structure is weighed, 6.7g of deionized water is added, and 3g of uniformly mixed oil is added. Shearing at high speed of 5000rpm/min for 30s, standing and layering to obtain 30% oil content corn starch pickering emulsion.
Fig. 2, photograph 1, is a microscope photograph of a pickering emulsion prepared using corn husk and core structured starch granules. The prepared pickering emulsion is characterized by a fluorescence microscope and a laser confocal microscope, and as shown in fig. 3, the 1 st photograph and fig. 4, the 1 st photograph of the pickering emulsion prepared by the corn shell-core structure starch particles after fluorescent dyeing are shown in fig. 3, the fact that the surface of oil drops is covered by a layer of corn shell-core structure starch particles can be clearly observed to form the pickering emulsion. The appearance of a sample after oil polymerization and freeze drying is observed by using a scanning electron microscope, as shown in a group 1 photograph of fig. 5, a total appearance diagram and a local appearance diagram of a Pickering emulsion oil drop polymerization solid particle scanning electron microscope prepared from corn shell-core structure starch particles, starch can be clearly observed to be easily adsorbed on an oil-water interface after the core-shell structure is formed by zein, so that oil and water phases form Pickering emulsion.
The double wettability (hydrophilicity and hydrophobicity) of the core-shell structure starch flakes was measured by the three-phase contact angle, and as shown in fig. 6, photograph 1, the three-phase contact angle measured using the corn core-shell structure starch flakes was greater than the angle of the original starch. The core-shell structure of the corn starch is characterized in that the surface hydrophobicity of the corn starch is stronger, and the corn starch is easier to separate from a water phase and further to be adsorbed on oil drops.
The pickering emulsion is regulated and controlled through an optimization experiment. We found that after fixing the rotation speed (10000 rpm) and the oil phase concentration (30%) as shown in fig. 7, the particle size of the prepared pickering emulsion gradually decreases with the increase (1%, 2%, 3%, 4% selected) of the emulsifier (tapioca core-shell structure starch); as shown in fig. 8, after fixing the emulsifier concentration (3%) and the oil phase (30%), the particle size of the produced pickering emulsion gradually decreased with increasing shear rate; as shown in FIG. 9, after fixing the emulsifier concentration (3%) and shear rate (10000 rm), the particle size of the pickering emulsion obtained gradually increased with the increase of the oil phase ratio.
Fig. 10 is a photograph of pickering emulsion prepared by manually shaking for five seconds using the prepared core-shell structure starch particles as an emulsifier without high-speed shearing, wherein the oil phase concentration is 50% and the emulsifier (tapioca core-shell structure starch) concentrations are 2% and 3%, respectively, which fully shows that the starch has excellent and stable emulsibility, and can be used to prepare novel foods such as salad sauce, mayonnaise and the like.
The raw materials of the shell-core structure starch in the method are not limited to corn starch, and the rest of potato starch, cassava starch, wheat starch, waxy corn starch and rice starch are all suitable for the method and are also suitable for other common starch, such as konjak starch, sweet potato starch and the like.
The oil raw material in the method is not limited to medium chain triglyceride, and the rest of the oil raw material such as soybean oil, peanut oil, rapeseed oil and the like are all suitable for the method.
Claims (10)
1. A preparation method of novel large-size Pickering emulsion is characterized by comprising the following steps: the pickering emulsion takes starch with a shell-core structure as a stable emulsifier, mixed oil of medium-chain triglyceride and sucrose acetate isobutyrate as an oil phase, and deionized water as a water phase, and the preparation method comprises the following steps:
(1) preparation of a sample solution: preparing ethanol-water solution, continuously preparing zein solution with the ethanol-water solution, shaking up, placing in a water bath ultrasonic device, and performing ultrasonic treatment for 15min to obtain a solution for later use; preparing an OSA starch solution, magnetically stirring for 2 hours, and standing for later use; preparing sucrose acetate isobutyrate-medium chain triglyceride (SAIB-MCT) mixed oil, wherein the mixing volume ratio of the medium chain triglyceride to the sucrose acetate isobutyrate is 3:2, and after mixing, placing the mixture in a water bath at 70 ℃ and stirring the mixture for 2 hours at constant temperature to uniformly mix the mixture;
(2) preparing a core-shell structure starch emulsifier: adding starch into a zein solution, placing the zein solution on a magnetic stirrer for stirring at 200-400rpm, and simultaneously dropping an OSA starch solution at a constant speed to reduce the concentration of ethanol in the solution so as to separate out zein, and forming a shell layer on the surface of a starch particle by self-assembly to finally form starch particles with a shell-core structure of starch-zein; standing for precipitation, repeatedly washing with water for 3-4 times, removing residual ethanol and zein particles in the solution, and freeze drying;
(3) preparation of pickering emulsion: preparing the oil phase and the water phase in the step (1) into an oil-water mixed solution, adding the starch with the shell-core structure in the step (2), shearing the mixture for 20 to 30 seconds by using a high-speed shearing instrument at a shearing rate of 5000rpm/min to 20000rm/min, and standing to finally form the large-size Pickering emulsion taking the starch with the shell-core structure as an emulsifier.
2. The method of claim 1 for preparing a novel large size pickering emulsion, wherein: the ethanol-water solution of zein in the step (1), wherein the volume concentration of ethanol is 70%, and the mass concentration of zein is 1.0-3.0%; the mass concentration of the OSA starch is 1-3%, preferably 2%.
3. A method for preparing a novel large size pickering emulsion according to claim 1, wherein the volume concentration of ethanol in the ethanol-water solution in step (2) is reduced from 70% to 30%, preferably 45%.
4. The method of claim 1 for preparing a novel large size pickering emulsion, wherein: the mass content of the starch added into the zein solution in the step (2) is 2.5% w/w-7.5%, and the starch is preferably 4.5%.
5. The method of claim 1 for preparing a novel large size pickering emulsion, wherein: the dropping rate of the OSA starch solution in the step (2) is controlled to be 0.1-0.5ml/min, and preferably 0.2 ml/min.
6. The method of claim 1 for preparing a novel large size pickering emulsion, wherein: the mass content of SAIB in the mixed oil phase prepared in the step (3) is 20% -50%, and preferably 40%.
7. The method of claim 1 for preparing a novel large size pickering emulsion, wherein: the amount of the starch with the shell-core structure added in the step (3) is 1-5% of the mass of the oil-water mixed solution, and is preferably 3%.
8. The method of claim 1 for preparing a novel large size pickering emulsion, wherein: the mixing volume ratio of the oil phase and the water phase in the step (3) is 10-70%, preferably 50-60%.
9. The method of claim 1 for preparing a novel large size pickering emulsion, wherein: the shear rate in said step (3) is 5000rpm/min, preferably 30 s.
10. The application of the novel large-size Pickering emulsion is characterized in that: the Pickering emulsion can be used for preparing food-grade salad juice and food-grade mayonnaise.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201910143995X | 2019-02-27 | ||
CN201910143995.XA CN109912818A (en) | 2019-02-27 | 2019-02-27 | A kind of preparation method and application of core-shell structure slow-digestion starch |
Publications (1)
Publication Number | Publication Date |
---|---|
CN110615900A true CN110615900A (en) | 2019-12-27 |
Family
ID=66962414
Family Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201910143995.XA Pending CN109912818A (en) | 2019-02-27 | 2019-02-27 | A kind of preparation method and application of core-shell structure slow-digestion starch |
CN201910947270.6A Pending CN110615900A (en) | 2019-02-27 | 2019-10-06 | Preparation method and application of novel large-size Pickering emulsion |
Family Applications Before (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201910143995.XA Pending CN109912818A (en) | 2019-02-27 | 2019-02-27 | A kind of preparation method and application of core-shell structure slow-digestion starch |
Country Status (1)
Country | Link |
---|---|
CN (2) | CN109912818A (en) |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113017095A (en) * | 2021-03-15 | 2021-06-25 | 南京财经大学 | Preparation method and application of corn oil quinoa protein pickering high internal phase emulsion |
CN113368049A (en) * | 2021-06-17 | 2021-09-10 | 江南大学 | Pickering emulsion based on fat crystal nanoparticle stability and preparation method thereof |
CN115553451A (en) * | 2022-09-09 | 2023-01-03 | 华南农业大学 | Low-cholesterol and high-freeze-thaw stability vegetable protein-based mayonnaise and preparation method thereof |
CN115886122A (en) * | 2023-01-10 | 2023-04-04 | 青岛农业大学 | Method for improving stability of vegetable protein emulsion and application |
CN116426038A (en) * | 2023-04-06 | 2023-07-14 | 江南大学 | Synergistically stable starch-based pickering emulsion and application thereof in medicine and food fields |
Families Citing this family (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109912818A (en) * | 2019-02-27 | 2019-06-21 | 湖北工业大学 | A kind of preparation method and application of core-shell structure slow-digestion starch |
WO2021033742A1 (en) * | 2019-08-20 | 2021-02-25 | 日揮触媒化成株式会社 | Particles containing starch, method for producing same, and cosmetic preparation |
CN110917137B (en) * | 2019-11-26 | 2021-08-10 | 江南大学 | Preparation method of Pickering emulsion with synergistic and stable prolamin nanoparticles and starch nanoparticles |
CN113552249A (en) * | 2021-06-24 | 2021-10-26 | 上海交通大学 | Method for extracting and identifying starch shell protein |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5145702A (en) * | 1988-09-19 | 1992-09-08 | Opta Food Ingredients, Inc. | Hydrophobic protein microparticles and preparation thereof |
CN108185406A (en) * | 2018-02-02 | 2018-06-22 | 河南工业大学 | Starch octenyl succinate anhydride-zeins compound and preparation method thereof |
CN108752603A (en) * | 2018-06-01 | 2018-11-06 | 华南理工大学 | A kind of preparation method of starch base Pickering emulsion gels |
CN109912818A (en) * | 2019-02-27 | 2019-06-21 | 湖北工业大学 | A kind of preparation method and application of core-shell structure slow-digestion starch |
-
2019
- 2019-02-27 CN CN201910143995.XA patent/CN109912818A/en active Pending
- 2019-10-06 CN CN201910947270.6A patent/CN110615900A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5145702A (en) * | 1988-09-19 | 1992-09-08 | Opta Food Ingredients, Inc. | Hydrophobic protein microparticles and preparation thereof |
CN108185406A (en) * | 2018-02-02 | 2018-06-22 | 河南工业大学 | Starch octenyl succinate anhydride-zeins compound and preparation method thereof |
CN108752603A (en) * | 2018-06-01 | 2018-11-06 | 华南理工大学 | A kind of preparation method of starch base Pickering emulsion gels |
CN109912818A (en) * | 2019-02-27 | 2019-06-21 | 湖北工业大学 | A kind of preparation method and application of core-shell structure slow-digestion starch |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113017095A (en) * | 2021-03-15 | 2021-06-25 | 南京财经大学 | Preparation method and application of corn oil quinoa protein pickering high internal phase emulsion |
CN113017095B (en) * | 2021-03-15 | 2023-01-24 | 南京财经大学 | Preparation method and application of corn oil quinoa protein pickering high internal phase emulsion |
CN113368049A (en) * | 2021-06-17 | 2021-09-10 | 江南大学 | Pickering emulsion based on fat crystal nanoparticle stability and preparation method thereof |
CN115553451A (en) * | 2022-09-09 | 2023-01-03 | 华南农业大学 | Low-cholesterol and high-freeze-thaw stability vegetable protein-based mayonnaise and preparation method thereof |
CN115886122A (en) * | 2023-01-10 | 2023-04-04 | 青岛农业大学 | Method for improving stability of vegetable protein emulsion and application |
CN116426038A (en) * | 2023-04-06 | 2023-07-14 | 江南大学 | Synergistically stable starch-based pickering emulsion and application thereof in medicine and food fields |
CN116426038B (en) * | 2023-04-06 | 2023-10-17 | 江南大学 | Synergistically stable starch-based pickering emulsion and application thereof in medicine and food fields |
Also Published As
Publication number | Publication date |
---|---|
CN109912818A (en) | 2019-06-21 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN110615900A (en) | Preparation method and application of novel large-size Pickering emulsion | |
Gao et al. | Review of recent advances in the preparation, properties, and applications of high internal phase emulsions | |
Mao et al. | Emulsion design for the delivery of β-carotene in complex food systems | |
Komaiko et al. | Formation of food‐grade nanoemulsions using low‐energy preparation methods: A review of available methods | |
Qin et al. | Fabrication and characterization of quinoa protein nanoparticle-stabilized food-grade pickering emulsions with ultrasound treatment: Effect of ionic strength on the freeze–thaw stability | |
Gharsallaoui et al. | Pea (Pisum sativum, L.) protein isolate stabilized emulsions: a novel system for microencapsulation of lipophilic ingredients by spray drying | |
Wei et al. | Novel bilayer emulsions costabilized by zein colloidal particles and propylene glycol alginate, Part 1: Fabrication and characterization | |
US4931284A (en) | Micro-capsules | |
Kaushik et al. | Limonene encapsulation in freeze-drying of gum Arabic–sucrose–gelatin systems | |
Li et al. | Effects of maltose on stability and rheological properties of orange oil-in-water emulsion formed by OSA modified starch | |
DK2651243T3 (en) | Hitherto unknown particle stabilized emulsions and foams. | |
CN103283866B (en) | camellia oil microemulsion and preparation method thereof | |
CN108634169B (en) | Preparation method of lutein nano emulsion | |
CN110917064A (en) | Preparation method of pumpkin seed protein nanoparticles, pumpkin seed protein nanoparticles and application of pumpkin seed protein nanoparticles | |
Chen et al. | Development of anti-photo and anti-thermal high internal phase emulsions stabilized by biomass lignin as a nutraceutical delivery system | |
Cheng et al. | Impact of polysaccharide mixtures on the formation, stability and EGCG loading of water-in-oil high internal phase emulsions | |
Zhang et al. | Edible oil powders based on spray-dried Pickering emulsion stabilized by soy protein/cellulose nanofibrils | |
Dong et al. | Emulsifying behaviors and interfacial properties of different protein/gum arabic complexes: Effect of pH | |
JPH09501100A (en) | Water / oil emulsions and water / oil / water emulsions with high internal phase content | |
Yin et al. | Fabrication and characterization of tunable high internal phase emulsion gels (HIPE-Gels) formed by natural triterpenoid saponin and plant soy protein | |
Laine et al. | Emulsion preparation with modified oat bran: Optimization of the emulsification process for microencapsulation purposes | |
Wang et al. | CaCl2 supplementation of hydrophobised whey proteins: Assessment of protein particles and consequent emulsions | |
Akcicek et al. | Egg yolk-free vegan mayonnaise preparation from pickering emulsion stabilized by gum nanoparticles with or without loading olive pomace extracts | |
Shirvani et al. | Fabrication of edible solid lipid nanoparticle from beeswax/propolis wax by spontaneous emulsification: Optimization, characterization and stability | |
Pichot et al. | Particle-stabilized food emulsions |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20191227 |
|
RJ01 | Rejection of invention patent application after publication |