Classifications

• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
  • A23L35/00—Foods or foodstuffs not provided for in groups A23L5/00 - A23L33/00; Preparation or treatment thereof
  • A23L35/10—Emulsified foodstuffs
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS OR COOKING OILS
  • A23D7/00—Edible oil or fat compositions containing an aqueous phase, e.g. margarines
  • A23D7/005—Edible oil or fat compositions containing an aqueous phase, e.g. margarines characterised by ingredients other than fatty acid triglycerides
  • A23D7/0053—Compositions other than spreads
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23C—DAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; PREPARATION THEREOF
  • A23C11/00—Milk substitutes, e.g. coffee whitener compositions
  • A23C11/02—Milk substitutes, e.g. coffee whitener compositions containing at least one non-milk component as source of fats or proteins
  • A23C11/06—Milk substitutes, e.g. coffee whitener compositions containing at least one non-milk component as source of fats or proteins containing non-milk proteins
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23C—DAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; PREPARATION THEREOF
  • A23C11/00—Milk substitutes, e.g. coffee whitener compositions
  • A23C11/02—Milk substitutes, e.g. coffee whitener compositions containing at least one non-milk component as source of fats or proteins
  • A23C11/10—Milk substitutes, e.g. coffee whitener compositions containing at least one non-milk component as source of fats or proteins containing or not lactose but no other milk components as source of fats, carbohydrates or proteins
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23C—DAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; PREPARATION THEREOF
  • A23C11/00—Milk substitutes, e.g. coffee whitener compositions
  • A23C11/02—Milk substitutes, e.g. coffee whitener compositions containing at least one non-milk component as source of fats or proteins
  • A23C11/10—Milk substitutes, e.g. coffee whitener compositions containing at least one non-milk component as source of fats or proteins containing or not lactose but no other milk components as source of fats, carbohydrates or proteins
  • A23C11/103—Milk substitutes, e.g. coffee whitener compositions containing at least one non-milk component as source of fats or proteins containing or not lactose but no other milk components as source of fats, carbohydrates or proteins containing only proteins from pulses, oilseeds or nuts, e.g. nut milk
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23C—DAIRY PRODUCTS, e.g. MILK, BUTTER OR CHEESE; MILK OR CHEESE SUBSTITUTES; PREPARATION THEREOF
  • A23C11/00—Milk substitutes, e.g. coffee whitener compositions
  • A23C11/02—Milk substitutes, e.g. coffee whitener compositions containing at least one non-milk component as source of fats or proteins
  • A23C11/10—Milk substitutes, e.g. coffee whitener compositions containing at least one non-milk component as source of fats or proteins containing or not lactose but no other milk components as source of fats, carbohydrates or proteins
  • A23C11/103—Milk substitutes, e.g. coffee whitener compositions containing at least one non-milk component as source of fats or proteins containing or not lactose but no other milk components as source of fats, carbohydrates or proteins containing only proteins from pulses, oilseeds or nuts, e.g. nut milk
  • A23C11/106—Addition of, or treatment with, microorganisms
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS OR COOKING OILS
  • A23D7/00—Edible oil or fat compositions containing an aqueous phase, e.g. margarines
  • A23D7/003—Compositions other than spreads
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS OR COOKING OILS
  • A23D7/00—Edible oil or fat compositions containing an aqueous phase, e.g. margarines
  • A23D7/02—Edible oil or fat compositions containing an aqueous phase, e.g. margarines characterised by the production or working-up
  • A23D7/04—Working-up
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23D—EDIBLE OILS OR FATS, e.g. MARGARINES, SHORTENINGS OR COOKING OILS
  • A23D9/00—Other edible oils or fats, e.g. shortenings or cooking oils
  • A23D9/02—Other edible oils or fats, e.g. shortenings or cooking oils characterised by the production or working-up
  • A23D9/04—Working-up
  • A23D9/05—Forming free-flowing pieces
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
  • A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
  • A23L27/20—Synthetic spices, flavouring agents or condiments
  • A23L27/21—Synthetic spices, flavouring agents or condiments containing amino acids
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
  • A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
  • A23L27/20—Synthetic spices, flavouring agents or condiments
  • A23L27/26—Meat flavours
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
  • A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
  • A23L27/30—Artificial sweetening agents
  • A23L27/31—Artificial sweetening agents containing amino acids, nucleotides, peptides or derivatives
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
  • A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
  • A23L27/50—Soya sauce
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
  • A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
  • A23L29/10—Foods or foodstuffs containing additives; Preparation or treatment thereof containing emulsifiers
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
  • A23L9/00—Puddings; Cream substitutes; Preparation or treatment thereof
  • A23L9/20—Cream substitutes
• • A—HUMAN NECESSITIES
  • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
  • A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
  • A23L9/00—Puddings; Cream substitutes; Preparation or treatment thereof
  • A23L9/20—Cream substitutes
  • A23L9/24—Cream substitutes containing non-milk fats and non-milk proteins, e.g. eggs or soybeans

Definitions

• the present invention relates to an oil-in-water emulsion that is a nanoemulsion and a method for producing the same.
• Emulsions with extremely small emulsion particle diameters of 200 nm or less are called nanoemulsions. Furthermore, when the emulsified particle size is 100 nm or less, the transparency is remarkably improved.
• Non-Patent Document 1 many of the oil-based ingredients correspond to functional ingredients, that is, bioactive compounds, and are used in the development of functional foods. Alternatively, it has low solubility in water and low bioavailability. As a solution to this problem, utilization of an oil-in-water emulsion, which is a nanoemulsion, has been considered.
• Patent Document 1 1 to 70 parts by weight of a water-insoluble substance is mixed with 1 to 90 parts by weight of polyglycerin fatty acid ester, 0.1 to 50 parts by weight of water, and 1 to 90 parts by weight of polyhydric alcohol to emulsify and solubilize.
• Patent Document 2 discloses a method for producing a solubilized solution characterized by containing a polyhydric alcohol and an emulsifier having an HLB of 9 or more, as described in Patent Document 3.
• Patent document discloses a solubilized tocopherol characterized by mixing 1 to 50% by weight of tocopherol, 1 to 90% by weight of saccharides, 0.1 to 30% by weight of emulsifier, and 1 to 10% by weight of ethanol.
• Non-Patent Document 2 describes an emulsion with a particle size of 92 to 220 nm using casein.
• Non-Patent Document 3 describes a ⁇ -carotene emulsion with an emulsified particle size of 70 to 160 nm using gelatin or casein.
• Non-Patent Document 4 describes a ⁇ -carotene emulsion with an emulsified particle size of 17-110 nm using WPI, sodium caseinate, and SPI.
• ⁇ is the surface excess concentration of the emulsifier (adsorbed amount, kg/m ⁇ 2)
• Cs is the emulsifier concentration (kg/m ⁇ 3)
• ⁇ is the volume fraction of the dispersed phase.
• macromolecular materials are generally hydrocolloids, and when hydrocolloids are used, emulsification may not be possible even if the concentration is high.
• depletion interaction depletion aggregation
• Non-Patent Document 6 Japanese Patent Document 6
• Patent Documents 1 to 4 are all based on synthetic emulsifiers.
• Non-Patent Documents 2 to 4 also require the use of butanol or hexane, making it difficult to apply to foods (Non-Patent Documents 2 and 4), and Tween 20, a synthetic emulsifier, is included ( Non-Patent Document 3).
• the present invention provides an oil-based material having excellent transparency without using a synthetic emulsifier or an organic solvent having a boiling point lower than that of water when obtaining an oil-in-water emulsion that is a nanoemulsion that can be applied to foods and drinks.
• An object of the present invention is to provide a containing emulsion.
• an oil-in-water emulsion that is a nanoemulsion that does not use synthetic emulsifiers, organic solvents, etc. can be produced.
• the present invention was completed by discovering that it can be obtained.
• the present invention (1) contains 0.5 to 35% by mass of an oily material, 1 to 80% by mass of a readily water-soluble substance, 5 to 70% by mass of water, and a crude protein content of a protein material having the following properties: An oil-in-water emulsion containing 30 to 1,200% by mass and having an emulsified particle size of 100 nm or less.
• the protein material has a viscosity of 10,000 mPa s or less when measured at 25°C after heating an aqueous solution of 20% by mass of crude protein at 80°C for 30 minutes, and the solubilization rate of 0.22M TCA is 30% or higher. It has 95% properties.
• the NSI is 80 or more, the total amount of water-soluble substances and water is 2 times or more by mass of the protein material, and the water-soluble substances are 30 (g/100g) or more to water. It has a solubility and a boiling point higher than that of water, and the transmittance (660 nm) of a dispersion obtained by dispersing an oily material in water to 0.5% by mass is 50% or more, and the water content is 65% by mass or less, The oil-in-water emulsion according to (1), which does not contain an emulsifier.
• the protein material is added to a solution of 30 to 1,200% by mass of the oily material, 1 to 80% by mass of the easily water-soluble substance, and 5 to 70% by mass of water.
• the protein material has a viscosity of 10,000 mPa s or less when measured at 25°C after heating an aqueous solution with a crude protein content of 20% by mass at 80°C for 30 minutes, and a 0.22M TCA solubilization rate of 30 to
• the protein material has a viscosity of 10,000 mPa s or less when measured at 25°C after heating an aqueous solution with a crude protein content of 20% by mass at 80°C for 30 minutes, and a 0.22M TCA solubilization rate of 30 to 95%, and NSI is 80 or more, a high-pressure emulsifying device is used for emulsification of the oil-in-water emulsion, the pressure during the emulsification is 50 MPa or more, and no emulsifier is used, oil-in-water type according to (9) A method for producing an emulsion.
• a method for producing an emulsion powder comprising drying the oil-in-water emulsion according to any one of (9) to (13). is.
• the present invention can also provide the following aspects. (1) 0.5 to 35% by mass of an oily material, 1 to 80% by mass of a water-soluble substance, 5 to 70% by mass of water, and 30 to 1,200% by mass of a protein material having the following properties as a crude protein amount. % and having an emulsified particle size of 100 nm or less.
• the protein material has a viscosity of 10,000 mPa s or less when measured at 25°C after heating an aqueous solution of 20% by mass of crude protein at 80°C for 30 minutes, and the solubilization rate of 0.22M TCA is 30% or higher. It has 95% properties.
• the oil-in-water emulsion according to any one of (1) to (5) which has a water content of 65% by mass or less.
• the oil-in-water emulsion according to any one of (1) to (6) which does not contain an emulsifier.
• the oily material of the present invention refers to a substance that is insoluble or sparingly soluble in water and easily soluble in neutral lipids.
• examples include triglycerides such as oils, those modified by transesterification, hydrogenation, etc., and fatty acids obtained by decomposing these.
• Fatty acids also include polyunsaturated fatty acids (eg, eicosapentaenoic acid, docosahexaenoic acid, arachidonic acid and gamma-linolenic acid and/or ethyl esters), and the like.
• polyunsaturated fatty acids eg, eicosapentaenoic acid, docosahexaenoic acid, arachidonic acid and gamma-linolenic acid and/or ethyl esters
• an oily material having a melting point of 40° C. or lower is preferable, triglycerides having the same melting point are more preferable, and medium-chain fatty acid oils (MCT) are most preferable.
• MCT medium-chain fatty acid oils
• oil-soluble substances listed below can be added for the purpose of imparting physiological functions, coloring, or flavoring, but these have boiling points higher than that of water. That is, one selected from natural fragrance materials such as essential oils, extracts, oleoresins, recovered flavors, and isolated fragrances, and synthetic fragrance materials such as alcohols, esters, aldehydes, ketones, and lactones. Mixed flavors, carotenoids and carotenoid derivatives (e.g.
• antioxidants such as fat-soluble vitamins, dibutylhydroxytoluene (BHT), butylhydroxyanisole (BHA), licorice oil extract, sesame oil unsaponifiables, ⁇ -oryzanol, rapeseed oil extract, and L-ascorbic acid ester.
• Methanol, ethanol, isopropanol, propanol, acetone, methyl ethyl ketone, hexane, heptane, ethyl acetate, etc. are not applicable since they have lower boiling points than water.
• the protein material used in the present invention is required to have a low viscosity after heating. That is, it can be measured by preparing an aqueous solution of the protein material with a crude protein content of 20% by mass, heating it at 80°C for 30 minutes, and then measuring the viscosity at 25°C.
• the viscosity after heating is 10,000 mPa ⁇ s or less, preferably 5,000 mPa ⁇ s or less, 1,000 mPa ⁇ s or less, 500 mPa ⁇ s or less, and more preferably 200 mPa ⁇ s or less, 100 mPa ⁇ s or less.
• the present protein material requires a molecular weight of a certain size. Molecular weight is defined by the TCA solubilization rate.
• the TCA solubilization rate is defined as the ratio of crude protein dissolved in 0.22M TCA to total crude protein.
• the TCA solubilization rate is 30-95%, preferably 35-90%, more preferably 40-85%, 50-80%. If the TCA solubilization rate is too low, the viscosity tends to increase after heating, which is not appropriate, and the transmittance decreases. On the other hand, if the TCA solubilization rate is too high, the amount of protein that contributes to emulsifiability will decrease, and it will be necessary to add a large amount of protein material, which reduces the degree of freedom in blending, which is not preferable.
• the present protein material preferably has an NSI (Nitrogen Solubility Index) of 80 or higher, which is used as an index of protein solubility. More preferably, those having an NSI of 85 or higher, 90 or higher, 95 or higher, or 97 or higher can be used.
• a high NSI of a protein material indicates high dispersibility in water, and can contribute to the dispersion stability of the oil-in-water emulsion composition of the present invention. If the NSI is too low, precipitation tends to occur, which is not preferred.
• the crude protein content in the protein material is preferably 30% by mass or more, more preferably 50% by mass or more, and most preferably 70% by mass or more.
• a protein material with a higher crude protein content can exhibit its function with a smaller amount. Although such protein material is not generally commercially available, it can be obtained by the denaturation and molecular weight adjustment treatment described later. Commercially available soybean protein materials such as Fujipro R, Fujipro 748, Fujipro CL, and Hinute AM (manufactured by Fuji Oil Co., Ltd.) do not meet this requirement.
• the origin of the protein material to be prepared is not particularly limited, but proteins derived from plants, animals or microorganisms can be used.
• Vegetable proteins include beans such as soybeans, peas, mung beans, lupine beans, chickpeas, kidney beans, lentils and cowpeas, seeds such as sesame seeds, canola seeds, coconut seeds and almond seeds, corn, buckwheat, wheat, Examples include proteins derived from grains such as rice, vegetables, fruits, algae, microalgae, and the like.
• soybean-derived protein material it is prepared by further concentrating protein from soybean raw materials such as defatted soybeans and whole soybeans. Alternatively, variously processed products thereof are conceptually included.
• animal proteins include egg proteins including ovalbumin, milk proteins such as casein, whey, lactalbumin, and lactalbumin, proteins derived from blood such as blood plasma, serum albumin, and bleached hemoglobin, and meat-derived proteins.
• milk proteins such as casein, whey, lactalbumin, and lactalbumin
• proteins derived from blood such as blood plasma, serum albumin, and bleached hemoglobin
• meat-derived proteins examples include proteins, proteins derived from fish and shellfish, and the like.
• proteins derived from microorganisms such as yeast, fungi, and bacteria can be used. Even proteins that are poorly soluble in water can be used in the present invention by the treatment described below.
• the protein material used in the oil-in-water emulsion of the present invention is applied in combination with "degradation/denaturation treatment” for degrading and/or denaturing the protein and "molecular weight distribution adjustment treatment” for adjusting the molecular weight distribution of the protein.
• degradation/denaturation treatment include enzyme treatment, pH adjustment treatment (e.g., acid treatment, alkali treatment), denaturant treatment, heat treatment, cooling treatment, high pressure treatment, organic solvent treatment, mineral addition treatment, supercritical treatment, sonication, electrolysis, combinations thereof, and the like.
• Examples of the “molecular weight distribution adjusting treatment” include filtration, gel filtration, chromatography, centrifugation, electrophoresis, dialysis, and combinations thereof.
• the order and number of times of the “decomposition/denaturation treatment” and “molecular weight distribution adjustment treatment” are not particularly limited, and the “decomposition/denaturation treatment” may be followed by the “molecular weight distribution adjustment treatment”, or the “molecular weight distribution adjustment treatment” may be performed. Treatment” may be followed by "decomposition/denaturation treatment", or both treatments may be performed at the same time.
• “degradation/denaturation treatment” is performed between two or more “molecular weight distribution adjustment treatments”
• “molecular weight distribution adjustment treatment” is performed between two or more “degradation/denaturation treatments”, each multiple times. , etc.
• the desired molecular weight distribution can be obtained by the "decomposition/denaturation treatment”
• the “molecular weight distribution adjustment treatment” may not be performed.
• all the treatments starting from the raw material may be carried out continuously, or may be carried out after an interval of time.
• a commercial product that has undergone a certain treatment may be used as a raw material and subjected to another treatment.
• a protein material that has undergone molecular weight distribution adjustment treatment and a protein material that has not undergone molecular weight distribution adjustment treatment may be mixed to form a specific protein material.
• the ratio of the two (treated protein material: untreated protein material) can be adjusted as appropriate within the range satisfying the above characteristics, but the mass ratio is, for example, 1:99 to 99:1, for example, 50 : 50-95:5, 75:25-90:10 and the like.
• the protein material used in the oil-in-water emulsion of this aspect is a protein material that has undergone "degradation/denaturation/molecular weight distribution adjustment treatment".
• a person skilled in the art can appropriately set the processing conditions for protein decomposition or denaturation, such as the types and concentrations of enzymes, pH, organic solvents, minerals, etc., temperature, pressure, output intensity, current, time, etc.
• enzymes examples include proteases classified into “metalloproteases,” “acid proteases,” “thiol proteases,” and “serine proteases.”
• the reaction temperature is 20 to 80°C, preferably 40 to 60°C.
• any of pH 2, 2.5, 3, 3.5, 4, 4.5, 5, 5.5, 6, 6.5, 7, 7.5, 8, 8.5, 9, 9.5, 10, 10.5, 11, 11.5, 12 can be treated in a pH range with upper and lower limits, eg, pH 2-12.
• acid treatment it may be a method of adding acid or a method of carrying out fermentation treatment such as lactic acid fermentation.
• acids to be added include inorganic acids such as hydrochloric acid and phosphoric acid; Organic acids are mentioned.
• acid may be added using acid-containing foods and drinks such as fruit juice such as lemon, concentrated fruit juice, fermented milk, yogurt, and brewed vinegar.
• alkali treatment an alkali such as sodium hydroxide or potassium hydroxide can be added.
• denaturant treatment denaturants such as guanidine hydrochloride, urea, arginine, PEG, etc. may be added.
• heating or cooling treatment examples of heating temperatures are 60°C, 70°C, 80°C, 90°C, 100°C, 110°C, 120°C, 125°C, 130°C, 135°C, 140°C, 145°C, and 150°C. °C with any upper and lower limit, such as 60°C to 150°C.
• cooling temperatures are -10°C, -15°C, -20°C, -25°C, -30°C, -35°C, -40°C, -45°C, -50°C, -55°C, -60°C, Ranges with upper and lower limits of -65°C, -70°C, and -75°C, such as -10°C to -75°C.
• heating or cooling times are 5 seconds, 10 seconds, 30 seconds, 1 minute, 5 minutes, 10 minutes, 20 minutes, 30 minutes, 40 minutes, 50 minutes, 60 minutes, 70 minutes, 80 minutes, 90 minutes, Ranges with upper and lower limits of 100 minutes, 120 minutes, 150 minutes, 180 minutes, and 200 minutes, such as 5 seconds to 200 minutes.
• examples of pressure conditions are 100 MPa, 200 MPa, 300 MPa, 400 MPa, 500 MPa, 600 MPa, 700 MPa, 800 MPa, 900 MPa, and 1,000 MPa. mentioned.
• examples of solvents used include alcohols and ketones such as ethanol and acetone.
• examples of minerals used include divalent metal ions such as calcium and magnesium.
• supercritical treatment for example, carbon dioxide in a supercritical state at a temperature of about 30° C. or higher and about 7 MPa or higher can be used.
• treatment can be performed by irradiating with a frequency of 100 KHz to 2 MHz and an output of 100 to 1,000 W.
• electrolysis treatment for example, a protein aqueous solution can be treated by applying a voltage of 100 mV to 1,000 mV.
• the treatment that degrades and/or denatures proteins is selected from denaturant treatment, heat treatment, and combinations thereof.
• a person skilled in the art can appropriately set the processing conditions for adjusting the molecular weight distribution of proteins, such as the type of filter medium, gel filtration carrier, centrifugation speed, current, and time.
• filter media include filter paper, filter cloth, diatomaceous earth, ceramics, glass, membranes, and the like.
• carriers for gel filtration include dextran and agarose.
• centrifugation conditions include 1,000-3,000 ⁇ g for 5-20 minutes.
• the continuous phase of the oil-in-water emulsion of the present invention is an aqueous solution of the protein material described above, and the amount of water in this case is preferably small. To reduce the water in the aqueous solution, it is necessary to replace the water with a readily water-soluble substance.
• the water-soluble substance used in the present invention means a substance having a solubility in water of 30 (g/100g) or more, preferably 60 (g/100g) or more, more preferably 100 (g/100g) or more. and most preferably, it can be mixed and dissolved with water in any proportion. It also has a higher boiling point than water.
• the substance is preferably an inorganic salt or an organic substance containing no nitrogen, and polyhydric alcohols containing sugars can be exemplified as the organic substance.
• Polyhydric alcohol is a general term for compounds having two or more hydroxyl groups in one molecule, and the type is not particularly limited.
• glycerin propylene glycol, sorbitol, maltitol, xylitol, erythritol, lactitol, sorbitan, xylose, arabinose, mannose, trehalose, lactose, sugar, coupling sugar, glucose, enzyme starch syrup, acid-saccharified starch syrup, maltose starch syrup, maltose, Examples include isomerized sugar, fructose, reduced maltose, reduced starch starch syrup, and honey. These can be used alone or in combination of two or more.
• salts chlorides, nitrates, sulfates, etc., phosphates or organic acid salts of monovalent or divalent metals such as sodium, potassium, calcium, and magnesium, or with ammonium, which satisfy the above solubility. things are mentioned. Examples include sodium chloride, ammonium sulfate, sodium dihydrogen phosphate, and sodium lactate.
• emulsifiers other than the protein materials described above do not need to be positively blended.
• inclusion of an emulsifier during the emulsification process may not be preferable in terms of quality.
• the emulsifiers referred to herein include synthetic emulsifiers and natural emulsifiers.
• emulsifiers such as monoacylglycerol, diacylglycerol, polyglycerin fatty acid ester, sucrose fatty acid ester, sodium stearoyl lactylate, calcium stearoyl lactylate, polyoxyethylene derivatives, fatty acid salts, modified starch, enzymatically decomposed lecithin, Derivatives of lecithin obtained by chemically or enzymatically treating naturally occurring lecithins such as hydrogenolytic lecithin, hydroxyl lecithin, phosphatidylglycerol, phosphatidic acid, and acetylated lecithin; and saponins.
• emulsifiers also include proteins that do not meet the above requirements for protein materials, such as milk casein and lactalbumin that have not been treated according to the present invention, as long as they have emulsifiability.
• the formulation is explained below. An aqueous phase and an oil phase are prepared separately, but finally the total amount is adjusted to 100 parts by mass using the following compounding ratio. While it is difficult to prepare an oil-in-water emulsion that is a nanoemulsion if the formulation is deviated from the formulation, an oil-in-water emulsion with a smaller particle size can be obtained with a preferable formulation.
• the oil phase is 0.5 to 35 parts by mass, preferably 1 to 30 parts by mass, more preferably 2 to 15 parts by mass as an oily material.
• the aqueous phase has the following composition.
• the protein material is 30 to 1,200 mass %, preferably 60 to 400 mass % of the oil and fat material in terms of crude protein content.
• the amount of crude protein satisfies the following.
• the amount of crude protein is 1 to 20 parts by mass, preferably 5 to 15 parts by mass, more preferably 10 to 12 parts by mass in 100 parts by mass of the total amount.
• Water is 5 to 70 parts by mass, preferably 65 parts by mass or less, more preferably 35 parts by mass or less, and most preferably 20 parts by mass or less.
• the easily water-soluble substance is 1 to 80 parts by mass, preferably 10 to 70 parts by mass, more preferably 40 to 65 parts by mass.
• the total weight of the water-soluble substance and water is preferably 2 times or more, more preferably 4 times or more, and most preferably 6 times or more, that of the protein material.
• the preparation method will be described below, but first, the preparation of the aqueous phase will be described.
• the protein material and the easily water-soluble substance are added to water and dissolved by stirring or the like.
• the temperature of the water to be used is not particularly limited, but warm water is preferable, and 60 to 80°C is suitable. If the temperature is too low, the viscosity increases and the workability deteriorates.
• the protein material used in the present invention is characterized by having a low viscosity after heating, and the water phase prepared here also exhibits a low viscosity in spite of its high crude protein concentration. Next, the preparation of the oil phase will be explained.
• the oil phase is the above-described oily material, and usually triglycerides alone or triglycerides added with oily materials other than triglycerides such as the above-described oil-soluble substances are used. Heating is preferable depending on the fatty acid that also constitutes the oil phase, and in many cases, the preparation is carried out at the melting point or above.
• Preliminary emulsification is to prepare an oil-in-water emulsion having a particle size of about 10 to 100 ⁇ m by treating with a homomixer or the like.
• the number of revolutions varies depending on the equipment, but in the case of HOMOGENIZING MIXER MARK II Model 2.5 manufactured by PRIMIX, for example, processing is performed at 8000 rpm for about 10 minutes. This is followed by main emulsification.
• Emulsification is not particularly limited, but emulsification equipment with high shearing force is preferred, and examples thereof include homomixers, colloid mills, high-pressure homogenizers, ultrahigh-pressure homogenizers, and vacuum emulsifiers.
• APV Gaulin homogenizer manufactured by APV
• Microfluidizer manufactured by Microfluidex
• Ultimizer manufactured by Sugino Machine
• Nanomizer manufactured by Nanomizer
• a microfluidizer it is effective to perform shearing treatment at a pressure of preferably 100 MPa or higher, more preferably 150 MPa or higher, twice or more, preferably four times or more, more preferably ten times or more.
• a homogenizer such as an ultrasonic emulsifier may be used.
• ultrasonic homogenizers US-600, US-1200T, RUS-1200T, and MUS-1200T manufactured by Nippon Seiki Seisakusho Co., Ltd.
• ultrasonic processors UIP-2000, UIP-4000, and UIP-8000, UIP-16000 both manufactured by Hielscher
• These high power ultrasonic irradiation devices are used at frequencies below 25 kHz, preferably between 15 and 20 kHz.
• the emulsion particle size is 100 nm or less, preferably 85 nm or less, more preferably 60 nm or less. If the emulsified particle size exceeds 100 nm, the transparency will be lowered, which is not suitable for the present invention.
• the emulsion of the present invention and its raw material are evaluated according to the following procedures. ⁇ moisture content> Determined by normal pressure heat loss method (105°C for 12 hours).
• the nitrogen conversion factor is 6.25. Basically, it is obtained by rounding off the second decimal place.
• ⁇ NSI> Add 60 ml of water to 3 g of the sample, stir with a propeller at 37° C. for 1 hour, centrifuge at 1400 ⁇ g for 10 minutes, and collect the supernatant (I). Next, 100 ml of water is added to the remaining precipitate, and the mixture is stirred again at 37°C for 1 hour with a propeller, and then centrifuged to collect the supernatant (II). Combine solution (I) and solution (II), and add water to the mixture to bring the total volume to 250 ml. After filtering this with filter paper (No. 5), the nitrogen content in the filtrate is measured by the Kjeldahl method.
• the amount of nitrogen in the sample is measured by the Kjeldahl method, and the ratio of the amount of nitrogen (water-soluble nitrogen) recovered as a filtrate to the total amount of nitrogen in the sample is expressed as mass % and defined as NSI. Basically, it is obtained by rounding off the second decimal place.
• TCA soluble rate An equal amount of 0.44M trichloroacetic acid (TCA) is added to a 2% by mass aqueous solution of the protein material to make a 0.22M TCA solution, and the ratio of soluble nitrogen is determined by the Kjeldahl method. Basically, it is obtained by rounding off the second decimal place.
• Viscosity (viscosity after heating)> The viscosity of the protein material is measured using a B-type viscometer (manufactured by Toki Sangyo Co., Ltd., type BM). A protein material aqueous solution is prepared so that the amount of crude protein is 20% by mass, filled in a measurement container, a rotor is set, and after sealing, heat in a hot water bath at 80°C for 30 minutes. Next, measure at an arbitrary number of revolutions at 25°C, read the indicator value, and multiply the rotor No. by a conversion multiplier corresponding to the number of revolutions to calculate the viscosity. (Unit: Pa ⁇ s) Measured value after 1 minute. The rotation speed is basically 60 rpm.
• ⁇ Emulsion particle size> The emulsion is diluted with water so that the content of the oily material is 0.03% by mass, and used as a sample.
• the z-average size is measured at 25° C. with a Malvern zetasizer nano-zs.
• Transparency The emulsion is diluted with water so that the content of the oily material is 0.5% by mass, and used as a sample.
• Transmittance T (%) is measured at a wavelength of 660 nm with UV-1900 manufactured by Shimadzu Corporation using a quartz cell with a light path of 1 cm. In the present invention, transparency is defined as a transmittance of 50% or more.
• the emulsified formulation oil-in-water emulsion of the present invention can be applied to all processed foods, beverages, and health foods to which an oily substance is desired.
• oil-soluble functional substances having physiological functions include the above-mentioned fat-soluble vitamins, pigments such as carotenoids, polyunsaturated fatty acids, plant sterols, plant estrogens, and the like.
• Instant noodles, retort food, instant food such as instant miso soup, clear soup, soup, carbonated drinks, fruit juice drinks, vegetable drinks, coffee drinks, sports drinks, tea drinks, alcoholic beverages, bread, pasta , noodles, flour products such as cake mixes, candy, chewing gum, chocolate, biscuits, snacks, Japanese confectionery, rice confectionery, confectionery such as dessert confectionery, sauces, curry ingredients, sauces, sauces, dressings, etc.
• Seasonings, oily foods such as butter, mayonnaise, margarine, processed milk, milk drinks, yogurts, lactic acid beverages, cheese, ice cream, dairy products such as cream, frozen foods, fish paste products, hams and sausages, Jams, marmalades, pickles, canned foods, etc.
• the present invention by transparently dispersing an oily material in a water system, it is possible to improve the commercial value of foods that require transparency.
• the oily material to be dispersed include the above-mentioned perfumes and pigments such as carotenoids.
• foods to which this effect can be suitably applied include instant foods such as instant soups and soups, carbonated beverages, fruit juice beverages, vegetable beverages, coffee beverages, sports drinks, tea and black tea beverages, alcoholic beverages and other beverages.
• confectionery such as candy, chewing gum, Japanese confectionery, and dessert confectionery; seasonings such as sauces, sauces, and dressings; frozen desserts, frozen desserts, jams and marmalades;
• Some aspects of the present invention can strongly impart to foods the effect of enhancing richness due to the inclusion of oils and fats.
• the full-bodied taste referred to here is the voluminous and rich feeling felt after the food is put into the oral cavity and after it is swallowed.
• the oil-in-water emulsion which is the nanoemulsion of the present invention, this richness can be expressed very strongly.
• the present invention it is possible to reduce the blending amount of fats and oils while maintaining deliciousness (rich taste).
• foods to which this effect can be suitably applied include instant noodles, retort foods, instant foods such as soups, bread, pasta, noodles, flour products such as cake mixes, chocolates, biscuits, snacks, desserts, and the like.
• Confectioneries, sauces, curry ingredients, seasonings such as dressings, fat foods such as butter, mayonnaise, margarine, processed milk, milk drinks, yogurts, lactic acid beverages, cheese, ice cream, cream, etc.
• dairy products, frozen foods, fish paste products, hams and sausages, and canned foods but are not limited to these.
• bitterness, astringency, and rough taste derived from the emulsifier are imparted at the same time, which is not suitable.
• the present invention can reduce the water activity to 0.4 or less, and can greatly improve the storage stability of the solubilized nanoemulsion. Specifically, water activity can be lowered by reducing water and increasing water-soluble substances. Glycerin, sorbitol, fructose, sucrose and the like are effective as water-soluble substances, and the water content in this case is preferably 20% by mass or less, more preferably 10% by mass or less.
• the present invention can expand the utility of solubilized nanoemulsions that can be powdered.
• the oil-in-water emulsion that is the nanoemulsion described above can be dried and pulverized as it is, diluted, or added with other substances.
• Other substances include carbohydrates such as dextrin and cellulose, protein materials, peptides, amino acids, salts and the like.
• Powderization includes spray drying, freeze drying, vacuum drying, and the like. By dissolving the dried product of the present invention in a solvent such as water, it becomes an oil-in-water emulsion again, and it is possible to maintain a nanoemulsion with an emulsified particle size of 100 nm or less.
• Oil-based material As oil-based materials, "fat and oil” containing triglyceride as a main component were used as fats A to F below, all of which were melted.
• Oil A Rapeseed oil (salad oil for confectionery, manufactured by Fuji Oil Co., Ltd.) Fats and oils B: Medium-chain fatty acid triglyceride (MCT-64, manufactured by Fuji Oil Co., Ltd.)
• Oil C Palm olein (Palm Ace N, manufactured by Fuji Oil Co., Ltd.)
• Oil D Coconut oil (commercially refined coconut oil (melting point: 24°C), manufactured by Fuji Oil Co., Ltd.)
• Oil E Cocoa butter (cocoa butter 201 (melting point: 33 ° C), manufactured by Fuji Oil Co., Ltd.) Fats F: High erucic acid rapeseed extremely hardened oil (High erucic acid rapeseed hardened oil (melting point 61 ° C), manufactured by Yokozeki Oil Industry Co.
• Oil-soluble substances A to D were used as oil-based materials other than the above oils and fats.
• Oil-soluble substance A Vitamin E preparation (Emix-70L (68.0% or more as total tocopherol), manufactured by Tama Biochemical Co., Ltd.)
• Oil-soluble substance B Oil containing 10% ⁇ -carotene. Mix 10 parts by mass of ⁇ -carotene 30% suspension ( ⁇ -carotene 30% suspension, manufactured by DSM Nutritional Products) and 20 parts by mass of medium-chain fatty acid triglycerides, and heat at 120°C for 10 minutes in a nitrogen atmosphere. Heating was performed, and a clear mixed solution containing 10% ⁇ -carotene was used.
• Oil-soluble substance C Oil containing 50% d-limonene.
• Oil-soluble substance D Oleic acid (Lunac OV, manufactured by Kao Corporation)
• Soybean protein material A A product processed by decomposition/denaturation and molecular weight distribution adjustment of isolated soybean protein. (Fuji Oil Co., Ltd. test product, moisture content 1.2%, crude protein content 79.3%, TCA solubilization rate 61.8%, viscosity after heating 28 mPa s, NSI 98.1)
• Raw material Isolated soy protein Fujipro R (manufactured by Fuji Oil Co., Ltd.) , crude protein content 87.2%, TCA solubilization rate 3.2%)
• Pea protein material A Product processed by decomposition/denaturation/adjustment of molecular weight distribution of pea protein.
• Raw material almond milk powder PP-CS (manufactured by Tsukuba Dairy Co., crude protein content 28.8%)
• Wheat protein material A Decomposed/denatured wheat protein product (Fuji Oil Co., Ltd.
• Raw material powdered wheat protein V-75 (manufactured by Glico Nutrition Foods, crude protein content 71.8%)
• Whey protein material A Decomposed/denatured whey protein product (Fuji Oil Co., Ltd.
• Soy protein material B (Fujipro R, manufactured by Fuji Oil Co., Ltd., crude protein content 87.2%, TCA solubilization rate 3.2%, viscosity after heating 100,000 mPa s or more, NSI 81.2)
• Soybean protein material C (Fujipro 748, manufactured by Fuji Oil Co., Ltd., crude protein content 86.1%, TCA solubilization rate 9.8%, viscosity after heating 100,000 mPa ⁇ s or more, NSI 94.5) was used.
• Soy protein material D (Fujipro CL, manufactured by Fuji Oil Co., Ltd., crude protein content 88.0%, TCA solubilization rate 23.0%, viscosity after heating 100,000 mPa ⁇ s or more, NS I 65.0) was used.
• Soybean protein material E (Hinute AM, manufactured by Fuji Oil Co., Ltd., crude protein content: 90.0%, TCA solubilization rate: 100.0%, viscosity after heating: 20 mPa ⁇ s, NSI: 100) was used.
• Pea protein material B manufactured by PP-CS Organo Foodtech Co., Ltd., crude protein content 79.1%, TCA solubilization rate 0.0%, viscosity after heating 100,000 mPa ⁇ s or more, NSI 87.3 was used.
• Sodium caseinate (SodiumCaseinate 180, manufactured by Fonterra, crude protein content 92.3%, TCA solubilization rate 0.0%, viscosity after heating 100,000 mPa ⁇ s or more, NSI 98.1) was used.
• whey protein material B (WPC80, manufactured by Warrnambool Cheese & Butter Pty Ltd., crude protein content 78.9%, TCA solubilization rate 0.0%, viscosity after heating 100,000 mPa s or more, NSI 98.2) .
• An oil-in-water emulsion which is a nanoemulsion, was prepared as follows. Namely. a) Each protein material, water-soluble substance and water are dissolved in water having a temperature of 65°C according to the formulation shown in Table 1, and the water phase is mixed using a homogenizing mixer (HOMOGENIZING MIXER MARK II Model 2.5, manufactured by PRIMIX). was prepared. b) An oily material was added to the water phase of step a) according to the formulation shown in Table 1, and pre-emulsified using a homomixer at 65°C for 5 minutes to an emulsified particle size of 10 to 60 ⁇ m.
• a homogenizing mixer HOMOGENIZING MIXER MARK II Model 2.5, manufactured by PRIMIX
• step b) The mixture in step b) was treated with a high-pressure homogenizer (manufactured by Microfluidizer, Microfluidics) at a predetermined pressure to prepare an oil-in-water emulsion that is a nanoemulsion.
• a high-pressure homogenizer manufactured by Microfluidizer, Microfluidics
• the following was used as a readily water-soluble substance.
• Glycerin manufactured by Shokuhin Kishida Chemical Co., Ltd., solubility in water: arbitrary, boiling point 290°C
• sorbitol manufactured by Bussan Food Science, solubility in water: arbitrary, boiling point 296°C
• maltose ("Sunmalt", Hayashibara Co., Ltd.) product, solubility in water: 1.08g/ml, 20°C, boiling point data not available
• sodium chloride manufactured by Fujifilm Wako Pure Chemical Industries, solubility in water: 35.9g/100g, 25°C, boiling point: 1413°C
• L - Sodium ascorbate manufactured by Fujifilm Wako Pure Chemical Industries, solubility in water: 62 g/100 ml, 25°C, boiling point 235°C).
• Embodision particle size measurement The sample oil-in-water emulsion was diluted with deionized water so that the oil content was 0.03%.
• the particle size of oil droplets in water was measured as a calculated Z-average (nm) using Zetasizer nano-ZS (MODEL ZEN3600) manufactured by Malvern. The measurement was carried out 3 times at 25° C. in a glass cell with a light path of 1 cm for 2 g of the sample, and the average value was taken as the average emulsified particle size.
• the setting conditions were as follows.
• RI (Material) 1.47, Absorption (Material) 0, Temperature (Dispersant) 25 (°C), Viscosity (Dispersant) 0.887 (cp), RI (Dispersant) 1.33, Equilibration time 60 (sec), Number of runs 10, Run duration 10, Number of measurements 1, Dela betwee measurements 0 (sec).
• Examples 1 to 7 acceptable quality was obtained by using the soybean protein material A with a moisture content of 60% or less and a glycerin content of 13.5% or more.
• Examples 4 to 7 had a particle size of less than 60 nm and were of particularly good quality.
• acceptable quality was obtained when the blending amount of the oily material was 27% or less.
• Examples 9 and 10 had a particle size of less than 60 nm and were of particularly good quality.
• a highly transparent emulsion having an emulsified particle size of 100 nm or less was obtained even with a high oil content.
• the water activity of Example 6 was 0.39, and the water activity of Example 5 was 0.31, both of which were very low.
• the water activity value (Aw) was measured using a water activity measuring device TH200 (manufactured by NOVASINA).
• Examples 19 to 22 acceptable quality was obtained by high-pressure emulsification treatment of 2 or more passes at 150 MPa.
• Examples 21 and 22 had a particle size of less than 60 nm and were of particularly good quality.
• acceptable quality was obtained by high-pressure emulsification treatment of 50 MPa or more.
• Example 25 had a particle size of less than 60 nm and was of particularly good quality. From the above, when the microfluidizer was used in the present invention, a high-pressure emulsification treatment of at least 50 MPa was required.
• Example 26 to 35 acceptable quality was obtained regardless of the room temperature solid fat and fatty acid chain length.
• Example 30 has a slightly larger particle size, which is considered to be due to operational problems due to the high melting point.
• the antioxidant component in Example 32 the pigment/physiologically active substance in Example 33, and the perfume component in Examples 34 and 35 all achieved acceptable quality. From the above, it was found that the present invention can obtain a highly transparent emulsion with an emulsified particle size of 100 nm or less, regardless of the material, as long as it is oil-soluble.
• Example 46 The emulsion of Example 43 was spray dried to obtain Example 46, an emulsified powder.
• the spray drying was carried out at an inlet temperature of 140°C and an outlet temperature of 90°C, and the water content of the dried product was 3.0% by the normal pressure heating weight loss method.
• the particle size was 69.2 nm
• the transmittance (T%) was 80.3
• the nanoemulsion was maintained. From this, it was found that the emulsion of the present invention can be dried, does not lose its quality when re-dissolved, and can significantly reduce restrictions on distribution and use.
• the present invention when used to impart flavor to foods, it exhibits a stronger flavor than oil-in-water emulsions having a particle size of more than 100 ⁇ m, and has a high function as a body-imparting agent.
• a sample was prepared by diluting the emulsion with water so that each oily material was 0.1% by mass.
• Four skilled panelists tasted water-diluted emulsions of the emulsions obtained in Examples and Comparative Examples, and carried out a sensory evaluation of the richness according to the following evaluation criteria.
• the full-bodied taste as used herein means the feeling of volume and richness that is felt from after the food is put into the oral cavity until after it is swallowed.
• the evaluation was based on the following criteria, and the richness was given 5 to 0 points. That is, 5 points: very good (feeling very strong aftertaste), 4 points: good (feeling strong body), 3 points: normal (feeling richness), 2 points: somewhat poor (feeling slightly) , 1 point: Poor (almost no richness is felt in the aftertaste), 0 point: Equivalent to water. A score of 3 or more was regarded as passing. Table 7 shows the average values of the panel evaluations. It was confirmed that the richness of the taste is strongly expressed as the particle size becomes smaller. In addition, the expression of richness was not affected by sugar or salt. It is one of the major features of the present invention that a similar effect can be obtained with a triglyceride emulsion instead of a taste substance.
• an oil-in-water emulsion having a particle size of 100 nm or less can be obtained without using a synthetic emulsifier. This makes it possible to prepare an oil-based material-containing emulsion with excellent transparency and good flavor and apply it to foods and the like.

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• 2023
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