Powder composition
A powder composition with a specific substrate surface area and pore volume supports oily components effectively, addressing fluidity and dispersibility issues while reducing volatilization and oxidation, enhancing handling and application in various products.
Patent Information
- Authority / Receiving Office
- JP · JP
- Patent Type
- Patents
- Current Assignee / Owner
- UENO FOOD TECHNO IND LTD
- Filing Date
- 2022-03-18
- Publication Date
- 2026-07-07
AI Technical Summary
Existing powdered oily compositions suffer from poor fluidity, low dispersibility in water, and issues with volatilization and oxidation of oily components during drying processes, leading to inadequate support and handling of oily components.
A powder composition is developed using a powdered substrate with a specific surface area of 5.0 m² and a pore volume of 0.45 mL/g, impregnated with an oily component at a concentration of 0.45 mL/g or more, ensuring excellent fluidity and dispersibility.
The composition achieves high oily component support, improved fluidity, and enhanced dispersibility in water, minimizing volatilization and oxidation, with a preferred impregnation rate of 1 to 50% by weight.
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Abstract
Description
Technical Field
[0001] The present invention relates to a powder composition containing an oily component supported on a powdered substrate.
Background Art
[0002] Oily components such as fats and oils, fat-soluble vitamins, and fat-soluble drugs are used for various products such as foods and drinks, cosmetics, fragrances, pharmaceuticals, quasi-drugs, and daily necessities according to the purpose.
[0003] Many of such oily components are liquid or semi-solid at normal temperature and are inconvenient to handle, so the use of powdered oily components has been increasing. As methods for powdering oily components, those obtained by supporting an oily component on a powdered substrate or by suspending an oily component in a solution of a powdered substrate and then drying are known. However, in the powdering method of supporting on a powdered substrate, the fluidity and dispersibility are poor, and the retention amount of the oily component is also small, so the convenience as a powder is insufficient. Further, in the powdering method involving a drying process, a polymeric powdered substrate is used, and the obtained powder has low dispersibility in water, so there is a problem that the oily component is likely to separate. Furthermore, depending on the type of the oily component, due to heating during the drying treatment, volatilization of the oily component and alteration due to an oxidation reaction occur, so improvement has been demanded.
[0004] Patent Document 1 describes a powder composition obtained by adding soluble starch or polyol to an aqueous solution of a starch decomposition product, using a powdered substrate dried with a drum dryer, and supporting an oily component such as α-pinene or salad oil. However, the powder supporting the oily component has poor fluidity, and it is difficult to say that the supported amount is sufficient.
[0005] Patent Document 2 proposes a powder composition obtained by suspending an oily component in an aqueous solution of highly branched cyclic dextrin and drying it in a drum dryer or freeze dryer. However, due to the low water solubility of the powdered base material, the dispersibility in the final product was insufficient. Furthermore, special equipment was required for its manufacture.
[0006] Patent Document 3 proposes a powder composition in which an oil-soluble component, an emulsifier, maltotriose, and water are emulsified using an emulsifier, and then dried using a spray dryer. However, although solubility and dispersibility in water were improved, the problem of deterioration due to volatilization and oxidation of the oil-soluble component remained unresolved because heating was performed during the drying process. Furthermore, the process was complicated and had other problems.
[0007] Therefore, in a powdered composition of oily components, there has been a need for a powder composition in which the volatilization and oxidation of the oily components are suppressed, the powder has excellent fluidity, and has excellent dispersibility in water. [Prior art documents] [Patent Documents]
[0008] [Patent Document 1] Japanese Patent Application Publication No. 8-143603 [Patent Document 2] Japanese Patent Publication No. 2007-238824 [Patent Document 3] Japanese Patent Publication No. 2006-000087 [Overview of the project] [Problems that the invention aims to solve]
[0009] The present invention aims to provide a powder composition that has a large amount of oily component support, excellent fluidity, and improved dispersibility of the oily component in products, etc. [Means for solving the problem]
[0010] As a result of diligent research, the inventors have found that a specific oily component has a specific surface area of 5.0 m² as measured by the BET (Brunauer-Emmett Teller) single-point method. 2 We discovered that the above problems can be solved by supporting the sorbitol on a powdered substrate containing sorbitol at a concentration of 0.45 mL / g or more and a pore volume of 0.45 mL / g or more as determined by mercury intrusion, and thus completed the present invention.
[0011] In other words, the present invention relates to a powder composition containing an oily component supported on a powdered substrate, wherein the oily component is a substance that has a solubility in water of 1 g / 100 mL or less and is liquid at room temperature, and the powdered substrate has a specific surface area of 5.0 m² as measured by the BET single-point method. 2 The present invention provides a powder composition containing sorbitol in an amount of 0.45 mL / g or more and having a pore volume of 0.45 mL / g or more as determined by mercury intrusion, wherein the impregnation rate of the oily component into the powdered substrate is 1 to 50% by weight. [Modes for carrying out the invention]
[0012] The present invention will be described in detail below. The oily component that can be used in the powder composition of the present invention has a solubility in water of 1 g / 100 mL or less. Preferably, the solubility of the oily component in water is 0.8 g / 100 mL or less, and more preferably 0.5 g / 100 mL or less.
[0013] Furthermore, the oily components that can be used in the powder composition of the present invention must be liquid at room temperature, in addition to meeting the solubility requirements mentioned above. Substances that are solid at room temperature cannot be used because they are difficult to support on the powdered substrate. In this invention, room temperature refers to approximately 25°C.
[0014] The oily component may consist of a single chemical substance or a mixture. Examples of oily components include edible oils and fats, fragrances, and emulsifiers. Multiple oily components may be used in combination.
[0015] Edible oils and fats include vegetable oils that are liquid at room temperature, such as rapeseed oil, salad oil, soybean oil, cottonseed oil, safflower oil, sunflower oil, corn oil, and rice oil, as well as animal oils such as fish oil, liver oil, whale oil, and marine mammal oil. Among these edible oils and fats, rapeseed oil, salad oil, soybean oil, and fish oil are cited as preferred edible oils and fats, with rapeseed oil being cited as a particularly preferred edible oil and fat.
[0016] Examples of fragrances include citrus essential oils such as orange, mandarin, lemon, grapefruit, and lime; flower essential oils; plant essential oils such as mint oil, cypress oil, and spice oil; oily extracts such as nut extract, coffee extract, vanilla extract, cocoa extract, and black tea extract; synthetic fragrance compounds; oily blended fragrance compositions; and oily fragrances of any mixture thereof. Among these fragrances, citrus essential oils are preferred, and orange fragrance is exemplified as a particularly preferred fragrance.
[0017] As an emulsifier, an emulsifier with an HLB value of 8 or less is preferred, an emulsifier with an HLB value of 0.1 to 7.9 is more preferred, and an emulsifier with an HLB value of 0.5 to 7.5 is even more preferred. In this invention, the HLB value refers to the value measured by the Griffin method.
[0018] Specific examples of emulsifiers include liquid emulsifiers at room temperature such as glycerin fatty acid esters, polyglycerin fatty acid esters, sucrose fatty acid esters, sorbitan fatty acid esters, propylene glycol fatty acid esters, lecithin, and saponins. More specifically, sorbitan laurate, propylene glycol monooleate, and hexaglycerin condensed ricinolate are cited as preferred emulsifiers, with hexaglycerin condensed ricinolate being cited as a particularly preferred emulsifier.
[0019] In addition to the edible oils and fats, fragrances and emulsifiers mentioned above, oily components may include pesticide components such as metrachlor, pharmaceutical components such as ibuprofen piconol or teprenone, fat-soluble vitamins or their derivatives such as retinyl palmitate, tocopherol, and phylloquinone, and coenzymes such as ubiquinone Q10.
[0020] The powdered substrate of the present invention contains sorbitol (referred to as porous sorbitol in this specification) having a specific surface area of 5.0 m 2 / g or more by the BET single-point method and a pore volume of 0.45 mL / g or more by the mercury intrusion method. In certain embodiments, the powdered substrate consists of porous sorbitol.
[0021] The porous sorbitol can be produced, for example, by kneading molten sorbitol and ethanol and then drying under reduced pressure. In one preferred embodiment, the method for producing the porous sorbitol of the present invention comprises the following steps: a) A step of supplying molten sorbitol and ethanol into a kneading apparatus, b) A step of kneading the molten sorbitol and ethanol in the kneading apparatus while maintaining the temperature at 50 - 78°C, and c) A step of removing ethanol by drying the kneaded product obtained in b) under reduced pressure at 25 - 90°C and 100 - 30000 Pa is included.
[0022] Furthermore, the above manufacturing method will be described more specifically. First, in step a), 10 - 70 parts by weight of molten sorbitol and 30 - 90 parts by weight of ethanol are supplied into the kneading apparatus. The supply amount into the kneading apparatus is preferably 15 - 68 parts by weight of molten sorbitol and 32 - 85 parts by weight of ethanol, more preferably 20 - 65 parts by weight of molten sorbitol and 35 - 80 parts by weight of ethanol.
[0023] The water content contained in the ethanol used in step a) is, for example, 10% by weight or less. The water content contained in the ethanol is preferably 8% by weight or less, more preferably 5% by weight or less, still more preferably 2% by weight or less, and particularly preferably 0% by weight (ethanol only). The lower the water content contained in the ethanol, the more likely the specific surface area of the produced porous sorbitol is to increase.
[0024] Next, in step b), the molten sorbitol and ethanol in the kneading apparatus are kneaded while maintaining a temperature of 50 to 78°C. By maintaining the temperature in the kneading apparatus at 50 to 78°C, the molten sorbitol in the kneading apparatus does not solidify rapidly, and the molten sorbitol and ethanol can be kneaded while suppressing the volatilization of ethanol. The temperature in the kneading apparatus is preferably 55 to 78°C, and more preferably 60 to 75°C.
[0025] In step c), the kneaded mixture obtained in step b) is dried under reduced pressure at 25-90°C and 100-30000 Pa to remove ethanol and obtain porous sorbitol. Vacuum drying is performed using a vacuum dryer such as an evaporator. The porous sorbitol obtained in step c) can be crushed or granulated using a blender or the like to obtain a powder.
[0026] The kneading equipment used in the production of the porous sorbitol described above includes vertical kneaders, horizontal batch kneaders, and KRC kneaders.
[0027] In the porous sorbitol manufacturing process b) described above, the horizontal batch kneader is preferable from the viewpoint of manufacturing efficiency and quality because it can crystallize the molten mixture in a short time when molten sorbitol and ethanol are kneaded, and the porous sorbitol obtained through process c) exhibits a high specific surface area and pore volume.
[0028] The KRC kneader is preferable in terms of productivity and economics because, in the porous sorbitol manufacturing process b) described above, it can crystallize the molten mixture in a very short time when molten sorbitol and ethanol are kneaded together.
[0029] The specific surface area of the powdered substrate that can be used in the present invention is 5.0 m². 2 The amount is 6.0 to 50.0 m / g or more, preferably 6.0 to 50.0 m 2 / g, more preferably 7.0 to 30.0 m 2 It is / g.
[0030] In this invention, the specific surface area refers to the value measured by the BET single-point method using, for example, a MONOSORB (manufactured by Yuasa Ionics Co., Ltd.) or an equivalent specific surface area measuring device. For example, the specific surface area can be measured under the following measurement conditions. [Measurement conditions] Method: BET style one point method Carrier gas: Nitrogen-helium mixed gas (N2:He=30:70) Measured gas flow rate: 15cc / min Degassing conditions: 120°C, 20 minutes
[0031] The pore volume of the powdered substrate that can be used in the present invention is 0.45 mL / g or more, preferably 0.50 to 3.00 mL / g, and more preferably 0.55 to 2.50 mL / g.
[0032] In this invention, pore volume refers to the value measured by the mercury intrusion method using, for example, a Pascal 240 (manufactured by Thermo Fisher Scientific) or an equivalent pore volume measuring device.
[0033] By mixing a powdered substrate with an oily component, the oily component can be supported on the powdered substrate. For example, the oily component can be supported on the powdered substrate by adding the oily component to the powdered substrate in small amounts while mixing, in a weight ratio that achieves a desired impregnation rate.
[0034] The powder composition of the present invention has an impregnation rate of oily components to the powdered base material of 1 to 50% by weight, preferably 5 to 48% by weight, more preferably 10 to 45% by weight, and even more preferably 15 to 40% by weight. If the impregnation rate is less than 1% by weight, the amount of sorbitol, which is the powdered base material in the powder composition, becomes relatively large, which tends to change the taste and physical properties of the additive. If it exceeds 50% by weight, the oily components tend to be exposed on the surface of the powder composition, which tends to worsen the fluidity. In the present invention, the impregnation rate refers to the ratio of the weight of the oily components to the total weight of the oily components and the powdered base material.
[0035] The angle of repose of the powder composition of the present invention is preferably 30 to 60°, more preferably 35 to 58°, and even more preferably 40 to 55°. When the angle of repose is less than 30°, the powder tends to scatter easily, and when the angle of repose exceeds 60°, the powder tends to have poor fluidity.
[0036] In this invention, the angle of repose refers to the value measured by the cylindrical rotation method using, for example, a cylindrical rotation method angle of repose measuring instrument (Tsutsui Rikagakukikai Co., Ltd.) or an equivalent measuring instrument.
[0037] When the powder composition of the present invention is dispersed in water, the mode diameter of the oil droplets of the oily component is preferably 0.1 to 5 μm, more preferably 0.2 to 4.8 μm, and even more preferably 0.3 to 4.5 μm. If the mode diameter is less than 0.1 μm, the stability of the oil droplets decreases, and the oil droplets tend to aggregate prematurely. If it exceeds 5 μm, the dispersion tends to be insufficient.
[0038] In this invention, the mode diameter is a value measured by dynamic light scattering using, for example, a dynamic light scattering particle size distribution analyzer (LB-500, manufactured by Horiba, Ltd.) or an equivalent device. Furthermore, unless otherwise specified, the mode diameter in this invention refers to the particle diameter corresponding to the mode of the particle size distribution measured by dynamic light scattering.
[0039] The powder composition of the present invention preferably has a dispersion turbidity in water of 0.1 to 1, more preferably 0.2 to 0.8, and even more preferably 0.25 to 0.7. If the dispersion turbidity in water is less than 0.1, the oily components tend not to be uniformly dispersed in water, and if it exceeds 1, the powder composition tends to aggregate.
[0040] In this invention, dispersed turbidity refers to the absorbance at a wavelength of 660 nm at a cell length of 1 cm, measured by a spectrophotometer using a dispersion prepared by adding the powder composition of the present invention to water so that the oily component is 0.025% by weight, stirring for 5 minutes.
[0041] The powder composition of the present invention can be used in various fields such as food and beverages, cosmetics, fragrances, pharmaceuticals, quasi-drugs, and daily necessities, depending on the purpose of the oily component.
[0042] One preferred embodiment of the present invention is a whitening agent in which the powder composition containing edible oils and fats is added to food and beverages to improve their whiteness.
[0043] Another preferred embodiment of the powder composition of the present invention is an emulsifying stabilizer in which the powder composition containing an emulsifier is added to a liquid to improve the emulsifying stability of foods, beverages, cosmetics, daily necessities, etc.
[0044] Another preferred embodiment of the powder composition of the present invention is to use a powder composition containing a fragrance as a powder fragrance preparation. [Examples]
[0045] The present invention will be described in detail below with reference to examples, but the present invention is not limited in any way to these examples.
[0046] Test Example 1 (Preparation of Powdered Substrate) The materials listed below were melt-kneaded in the proportions (by weight) and under the conditions shown in Table 1. The resulting crystallized mixture was then vacuum-dried using a rotary evaporator under the conditions shown in Table 1 to obtain powdered substrates 1 and 6-9. The obtained powdered substrates were pulverized in the blender shown below at 15,700 rpm for 30 seconds. The specific surface area and pore volume of the pulverized powdered substrates 1 and 6-9 were measured under the following conditions. Note that powdered substrates 2-5 did not crystallize during melt-kneading, and therefore their evaluation was terminated without measuring their specific surface area and pore volume.
[0047] <Material> • Sorbitol 1: Powdered sorbitol "Ueno" 20M (manufactured by Ueno Food Techno Co., Ltd., sorbitol purity 92%) • Sorbitol 2: Pertec® SI 150 (Merck, sorbitol purity 98.4%) • Maltitol: Powdered maltitol "Ueno" 60M (manufactured by Ueno Food Techno Co., Ltd.) • Xylitol: Primary xylitol (reagent, manufactured by Fujifilm Wako Pure Chemical Industries, Ltd.) • Maltose: Sanmalt (registered trademark) Midori (manufactured by Hayashibara Co., Ltd.) • Dextrin: Max 1000EX-C (Matsutani Chemical Industry Co., Ltd.) • Ethanol: Fermented ethanol (95% alcohol, manufactured by Daiichi Alcohol Co., Ltd., 92.3% ethanol by weight) Ion-exchanged water <Mixing device> • Horizontal type: Horizontal kneader (semi-KC-6 type, manufactured by Satake Corporation) • KRC: KRC Kneader (S2 model, manufactured by Kurimoto Iron Works Co., Ltd.) <Blender> • Blender (16-speed blender, made by Oster)
[0048] Measurement of specific surface area The powdered substrate is measured in a cell (volume: 1.7 cm³). 3 The sample was placed in a container to approximately half its capacity, and the specific surface area was measured using a BET-type specific surface area meter (MONOSORB, manufactured by Yuasa Ionics Corporation) under the following conditions. [Measurement conditions] Method: BET style one point method Carrier gas: Nitrogen-helium mixed gas (N2:He=30:70) Measured gas flow rate: 15cc / min Degassing conditions: 120°C, 20 minutes
[0049] Measurement of pore volume Pore volume was measured using a mercury porosimeter (Pascal 240, Thermo Fisher Scientific).
[0050] [Table 1]
[0051] Examples 1-6 and Comparative Examples 1-24 60g of the powdered base material produced in the above test example was placed in a resin bag, and 20g of the oily component listed below was added little by little while shaking to prepare a powder composition with an impregnation rate of 25% by weight (Examples 1-3 and Comparative Examples 1-12). Similarly, a powder composition with an impregnation rate of 40% by weight was prepared in the same manner except that the oily component was changed to 40g (Examples 4-6 and Comparative Examples 13-24).
[0052] <Oily components> • Edible oils and fats (rapeseed oil): Canola oil (manufactured by Nisshin Oillio Group Ltd.) • Fragrance: Orange fragrance (manufactured by Ogawa Fragrance Co., Ltd.) • Emulsifier (hexaglycerin condensed ricinolate): Poem PR-300 (manufactured by Riken Vitamin Co., Ltd.)
[0053] Measurement of the angle of repose 150 mL of the powder composition was placed in a glass cylindrical container, and the angle of repose was measured using a cylindrical rotation angle of repose measuring instrument (Tsutsui Rikagakukikai Co., Ltd.). The results are shown in Tables 2 and 3.
[0054] Measurement of the mode diameter of an oil droplet 0.1 g of the powder composition was added to 100 g of deionized water while stirring at 1000 rpm, and the mixture was stirred for 5 minutes to prepare a dispersion. The mode diameter of the oil droplets in the dispersion was measured using a dynamic light scattering particle size distribution analyzer (LB-500, Horiba, Ltd.). The results are shown in Tables 2 and 3.
[0055] Measurement of dispersed turbidity A dispersion was prepared by adding deionized water to 0.1 g of a powder composition with an impregnation rate of 25% by weight (0.025 g as oily component) to make a total volume of 100 g, and stirring at 1000 rpm for 5 minutes. The absorbance of the dispersion at a wavelength of 660 nm at a cell length of 1 cm was measured using a spectrophotometer UH5300 (manufactured by Hitachi High-Tech Science Co., Ltd.). The absorbance was also measured in the same manner as above, except that 0.1 g of a powder composition with an impregnation rate of 40% by weight (0.040 g as oily component) was added to make a total volume of 160 g using deionized water. The results are shown in Tables 2 and 3.
[0056] The powder compositions of Examples 1 to 6 of the present invention were found to have superior fluidity, as they exhibited a lower angle of repose compared to the powder compositions of Comparative Examples 1 to 24. Furthermore, due to the small mode diameter of the oil droplets and high dispersion turbidity, it was confirmed that when the powder compositions were dispersed in water, the base material dissolved rapidly and the small-particle-sized oil droplets were uniformly dispersed.
[0057] [Table 2]
[0058] [Table 3]
Claims
1. A powder composition containing an oily component supported on a powdered substrate, The oily component is a substance whose solubility in water is 1 g / 100 mL or less and which is liquid at room temperature. The powdered substrate has a specific surface area of 5.0 m² as measured by the BET single-point method. 2 It contains sorbitol in an amount of 0.45 mL / g or more, and a pore volume of 0.45 mL / g or more as determined by mercury intrusion method. A powder composition in which the impregnation rate of the oily component into the powdered substrate is 1 to 50% by weight.
2. The powder composition according to claim 1, wherein the angle of repose is 30 to 60°.
3. The powder composition according to claim 1 or 2, wherein the oily component is one or more selected from the group consisting of edible oils and fats, fragrances, and emulsifiers.
4. The powder composition according to claim 3, wherein the oily component is rapeseed oil.
5. The powder composition according to claim 3, wherein the oily component is orange flavoring.
6. The powder composition according to claim 3, wherein the oily component is an emulsifier with an HLB value of 8 or less.
7. The powder composition according to claim 6, wherein the emulsifier is a polyglycerin fatty acid ester.
8. The powder composition according to any one of claims 1 to 7, wherein the mode diameter of oil droplets of the oily component when the powder composition is dispersed in water is 0.1 to 5 μm.
9. The powder composition according to any one of claims 1 to 8, wherein the dispersion turbidity when the powder composition is dispersed in water such that the oily component is 0.025% by weight relative to water is 0.1 to 1.