Method for producing granules, and granule
The method of mixing crystalline sugars or sugar alcohols with functional materials and spray drying under low-temperature conditions addresses the challenges of maintaining stability and preventing lump formation in granules from high-water-content materials, resulting in granules with excellent dispersibility and usability.
Patent Information
- Application Number
- PCT/JP2024/038765
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2023-11-15
- Filing Date
- 2024-10-30
- Publication Date
- 2025-05-22
AI Technical Summary
Existing methods for producing granules from functional materials with high water content, such as liquid egg and fruit juice, face challenges in maintaining the quality and stability of these materials during storage and in preventing lump formation when dissolved in solvents at room temperature to low temperature.
A method involving the direct mixing of crystalline sugars or sugar alcohols with functional materials to create a spray liquid containing a portion of the raw material in a crystalline state, followed by spray drying under low-temperature conditions, which allows for the production of granules with excellent dispersibility in solvents at room temperature to low temperature.
The method effectively produces granules that maintain the quality and stability of functional materials, prevent lump formation, and exhibit excellent dispersibility in solvents, thereby enhancing usability and storage stability.
Smart Images

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Abstract
Description
Granule manufacturing method and granules
[0001] The present invention relates to a method for producing granules and to the granules.
[0002] When functional materials that are susceptible to deterioration due to factors such as light, heat, moisture, oxygen, and changes over time are provided as raw materials for foods and pharmaceuticals, it is extremely important to maintain the quality of the functional materials over a long period of time, taking into consideration the factors that cause deterioration (light, temperature, humidity, oxygen, changes over time, etc.) during storage before use as raw materials. Methods for improving the stability of such functional materials include drying and powdering, and one method of drying and powdering is spray drying (also known as spray drying, SD).
[0003] Spray drying is a method in which a solution or suspension containing a functional material is sprayed into a dry gas and rapidly dried to obtain a dry powder or granules. Generally, high-temperature air heated to approximately 100-200°C is used as the drying gas. However, there are cases in which it is desirable to avoid the use of high-temperature gas, such as when the functional material is heat-sensitive. As such a technique, a method of spray-drying a functional material at low temperature together with a crystalline suspension containing crystalline sugars and / or sugar alcohols in part in a crystalline state, and inventions relating to granules produced by this method have been disclosed (Patent Documents 1 and 2).
[0004] JP 2021-106571 A Patent No. 7197743 A
[0005] The methods disclosed in Patent Documents 1 and 2 first prepare a crystal suspension containing a portion of the crystalline sugar and / or sugar alcohol in a crystalline state, and then mix this crystal suspension with a functional material to prepare a spray liquid. In this process, it is necessary to maintain a state in which a portion of the crystalline sugar and / or sugar alcohol is contained in a crystalline state in the spray liquid so that a dry powder (granules) can be produced by spray drying at low temperatures.
[0006] For these reasons, in the methods disclosed in Patent Documents 1 and 2, when using functional materials with a high water content (for example, liquid eggs which are about 75% water, creamers (coffee creamers, etc.) which are about 50-70% water, liquid dairy ingredients such as whole milk which are about 88% water, and fruit juices and vegetable juices which are 90% water or more), in order to obtain granules which contain sufficient components other than water (solids, etc.), it is necessary to increase the blending ratio of the functional material, which inevitably increases the water ratio, and therefore it may be difficult to obtain a spray liquid which contains some of the crystalline sugar and / or sugar alcohol in a crystalline state.
[0007] On the other hand, it is known that compositions prepared into powder or granule form using a general spray drying method from functional materials with high moisture content, such as powdered eggs, powdered milk, powdered pressed fruit juice, powdered pressed vegetable juice, and powdered coffee creamer, tend to form lumps when the composition is dissolved in a solvent at room temperature to low temperature.There has been a growing need for a technology that makes it difficult for such functional materials with high moisture content to form lumps when spray-dried and then dissolved in a solution at room temperature to low temperature.
[0008] In view of the above-mentioned problems of the conventional art, an object of the present invention is to provide a method for producing granules of a functional material having a high water content, which can be obtained by spray drying under low-temperature conditions and has excellent dispersibility in solvents at room temperature to low temperature. Another object of the present invention is to provide granules obtained by the method.
[0009] The present invention relates to a method for producing granules, which comprises the steps of: mixing at least one raw material selected from the group consisting of crystalline sugars and crystalline sugar alcohols with a functional material to obtain a spray liquid containing the raw material and the functional material, with a portion of the raw material being in a crystalline state; and spray-drying the spray liquid under low-temperature conditions, wherein the functional material is a functional material with a high water content.
[0010] The present invention also relates to a method for producing granules, which comprises the steps of: mixing at least one raw material selected from the group consisting of crystalline sugars and crystalline sugar alcohols with a functional material, without using a solvent, to obtain a spray liquid containing the raw material and the functional material, with a portion of the raw material being in a crystalline state; and spray-drying the spray liquid under low-temperature conditions.
[0011] The method for producing granules according to the present invention includes directly mixing at least one raw material selected from the group consisting of crystalline sugars and crystalline sugar alcohols with a functional material without previously preparing a crystalline suspension of at least one raw material selected from the group consisting of crystalline sugars and crystalline sugar alcohols to obtain a spray liquid containing the raw material and the functional material, with a portion of the raw material being in a crystalline state, and then spray-drying the spray liquid at low temperatures. This allows granules to be produced by spray-drying at low temperatures even from functional materials with high moisture contents, and the resulting granules have excellent dispersibility in solvents at room temperature to low temperatures.
[0012] In the production method, the crystallization rate of the raw material in the spray liquid may be 5% by mass or more and 50% by mass or less, whereby the above-mentioned effects of the present invention are more significantly exhibited.
[0013] In the production method, the spray drying may be carried out under conditions where the inlet temperature is 0 to 60°C, for example.
[0014] The present invention further relates to granules containing at least one selected from the group consisting of crystalline sugars and crystalline sugar alcohols, and a solid portion of a functional material having a high moisture content, wherein a portion of the sugar and / or sugar alcohol is in a crystalline state and another portion is in an amorphous state.
[0015] The granules may be such that the amorphous sugar and / or sugar alcohol and the solid content are held in gaps formed between the crystalline sugar and / or sugar alcohol.
[0016] The sugar and sugar alcohol may be, for example, a monosaccharide, a disaccharide, a trisaccharide, or a sugar alcohol thereof. The sugar and sugar alcohol may be, for example, at least one selected from the group consisting of palatinose, sucrose, and trehalose.
[0017] The functional ingredient may be, for example, liquid egg, creamer, fruit juice, vegetable juice, or liquid dairy ingredients.
[0018] The present invention includes, for example, the following inventions. [1] A method for producing granules, comprising the steps of: mixing at least one raw material selected from the group consisting of crystalline sugars and crystalline sugar alcohols with a functional material to obtain a spray liquid containing the raw material and the functional material, with a portion of the raw material being in a crystalline state; and spray-drying the spray liquid at low temperatures, wherein the functional material has a high moisture content. [2] A method for producing granules, comprising the steps of mixing at least one raw material selected from the group consisting of crystalline sugars and crystalline sugar alcohols with a functional material to obtain, without using a solvent, a spray liquid containing the raw material and the functional material, with a portion of the raw material being in a crystalline state; and spray-drying the spray liquid at low temperatures. [3] The production method according to [1] or [2], wherein the crystallization rate of the raw material in the spray liquid is 5% by mass or more and 50% by mass or less. [4] The production method according to any of [1] to [3], wherein the sugar and sugar alcohol are monosaccharides, disaccharides, trisaccharides, and their sugar alcohols. [5] The method according to any one of [1] to [4], wherein the sugar and the sugar alcohol are at least one selected from the group consisting of palatinose, sucrose, and trehalose. [6] The manufacturing method according to any one of [1] to [5], wherein the spray drying is carried out under conditions where the inlet temperature is 0 to 60°C. [7] The manufacturing method according to any one of [1] to [6], wherein the functional material is liquid egg, creamer, fruit juice, vegetable juice, or liquid dairy material. [8] Granules containing at least one selected from the group consisting of crystalline sugars and crystalline sugar alcohols and the solid content of a functional material having a high moisture content, wherein a portion of the sugar and / or the sugar alcohol is crystalline and another portion is amorphous. [9] The granules according to [8], wherein the amorphous sugar and / or sugar alcohol and the solid content are retained in the gaps formed between the crystalline sugars and / or sugar alcohols.
[10] The granule according to [8] or [9], wherein the sugar and the sugar alcohol are monosaccharides, disaccharides, trisaccharides and their sugar alcohols.
[11] The granule according to any one of [8] to
[10] , wherein the sugar and the sugar alcohol are at least one selected from the group consisting of palatinose, sucrose and trehalose.
[12] The granules according to any one of [8] to
[11] , wherein the functional ingredient having a high water content is liquid egg, creamer, fruit juice, vegetable juice, or liquid dairy material.
[0019] The present invention provides a method for producing granules of a functional material having a high water content, which can be obtained by spray drying under low-temperature conditions and has excellent dispersibility in solutions at room temperature to low temperature.The present invention also provides granules obtained by the method.
[0020] The present inventors have discovered that by adding at least one raw material selected from the group consisting of crystalline sugars and sugar alcohols to a functional material with a high water content and using the inherent water content of the functional material to prepare a spray liquid (crystal suspension) without adding additional water, spray drying can be performed under low temperature conditions, and the granules obtained by spray drying have excellent dispersibility in solvents at room temperature to low temperature. The present invention is based on this discovery.
[0021] The granules according to the present invention contain sugars and / or sugar alcohols in a crystalline state, which forms irregularities on the surface of the granule particles, reducing the contact area between the granule particles and resulting in excellent fluidity. Therefore, the granules according to the present invention are easy to handle. Because the granules according to the present invention contain sugars and / or sugar alcohols in a crystalline state, the granule particles are less likely to deteriorate or break due to physical or mechanical stimuli, and the stability of the particle structure and storage stability are also excellent.
[0022] Furthermore, when the granules according to the present invention are reconstituted in a solution containing a functional material using a solvent (e.g., water) at room temperature to low temperature, the formation of lumps (dust) is suppressed and the granules are rapidly dispersed in the solution. Therefore, when the granules are used as a food ingredient as a functional material, the usability of the food processor and the consumer is not impaired.
[0023] When the granules of the present invention are incorporated into powder mix products and the like that are consumed in solutions at room temperature to low temperature (e.g., solutions such as water, milk, carbonated water, etc.), they can be prepared from the beginning at a temperature range of room temperature to low temperature that is suitable for consumption, and therefore do not require operations such as mixing with ice, maintaining at room temperature or under refrigeration, or temporarily heating to a high temperature for dissolution followed by cooling.
[0024] Furthermore, because the granules of the present invention are obtained by spray drying at low temperatures, the functionality of the functional material contained therein is less likely to be lost due to heat. In other words, the granules of the present invention maintain the functionality of the functional material well. Normally, when granules are obtained by spray drying, it is difficult to obtain suitable granules unless the spray drying is performed at higher temperatures. However, because the granules of the present invention use a mixed suspension containing crystalline sugar and / or sugar alcohol as the spray liquid for spray drying, suitable granules can be easily obtained even at low temperatures. For example, while conventional methods for spray drying fruit and vegetable juices can cause discoloration and deterioration in taste and aroma, the method of the present invention allows for powdering (granulation) of the functional material while retaining its color, taste, and aroma.
[0025] Furthermore, the method for producing granules according to the present invention can omit the step of drying by vacuum freezing or the step of heating the spray liquid before spray drying. Furthermore, there is no need to separately prepare a crystalline suspension of at least one raw material selected from the group consisting of sugars and sugar alcohols, and the steps of completely dissolving the raw material and crystallizing the raw material can be omitted, making it possible to produce granules by a simpler method than conventional methods.
[0026] The method for producing granules according to the present invention allows spray drying of functional materials with high water content at low temperatures, and therefore enables dry granules to be produced without deteriorating the quality of less stable ingredients contained in liquid eggs, liquid dairy ingredients, fruit and vegetable juices, fruit and vegetable extracts, creamers, etc. Therefore, the quality of the functional materials can be maintained over a long period of time, taking into consideration factors that may cause deterioration during storage of the functional materials (light, temperature, humidity, oxygen, changes over time, etc.).
[0027] 1 is an optical microscope image of the spray liquid prepared in Test Example 1. 2 is an electron microscope image of the dry powder (granules) produced in Test Example 1. 3 is an optical microscope image of the spray liquid prepared in Test Example 2. 4 is an electron microscope image of the dry powder (granules) produced in Test Example 2.
[0028] Hereinafter, embodiments of the present invention will be described in detail, but the present invention is not limited to the following embodiments.
[0029] [Method for producing granules] One aspect of the present invention relates to a method for producing granules, comprising a step (mixing step A) of mixing at least one raw material selected from the group consisting of crystalline sugars and crystalline sugar alcohols with a functional material to obtain a spray liquid containing the raw material and the functional material, with a portion of the raw material being in a crystalline state, and a step (spray drying step) of spray-drying the spray liquid under low-temperature conditions, wherein the functional material is a functional material with a high water content.
[0030] Another aspect of the present invention relates to a method for producing granules, comprising a step (mixing step B) of mixing at least one raw material selected from the group consisting of crystalline sugars and crystalline sugar alcohols with a functional material, without using a solvent, to obtain a spray liquid containing the raw material and the functional material, with a portion of the raw material being in a crystalline state, and a step (spray drying step) of spray-drying the spray liquid under low-temperature conditions.
[0031] <Mixing step> In the mixing step, a spray liquid is obtained. The spray liquid contains at least one raw material selected from the group consisting of crystalline sugars and crystalline sugar alcohols (hereinafter also simply referred to as "raw material") and a functional material, with a portion of the raw material being contained in a crystalline state.
[0032] The spray liquid may contain other ingredients in addition to the raw materials and functional materials, provided that the effects of the present invention are not impaired. Examples of other ingredients include ingredients acceptable for use in foods or pharmaceuticals, such as preservatives, high-intensity sweeteners, flavorings, thickeners, lubricants (e.g., calcium stearate), protective ingredients for proteins and live bacteria (e.g., proteins such as casein, antioxidants such as vitamin C, phosphate buffer), ethanol, anti-caking agents (e.g., fine silicon dioxide), emulsifiers (e.g., lecithin, modified starch, gum arabic), excipients other than sugars and sugar alcohols (e.g., dextrin, cellulose), etc.
[0033] One aspect of the mixing step may be a step (mixing step A) of mixing at least one raw material selected from the group consisting of crystalline sugars and crystalline sugar alcohols with a functional material having a high water content to obtain a spray liquid containing a portion of the raw material in a crystalline state. In mixing step A, other components may be mixed in addition to the raw material and functional material, as needed. A solvent may also be mixed as long as the above-described spray liquid is obtained. Mixing may be performed, for example, by stirring. Mixing step A can be performed, for example, by stirring for 10 minutes to 3 hours while maintaining a temperature of 25 to 35°C. The rotation speed during stirring may be, for example, 250 to 400 rpm.
[0034] Another aspect of the mixing step may be a step (mixing step B) of mixing at least one raw material selected from the group consisting of crystalline sugars and crystalline sugar alcohols with a functional material to obtain a spray liquid containing a portion of the raw material in a crystalline state without using a solvent. In mixing step B, other components may be mixed in addition to the raw material and functional material, as necessary. Mixing step B can be performed, for example, by mixing the raw material, functional material, etc. Mixing can be performed, for example, by stirring. Mixing step B can be performed, for example, by stirring for 10 minutes to 3 hours while maintaining a temperature of 25 to 35°C. The rotation speed during stirring can be, for example, 250 to 400 rpm. The functional material used in mixing step B may or may not have a high water content; however, since no solvent is used, a high water content functional material is preferred.
[0035] In the mixing steps (mixing steps A and B), a spray solution containing some of the raw materials in a crystalline state may be obtained without dissolving all of the raw materials, or a spray solution containing some of the raw materials in a crystalline state may be obtained by dissolving all of the raw materials and then precipitating crystals of the raw materials and / or recrystallizing the raw materials. The fact that some of the raw materials are contained in a crystalline state can be confirmed, for example, by visual inspection. Another method for confirming that some of the raw materials are contained in a crystalline state includes, for example, observing crystallization induction with a microscope. When the spray solution dropped onto a glass slide is observed with a microscope at room temperature of 25°C for 5 minutes, it can be determined that some of the raw materials are contained in a crystalline state if the presence of crystals is confirmed.
[0036] Precipitation of crystals of the raw materials after dissolution of all the raw materials and / or recrystallization of the raw materials can be carried out by known methods, such as a method of cooling a solution of the raw materials (cooling crystallization), a method of adding a non-solvent such as ethanol to a mixed solution (non-solvent crystallization), and a reactive crystallization method.
[0037] As used herein, "crystalline sugars and / or sugar alcohols" refers to solid sugars and / or sugar alcohols whose constituent atoms are three-dimensionally ordered and repeating. As used herein, "amorphous sugars and / or sugar alcohols" refers to solid or liquid sugars and / or sugar alcohols that do not have such ordered and repeating atoms.
[0038] From the viewpoint of improving operability in the mixing step, the crystalline sugar and crystalline sugar alcohol are preferably monosaccharides, disaccharides, trisaccharides, and sugar alcohols thereof.
[0039] Examples of monosaccharides include glucose, galactose, mannose, fructose, allose, and allulose. Examples of disaccharides include isomaltulose, sucrose, lactulose, lactose, maltose, trehalose, and cellobiose. Examples of trisaccharides include nigerotriose, maltotriose, and raffinose. Isomaltulose is a disaccharide registered as a trademark by DM Mitsui Sugar Co., Ltd. under the name "palatinose."
[0040] Examples of sugar alcohols include sorbitol, erythritol, xylitol, maltitol, lactitol, mannitol, α-glucopyranosyl-1,1-mannitol (1,1-GPM), α-glucopyranosyl-1,6-sorbitol (1,6-GPS), reduced palatinose, etc. Reduced palatinose is a mixture of 1,1-GPM and 1,6-GPS, which is registered as a trademark by DM Mitsui Sugar Co., Ltd. as "reduced palatinose."
[0041] The above-mentioned crystalline sugars and sugar alcohols may be used alone or in combination of two or more. The spray liquid may contain two or more crystalline sugars, may contain two or more crystalline sugar alcohols, or may contain a combination of two or more crystalline sugars and crystalline sugar alcohols.
[0042] The content of crystalline sugar and / or sugar alcohol contained in the spray liquid can be appropriately set depending on the type of functional material used, etc. For example, the content of crystalline sugar and / or sugar alcohol contained in the spray liquid can be set so that the crystallization rate in the spray liquid is within the range described below. Furthermore, for example, but not limited to, the content of crystalline sugar and / or sugar alcohol contained in the spray liquid is, for example, 30% by mass or more, 35% by mass or more, 40% by mass or more, 45% by mass or more, or 50% by mass or more, based on the total amount of the spray liquid, and the upper limit is, for example, 70% by mass or less, 65% by mass or less, 60% by mass or less, 55% by mass or less, or 50% by mass or less.
[0043] The functional material is not limited to a material or component that exhibits some function in a composition (e.g., food, pharmaceutical, etc.) obtained by combining with other materials. The functional material may be a material that is affected by the surrounding environment, such as moisture, heat, light, acid, oxygen, molecular motion, ultraviolet light, electrical interaction, or physical stimuli, or a material that loses its function when heated.
[0044] The granule manufacturing method according to this embodiment can obtain granules by spray drying under low-temperature conditions even when the functional material contains a large amount of water, and the granules have the advantage of being highly dispersible in solvents at room temperature to low temperature, so that functional materials with a high water content can be used.
[0045] As used herein, a "functional material with a high moisture content" refers to a functional material having a moisture content of 20% or more by mass, based on the total amount of the functional material. The moisture content may be, for example, 25% or more, 30% or more, 35% or more, 40% or more, 45% or more, 50% or more, 55% or more, 60% or more, 65% or more, 70% or more, 75% or more, 80% or more, 85% or more, or 90% or more by mass, based on the total amount of the functional material. The moisture content can be measured by an appropriate known method, such as a heat drying method, a Karl Fischer method, or a distillation method, depending on the type of functional material.
[0046] Examples of functional ingredients with a high water content include, but are not limited to, liquid dairy ingredients such as liquid egg, creamer, whole milk, whey, and cream, fruit juice, vegetable juice, and fruit and vegetable extracts.
[0047] The technique of powdering liquid egg by spray drying has been known for a long time, and a technique of adding additives such as sugars and casein during spray drying to prevent deterioration and improve quality has also been known. However, powdered egg obtained by spray drying liquid egg (whole egg liquid, egg white liquid, egg yolk liquid, etc.) using conventional methods tends to form lumps (powder) when dissolved in a solvent (e.g., water) at room temperature to low temperature, making the dissolution difficult and affecting the texture, etc. The method for producing granules according to this embodiment can solve these problems of the conventional techniques.
[0048] Creaming powders prepared by drying creamers prepared by emulsifying oil in water, such as non-dairy coffee creamers in which vegetable oils are emulsified with casein or dairy coffee creamers in which milk fat is emulsified with casein or the like, or powders prepared by spray-drying liquid dairy ingredients such as whole milk, whey, and cream using conventional methods, have problems with solubility in solvents (e.g., water) at room temperature to low temperatures. To improve solubility in cold water, a method has been known in which the surface of the powder is coated with a composition of fats, oils, fatty acids, etc. However, this method has problems such as a complicated manufacturing process and the need to use additives such as fats, oils, and fatty acids. The method for producing granules according to this embodiment can solve these problems of the prior art.
[0049] Powders made by spray drying fruit juices, vegetable juices, and fruit and vegetable extracts using conventional methods have the problem of deterioration in color, taste, and aroma. The method for producing granules according to the present embodiment can solve these problems of the conventional techniques.
[0050] The content of the functional material contained in the spray liquid can be appropriately set depending on the type of functional material used, etc. For example, the content of the functional material contained in the spray liquid can be set so that the crystallization rate in the spray liquid is within the range described below. Furthermore, for example, but not limited to, the content of the functional material contained in the spray liquid is, for example, 30% by mass or more, 35% by mass or more, 40% by mass or more, 45% by mass or more, or 50% by mass or more based on the total amount of the spray liquid, and the upper limit is, for example, 70% by mass or less, 65% by mass or less, 60% by mass or less, 55% by mass or less, or 50% by mass or less.
[0051] The crystallization rate in the spray liquid may be 5% by mass or more, 10% by mass or more, 15% by mass or more, 20% by mass or more, 25% by mass or more, 30% by mass or more, 35% by mass or more, or 40% by mass or more, since this can more significantly exhibit the effects of the present invention. The upper limit of the crystallization rate in the spray liquid may be, for example, 55% by mass or less, 50% by mass or less, 45% by mass or less, or 40% by mass or less. The "crystallization rate" in this specification is a value measured by the method described in the Examples below. Specifically, 1 g of the spray liquid is placed in a 1.5 mL Eppendorf tube, centrifuged at 16,000 rpm for 3 minutes using a centrifuge (e.g., Sakuma Seisakusho M150IV), and the remaining crystal mass after removing the supernatant and the mass of the spray liquid are applied to the following formula to calculate the crystallization rate. Crystallization rate (mass%) = remaining crystal mass (g) / mass of spray liquid (g) × 100
[0052] The crystallization rate in the spray solution can be adjusted by adjusting the ratio of at least one raw material selected from the group consisting of crystalline sugars and crystalline sugar alcohols to the functional material. The crystallization rate in the spray solution can also be adjusted by physically or chemically adding or removing crystals, such as by filtration, centrifugation, gravity settling, dissolution by adding water and / or heating, or adjusting the consumption of crystal components associated with chemical reactions. Furthermore, the crystallization rate can also be adjusted by adding and mixing crystal components, or other operations that increase the crystals.
[0053] The spray liquid contains a portion of the raw material in a crystalline state. The spray liquid may contain crystal nuclei, and the size of the crystal nuclei is not particularly limited as long as they are large enough to exist stably in the spray liquid. The size of the crystal nuclei may be, for example, larger than the critical crystal nucleus.
[0054] The average particle size of the crystalline sugar and / or sugar alcohol in the spray liquid may be, for example, 1.00 μm or more, 2.00 μm or more, 3.00 μm or more, 4.00 μm or more, 5.00 μm or more, 6.00 μm or more, 7.00 μm or more, 8.00 μm or more, 9.00 μm or more, 10.00 μm or more, 11.00 μm or more, or 12.00 μm or more. The average particle size of the crystalline sugar and / or sugar alcohol in the spray liquid may be 30.00 μm or less, 25.00 μm or less, 20.00 μm or less, 18.00 μm or less, 15.90 μm or less, 14.00 μm or less, 13.00 μm or less, 12.00 μm or less, or 11.00 μm or less. The average particle size of the crystalline sugar and / or sugar alcohol in the spray liquid may be, for example, 1.00 to 15.90 μm.
[0055] The average particle size of the crystalline sugar and / or sugar alcohol in the spray liquid can be adjusted by adding or removing solvent or solute, changing the solvent temperature, dissolution time, or stirring time, crushing with a stirrer or grinder, fractionation by filtration, or crystallization by sugar hydrolysis, etc.
[0056] The "average particle size of crystalline sugars and / or sugar alcohols" herein can be measured using a digital microscope. For example, an SKM-S31B-PC manufactured by Saito Optical Co., Ltd. can be used for the measurement. Specifically, for example, the measurement can be performed by the following method. The sprayed liquid is dropped onto a glass slide, a cover glass is placed on top, and measurements are taken at 1000x magnification. The average particle size is measured by using a digital microscope (e.g., SKM-S31B-PC manufactured by Saito Optical Co., Ltd.) to calculate the average particle size of 10 or more crystals selected from any 10 or more crystals. For 10 or more particles to be measured in the sprayed liquid, the distance in the first direction and the distance in the second direction perpendicular to the first direction intersect at their midpoints, and these distances are defined as the width and length, respectively. The first direction is the same for all particles to be measured. The longer of the measured widths and length are defined as the major axis, and the shorter of the measured widths and length are defined as the minor axis, and the averages of the particles to be measured are defined as the average major axis and average minor axis.
[0057] The standard deviation of the average particle size of the crystalline sugar and / or sugar alcohol in the spray liquid may be, for example, 10.00 μm or less, 9.00 μm or less, 8.00 μm or less, 7.00 μm or less, or 6.00 μm or less. A small standard deviation of the average particle size means that there is little variation in the average particle size. The standard deviation of the average particle size of the crystalline sugar and / or sugar alcohol in the spray liquid may be, for example, 1.0 μm or more, 3.0 μm or more, or 50 μm or more. The standard deviation of the average particle size of the crystalline sugar and / or sugar alcohol in the spray liquid may be, for example, 1.00 to 10.70 μm.
[0058] In this specification, the "standard deviation" refers to the unbiased standard deviation calculated using the STDEV.S function in Microsoft Excel (registered trademark).
[0059] The spray liquid may or may not contain a solvent. The solvent may be, for example, an organic solvent such as ethanol, methanol, acetone, isopropanol, or water (added water, not derived from the functional material). If the functional material has a high water content, the spray liquid can be obtained by utilizing the water originally contained in the functional material without adding a new solvent, so it does not necessarily need to contain a solvent.
[0060] The content of the solvent in the spray liquid may be, for example, 20% by mass or less, 15% by mass or less, 10% by mass or more, 5% by mass or less, 3% by mass or less, 1% by mass or less, or 0% by mass, based on the total mass of the spray liquid.
[0061] <Spray drying step> The spray drying step is a step of spray-drying the above-mentioned spray liquid under low-temperature conditions. Spray drying can be performed using, for example, a spray drying apparatus (spray dryer). As the spray drying apparatus, for example, OC-16 manufactured by Okawara Kakoki Co., Ltd. can be used.
[0062] The low-temperature conditions refer to temperatures (e.g., 60°C or lower) lower than the temperatures (e.g., higher than 60°C) used in conventional spray drying. In this embodiment, a spray liquid containing a portion of the sugar and / or sugar alcohol in a crystalline state is used, so suitable granules can be obtained even when spray drying is performed at temperatures lower than conventional conditions. The low-temperature conditions may be temperature conditions at which the functionality of the functional material is not lost.
[0063] Spray drying carried out under low temperature conditions means that the inlet temperature (inlet air temperature) of the spray drying apparatus is set to the temperature conditions described above.
[0064] In one embodiment, the inlet temperature in the spray drying step is, for example, 60°C or less, 55°C or less, 50°C or less, 45°C or less, 40°C or less, 35°C or less, 30°C or less, 25°C or less, 20°C or less, or 15°C or less. The inlet temperature may be, for example, 0°C or more, 5°C or more, or 10°C or more. That is, the inlet temperature in the spray drying step may be, for example, 0 to 60°C, or 0 to 50°C.
[0065] The outlet temperature (exhaust air temperature) in the spray drying apparatus may be, for example, 50°C or less, 40°C or less, 35°C or less, 30°C or less, 25°C or less, 20°C or less, or 15°C or less, or may be 0°C or more, 5°C or more, or 10°C or more.
[0066] The liquid temperature of the spray liquid in the spray drying step may be, for example, 60°C or lower, 50°C or lower, or 45°C or lower, or 10°C or higher, 15°C or higher, or 20°C or higher.
[0067] In the spray drying, other conditions such as the amount of the spray liquid supplied, the atmospheric temperature, and the atmospheric humidity may be adjusted as appropriate.
[0068] For example, the atomizer rotation speed in spray drying may be 3,000 rpm or more, 5,000 rpm or more, or 10,000 rpm or more, and may be 25,000 rpm or less, 20,000 rpm or less, or 18,000 rpm or less.
[0069] The spray drying process may include a post-drying process, for example, to adjust the moisture content of the granules. The post-drying process may involve, for example, blowing air onto the granules adhering to the can wall of the spray dryer for a predetermined period of time to further volatilize the moisture in the granules. Alternatively, the granules obtained by spray drying may be stored for a predetermined period of time in a desiccator containing silica gel.
[0070] Granules according to this embodiment contain at least one selected from the group consisting of crystalline sugars and crystalline sugar alcohols, and a solid content of a functional material having a high water content, wherein the crystalline sugar and / or sugar alcohol is partially crystalline and partially amorphous. The granules can be obtained, for example, by the above-described method for producing granules.
[0071] In this specification, the term "granules" refers to an aggregate of particles, and the particles that make up the granules (granule particles) contain one or more types selected from the group consisting of crystalline sugars and sugar alcohols.
[0072] In this specification, the "solid content of the functional material" refers to the solid content remaining after removing water from the functional material. The removal of water is carried out, for example, by spray drying as described above.
[0073] The granules may contain two or more types of crystalline sugars, may contain two or more types of crystalline sugar alcohols, or may contain two or more types of crystalline sugars and crystalline sugar alcohols in combination.
[0074] In one embodiment, the granules are composed of granule particles in which a portion of the crystalline sugar and / or sugar alcohol is in a crystalline state and the crystalline sugar and / or sugar alcohol aggregates together. In this case, it is preferable that another portion (other portion) of the crystalline sugar and / or sugar alcohol is in a non-crystalline state and is held in the gaps formed by the aggregated crystalline sugar and / or sugar alcohol. It is also preferable that the functional material is held in the gaps formed by the crystalline sugar and / or sugar alcohol.
[0075] The aggregation of crystalline sugars and / or sugar alcohols can be confirmed by observing the appearance of the granule particles or the morphology of the fracture surface of the granule particles using a scanning electron microscope (SEM) or digital microscope. The retention of amorphous sugars and / or sugar alcohols and functional materials in the gaps can be confirmed by the following methods: (1) The morphology of the granules is observed during heating using a differential scanning calorimeter (DSC, for example, Real View DSC (TA7000) manufactured by Hitachi High-Tech Science Corporation). This allows visual confirmation of the glass transition of amorphous sugars and sugar alcohols due to heating. (2) The difference in polarization between the crystalline and amorphous states is visually confirmed using a polarizing microscope (for example, polarizing microscope (MT9200L) manufactured by Meiji Techno Co., Ltd.).
[0076] The number of crystalline sugars and / or sugar alcohols (number of crystals) contained in the particles constituting the granules is, for example, 10 or more, and may be 50 or more, or 100 or more. The number of crystals may be 1,000 or less. The number of crystals can be determined visually by observing with a scanning electron microscope.
[0077] The shape of the particles constituting the granules may be approximately ellipsoidal or approximately spherical. The particles constituting the granules may have irregularities on their surfaces.
[0078] The average particle size of the granules may be, for example, 10.00 μm or more, 20.00 μm or more, 40.00 μm or more, 60.00 μm or more, 80.00 μm or more, or 90.00 μm or more, and may be, for example, 200.00 μm or less, 150.00 μm or less, 140.00 μm or less, 135.00 μm or less, or 118 μm or less. The average particle size of the granules may be, for example, 20.00 to 118.00 μm.
[0079] The "average particle size of granules" in this specification can be measured using an electron microscope. For example, a Miniscope™ 3030 manufactured by Hitachi High-Technologies Corporation can be used for the measurement. Specifically, for example, the measurement can be performed by the following method. The crystal size of the particles constituting the granules is measured using an electron microscope. Ten or more granules are observed, and the long and short widths of each granule are measured to determine the average granule particle size.
[0080] The standard deviation of the average particle size of the granules may be, for example, 40 μm or less, or 30 μm or less, or 5 μm or more, or 10 μm or more.
[0081] The average minor axis of the granules may be, for example, 80 μm or more, or 95 μm or more, and 150 μm or less, or 130 μm or less. The average major axis of the granules may be, for example, 75 μm or more, or 95 μm or more, and 200 μm or less, or 150 μm or less.
[0082] The ratio of the average major axis to the average minor axis of the granules may be 1.40 or less, 1.20 or less, 1.10 or less, or 1.04 or less, and may be 1.00 or more, or 1.01 or more, since the stability and flowability of the granules are further improved. The standard deviation of the ratio of the average major axis to the average minor axis of the granules may be 0.20 or less, or 0.12 or less, and may be 0.01 or more, since the ease of drying, resistance to caking, and flowability of the granules are further improved.
[0083] The average particle size of the particles constituting the granules may be, for example, 5.00 μm or more, 10.00 μm or more, or 15.00 μm or more, and may be 50.00 μm or less, 40.00 μm or less, 30.00 μm or less, 25.00 μm or less, or 20.00 μm or less. The average particle size of the particles constituting the granules may be, for example, 10.00 to 20.00 μm.
[0084] The standard deviation of the average particle size of the particles constituting the granules may be, for example, 10.00 μm or less, 8.00 μm or less, 6.00 μm or less, 4.00 μm or less, or 3.3 μm or less, or may be 1.00 μm or more, or 2.00 μm or more. The standard deviation of the average particle size of the particles constituting the granules may be, for example, 1.00 to 3.30 μm.
[0085] The average minor axis of the particles constituting the granules may be, for example, 5.0 μm or more, or 10.0 μm or more, and 30.0 μm or less, or 25.0 μm or less. The average major axis of the particles constituting the granules may be, for example, 10.0 μm or more, or 15.0 μm or more, and 50 μm or less, or 35 μm or less.
[0086] The ratio of the average major axis to the average minor axis of the particles constituting the granules may be 3.1 or less, 2.8 or less, 2.5 or less, 2.2 or less, or 1.9 or less, or 0.5 or more, 1.0 or more, or 1.4 or more, since this further improves the stability and flowability of the granules. The standard deviation of the ratio of the average major axis to the average minor axis of the particles constituting the granules may be 0.4 or less, or 0.3 or less, or may be more than 0.0, or 0.1 or more.
[0087] The loose bulk density of the particles constituting the granules is, for example, 0.700 (g / cm 3 ) from the viewpoint that the formation of lumps (dust) is suppressed when the granules are returned to a solution containing a functional material using a solvent (for example, water) at room temperature to low temperature, and the effect of quickly dispersing the granules in the solution is more pronounced. 3 ) or less, 0.600 (g / cm 3 ) or less, 0.500 (g / cm 3 ), or 0.400 (g / cm 3 ) or less, and may be 0.100 (g / cm 3 ) or more, 0.200 (g / cm 3 ) or more, 0.300 (g / cm 3 ) or more, or 0.400 (g / cm 3 The loose bulk density of the particles constituting the granules may be, for example, 0.393 (g / cm 3 ) ~ 0.496 (g / cm 3 The loose bulk density of the particles constituting the granules can be measured by the method described in the examples below.
[0088] The packed bulk density of the particles constituting the granules is, for example, 1.000 (g / cm ) from the viewpoint that the formation of lumps (dust) is suppressed when the granules are returned to a solution containing a functional material using a solvent (for example, water) at room temperature to low temperature, and the effect of exhibiting the property of quickly dispersing in the solution is more pronounced. 3 ) or less, 0.900 (g / cm 3 ) or less, 0.800 (g / cm 3 ), or 0.700 (g / cm 3 ) or less, and 3 ) or more, 0.400 (g / cm 3 ) or more, 0.500 (g / cm 3 ) or more, or 0.600 (g / cm 3 The packed bulk density of the particles constituting the granules may be, for example, 0.6979 (g / cm 3 ) ~ 0.704 (g / cm 3 The packed bulk density of the particles constituting the granules can be measured by the method described in the examples below.
[0089] The dynamic bulk density of the particles constituting the granules is, for example, 0.700 (g / cm 3 ) from the viewpoint that the formation of lumps (dust) is suppressed when the granules are returned to a solution containing a functional material using a solvent (for example, water) at room temperature to low temperature, and the effect of exhibiting the property of quickly dispersing in the solution is more pronounced. 3 ) or less, 0.600 (g / cm 3 ) or less, or 0.500 (g / cm 3 ), and may be 0.200 (g / cm 3 ) or more, 0.300 (g / cm 3 ) or more, 0.400 (g / cm 3 ) or more, or 0.500 (g / cm 3 The dynamic bulk density of the particles constituting the granules may be, for example, 0.530 (g / cm 3 ) ~ 0.545 (g / cm 3 The dynamic bulk density of the particles constituting the granules can be measured by the method described in the examples below.
[0090] The granules according to this embodiment have the above-mentioned structure and therefore have excellent dispersibility in solvents at room temperature to low temperature.
[0091] The granules according to one embodiment have a simple sedimentation index of 2. That is, when 200 mL of water (4° C.) is poured into a 200 mL beaker, 6 g of the granules according to this embodiment is added, and the state is observed 1 minute, 5 minutes, and 10 minutes after the addition while maintaining the temperature at 4° C., the entire amount settles regardless of the time. The simple sedimentation index can be evaluated by the method described in the Examples below.
[0092] The granules according to one embodiment have a dispersibility index of 1.5 g or less. The dispersibility index can be evaluated by the method described in the Examples below, specifically by the following method. 200 mL of water (4.0°C) is poured into a 200 mL beaker containing 6 g of granules, and the mixture is stirred for 30 seconds with a magnetic stirrer (300 rpm). After stirring, the contents of the beaker are immediately poured onto a 1000 μm mesh sieve, and the weight of the contents remaining on the sieve is measured. The measured weight (weight on the sieve: unit g) is the dispersibility index. The dispersibility index of the granules according to this embodiment may be, for example, 1.4 g or less, 1.3 g or less, 1.2 g or less, 1.1 g or less, 1.0 g or less, 0.9 g or less, 0.8 g or less, 0.7 g or less, 0.6 g or less, or 0.5 g or less.
[0093] The granules according to this embodiment can be used as a material to be added to, for example, foods, food additives, pharmaceuticals, cosmetics, quasi-drugs or pharmaceuticals, animal feed, fertilizers, fragrances, antibiotics, soil conditioners, etc.
[0094] The present invention will be described in more detail below with reference to examples, although the present invention is not limited to the following examples.
[0095] [Test Method] In the following test examples, common procedures will be described first.
[0096] <Optical Microscope Observation> The sprayed liquid was dropped onto a slide glass, a cover glass was placed on top, and the sample was observed under an optical microscope at a magnification of 500 times.
[0097] <Measurement of Crystallization Rate> 1 g of the spray liquid was placed in a 1.5 mL Eppendorf tube and centrifuged at 16,000 rpm for 3 minutes using a centrifuge (Sakuma Seisakusho Co., Ltd., M150IV). The mass of the remaining crystals after removing the supernatant and the mass of the spray liquid were calculated using the following formula: Crystallization rate (mass %) = mass of remaining crystals (g) / mass of spray liquid (g) × 100
[0098] <Spray dryer> For spray drying, a spray dryer having the following configuration was used. Spray drying device: spray dryer (Okawahara Chemical Engineering Co., Ltd., OC-16 (dry type)) Spray liquid supply device: Mohno pump (Heishin Soubi Co., Ltd., 3NTL08PUL) Spray method: atomizer disk method The spray dryer settings are as follows: Hot air inlet temperature setting: 30°C Fan frequency setting: 60.0 Hz Exhaust fan frequency setting: 37.0 Hz Tower static pressure setting: slightly negative to slightly positive pressure (MPa) Atomizer disk frequency setting: 60 Hz Pump frequency setting: 11.0 Hz Raw material temperature setting: no setting (room temperature)
[0099] <Measurement of spray liquid supply rate> The liquid supply tube connected to the spray dryer was removed and placed in a 100 mL measuring cylinder, and the spray liquid was supplied. The spray liquid flowing out of the liquid supply tube was collected in the measuring cylinder for 60 seconds, and the spray liquid supply rate (mL / min) was measured.
[0100] <Measurement of moisture content of dried powder (loss on drying method)> 10 g of the recovered dried powder was weighed out, and the moisture content was measured at 105°C for 15 minutes using an infrared moisture meter (Kett Electric Laboratory).
[0101] <Measurement of Water Content of Dry Powder (Water Activity Method)> Water activity (Aw) was measured using 5 g or 10 mL of dry powder with a water activity measuring device (METER, Dew Point water activity Meter AquaLAb Series 4TE).
[0102] <Electron Microscope Observation of Dry Powder> The dry powder was sprinkled on an electromagnetic tape for electron microscope observation, and photographed using an electron microscope (Hitachi High-Technologies Corporation, Miniscope™3030).
[0103] <Evaluation of Dry Powder Fluidity> The "fluidity index" proposed by R. L. Carr was calculated for the dry powders of the Examples and Comparative Examples. (Carr, R. L. "Evaluating flow properties of solids." Chem. Eng. (1965) 72 (163-168)) The angle of repose (°), spatula angle (°), compressibility (%), and uniformity (-) of the dry powder were measured using a multifunctional powder property measuring instrument (Seishin Enterprise Co., Ltd., Multitester MT-02), and an index corresponding to each measured value was obtained based on Carr's theory. The index values for each measured value were summed to obtain the fluidity index. The temperature and humidity during the measurements were 25°C and 50%. The fluidity of the granules was evaluated based on Carr's evaluation criteria shown below. Fluidity evaluation criteria Fluidity index value Fluidity level 90-100 Very good 80-89 Good 70-79 Fairly good 60-69 Average 40-59 Not very good 0-19 Very poor
[0104] <Evaluation of bulk density of dry powder> The bulk densities (loose bulk density, packed bulk density, dynamic bulk density) of the dry powders of the examples and comparative examples were determined using a multifunctional powder property measuring instrument (Seishin Enterprise Co., Ltd., Multitester MT-02).
[0105] <Evaluation of cold water dispersibility of dry powder> The cold water dispersibility (simple sedimentation index, dispersibility index) of the dry powders of the examples and comparative examples was evaluated according to the method described in WO 2020 / 095663.
[0106] (Evaluation of Simple Settling Index) 200 mL of water (4°C) was poured into a 200 mL beaker. After adding 6 g of dry powder, the state of the powder was observed while the beaker was kept in a refrigerator at 4°C. The time from addition was measured with a stopwatch, and the degree to which the powder on the surface of the cold water had settled into the water was evaluated at 1 minute, 5 minutes, and 10 minutes based on the following simple settling index. Simple settling index 2: The entire amount settled regardless of the time 1: About half of the amount settled, but the entire amount did not settle 0: No settling at all
[0107] (Evaluation of Dispersibility Index) 200 mL of water (4.0°C) was poured into a 200 mL beaker containing 6 g of dry powder, and the mixture was stirred for 30 seconds with a magnetic stirrer (300 rpm). After stirring, the contents of the beaker were immediately poured onto a sieve with 1000 µm openings, and the weight of the contents remaining on the sieve was measured.
[0108] Test Example 1: Production and Evaluation of Granules Using Whole Egg Liquid as a Functional Ingredient (Preparation of Spray Liquid) 4,000 g of frozen whole eggs (Kewpie Corporation, frozen whole eggs (for confectionery)) were thawed overnight at room temperature of 25° C. to obtain 4,000 g of whole egg liquid. The resulting 4,000 g of whole egg liquid was transferred to a 10 L stainless steel mug, and then 4,000 g of trehalose (Hayashibara Co., Ltd., Treha Fine Powder) was gradually added while stirring at 350 rpm using a mixer (Shinto Co., Ltd., Three-One Motor, BL-1200) to obtain a total of 8,000 g of trehalose-containing whole egg liquid. This was used as the spray liquid.
[0109] The resulting spray solution was observed under an optical microscope and the crystallization rate was measured, confirming that a portion of the trehalose was contained in a crystalline state. Figure 1 shows an example of an optical microscope image (magnification: 500x) of the spray solution. The spray solution obtained above contained trehalose crystals with particle sizes of 20 to 80 µm. The crystallization rate of the spray solution obtained above was also 40%. These findings confirmed that the spray solution obtained contained trehalose in a crystalline state.
[0110] (Spray drying) The entire amount of the obtained spray liquid was used and spray-dried for 90 minutes in a spray dryer under the following conditions: Ambient temperature: 34.3°C Ambient humidity: 54.5% RH Spray liquid temperature: 29.0°C Inlet temperature: 35.0°C Outlet temperature: 29.7°C Spray liquid supply rate: 68 mL / min Atomizer rotation speed: 25,500 rpm Air flow rate: 60 Hz Exhaust air flow rate: 38 Hz Dried product temperature: 29.0°C After spraying was completed, dry air was continued to be sent for 30 minutes without changing the operating conditions of the spray dryer to dry the interior of the dryer. The dried powder was then scraped off and collected. The obtained dry powder was designated as the dried powder of Example 1-1.
[0111] (Evaluation of Dry Powder) The dry powder of Example 1-1 was evaluated. As a comparison, a similar evaluation was performed using dried egg white (Kewpie Corporation) (Comparative Example 1-1) and dried whole egg No. 1 (Kewpie Corporation) (Comparative Example 1-2).
[0112] The moisture content of the dried powder of Example 1-1 was confirmed by the water activity method and the loss on drying method. The water activity (Aw) measured by the water activity method was 0.6244. The moisture content measured by the loss on drying method was 9.80%.
[0113] The dry powder of Example 1-1 was observed under an electron microscope. Figure 2 shows an example of an electron microscope image of the dry powder of Example 1-1. Figure 2(A) is an electron microscope image at a magnification of 1000x, and Figure 2(B) is an electron microscope image at a magnification of 500x. As shown in Figure 2, it was confirmed that the dry powder of Example 1-1 was made up of granules surrounded by trehalose crystals.
[0114] The dry powders of Example 1-1 and Comparative Examples 1-1 and 1-2 were evaluated for dispersibility in cold water. The evaluation results of the simple sedimentation index and dispersibility index are shown in Table 1.
[0115] As a result of the evaluation of the simple sedimentation index, the dry powder of Example 1-1 immediately and completely settled, whereas the dry powders of Comparative Examples 1-1 and 1-2 did not settle. As a result of the evaluation of the dispersibility index, the dry powder of Example 1-1 formed few lumps (whole powder) and the contents remaining on the sieve were small, whereas the dry powders of Comparative Examples 1-1 and 1-2 formed many lumps (whole powder) and the contents remaining on the sieve were large. As is clear from these results, the dry powder of Example 1-1 had excellent dispersibility in cold water.
[0116] The dry powders of Example 1-1 and Comparative Examples 1-1 and 1-2 were evaluated for fluidity. The evaluation results of fluidity are shown in Table 2.
[0117] The bulk density of the dry powders of Example 1-1 and Comparative Examples 1-1 and 1-2 was evaluated. The results of the bulk density evaluation are shown in Table 3.
[0118] Test Example 2: Production and Evaluation of Granules Using Coffee Creamer as a Functional Material (Preparation of Spray Liquid) A container of liquid coffee creamer (Marim, Ajinomoto AGF Inc.) was opened and transferred to a 10 L stainless steel mug, and 2500 g of liquid coffee creamer was recovered. While stirring at 350 rpm using a mixer (Three-One Motor, BL-1200, Shinto Co., Ltd.), 2500 g of lactose (Ala, 100 mesh ON, Shoei Foods Industry Co., Ltd.) was gradually added to obtain a total of 5000 g of lactose-containing coffee creamer. This was used as the spray liquid.
[0119] The resulting spray liquid was observed under an optical microscope and the crystallization rate was measured, confirming that a portion of the lactose was present in a crystalline state. Figure 3 shows an example of an optical microscope image (magnification: 500x) of the spray liquid. The spray liquid obtained above contained lactose crystals with particle sizes of 20 to 80 μm. The crystallization rate of the spray liquid obtained above was also 40%. These findings confirmed that the spray liquid obtained contained crystalline lactose.
[0120] (Spray drying) The entire amount of the obtained spray liquid was used and spray-dried for 90 minutes in a spray dryer under the following conditions: Ambient temperature: 33.9°C Ambient humidity: 51.6% RH Spray liquid temperature: 28.7°C Inlet temperature: 33.3°C Outlet temperature: 28.7°C Spray liquid supply rate: 69 mL / min Atomizer rotation speed: 25,500 rpm Air flow rate: 60 Hz Exhaust air flow rate: 38 Hz Dried product temperature: 29.0°C After spraying was completed, dry air was continued to be sent for 30 minutes without changing the operating conditions of the spray dryer to dry the interior of the dryer. The dried powder was then scraped off and collected. The obtained dry powder was designated as the dried powder of Example 2-1.
[0121] (Evaluation of Dry Powder) The dry powder of Example 2-1 was evaluated. Similar evaluations were carried out using creaming powder (Nestlé Japan Ltd., Bright) (Comparative Example 2-1), powdered cream (Morinaga Milk Industry Co., Ltd., Crepe) (Comparative Example 2-2), and powdered oils and fats (The Nisshin Oillio Group, Ltd., Nisshin MCT Powder) (Comparative Example 2-3) as comparisons.
[0122] The moisture content of the dried powder of Example 2-1 was confirmed by the water activity method and the loss on drying method. The water activity (Aw) measured by the water activity method was 0.3542. The moisture content measured by the loss on drying method was 1.99%.
[0123] The dry powder of Example 2-1 was observed under an electron microscope. Figure 4 shows an example of an electron microscope image of the dry powder of Example 2-1. Figure 4(A) is an electron microscope image at a magnification of 1000x, and Figure 4(B) is an electron microscope image at a magnification of 500x. As shown in Figure 4, it was confirmed that the dry powder of Example 2-1 was made up of granules surrounded by lactose crystals.
[0124] The dry powders of Example 2-1 and Comparative Examples 2-1 to 2-3 were evaluated for cold water dispersibility. The evaluation results of the simple sedimentation index and dispersibility index are shown in Table 4.
[0125] As a result of the evaluation of the simple sedimentation index, the dry powder of Example 2-1 immediately and completely settled, while the dry powders of Comparative Examples 2-1 to 2-3 did not settle. As a result of the evaluation of the dispersibility index, the dry powder of Example 2-1 formed few lumps (whole powder) and the contents remaining on the sieve were small, while the dry powders of Comparative Examples 2-1 to 2-3 formed many lumps (whole powder) and the contents remaining on the sieve were large. As is clear from these results, the dry powder of Example 2-1 had excellent dispersibility in cold water.
[0126] The dry powders of Example 2-1 and Comparative Examples 2-1 to 2-3 were evaluated for fluidity. The results of the evaluation of fluidity are shown in Table 5.
[0127] The bulk density of the dry powders of Example 2-1 and Comparative Examples 2-1 to 2-3 was evaluated. The results of the bulk density evaluation are shown in Table 6.
Claims
1. A method for producing granules, comprising the steps of: mixing at least one raw material selected from the group consisting of crystalline sugars and crystalline sugar alcohols with a functional material to obtain a spray liquid containing the raw material and the functional material, with a portion of the raw material being in a crystalline state; and spray-drying the spray liquid under low-temperature conditions, wherein the functional material is a functional material with a high moisture content.
2. A method for producing granules, comprising the steps of: mixing at least one raw material selected from the group consisting of crystalline sugars and crystalline sugar alcohols with a functional material, and obtaining a spray liquid containing the raw material and the functional material without using a solvent, with a portion of the raw material being in a crystalline state; and spray-drying the spray liquid under low-temperature conditions.
3. The manufacturing method described in claim 1 or 2, wherein the crystallization rate of the raw material in the spray liquid is 5 mass% or more and 50 mass% or less.
4. The method according to claim 1 or 2, wherein the sugar and sugar alcohol are monosaccharides, disaccharides, trisaccharides and their sugar alcohols.
5. The method according to claim 1 or 2, wherein the sugar and the sugar alcohol are at least one selected from the group consisting of palatinose, sucrose and trehalose.
6. The method according to claim 1 or 2, wherein the spray drying is carried out under conditions of an inlet temperature of 0 to 60°C.
7. The method according to claim 1 or 2, wherein the functional ingredient is liquid egg, creamer, fruit juice, vegetable juice, or liquid dairy material.
8. Granules comprising at least one selected from the group consisting of crystalline sugar and crystalline sugar alcohol, and a solid portion of a functional material having a high moisture content, wherein a portion of the sugar and / or sugar alcohol is in a crystalline state and another portion is in a non-crystalline state.
9. The granules according to claim 8, wherein the amorphous sugar and / or sugar alcohol and the solid content are retained in gaps formed between the crystalline sugar and / or sugar alcohol.
10. A granule according to claim 8 or 9, wherein the sugar and sugar alcohol are monosaccharides, disaccharides, trisaccharides and their sugar alcohols.
11. Granules according to claim 8 or 9, wherein the sugar and sugar alcohol are at least one selected from the group consisting of palatinose, sucrose and trehalose.
12. A granule according to claim 8 or 9, wherein the high moisture functional ingredient is liquid egg, creamer, fruit juice, vegetable juice or liquid dairy product.
Citation Information
Patent Citations
Trehalose-containing composition
JP2000159788A
Solid milk and method for producing the same
JP2016039826A
Method for producing granule, and granule
JP2021106571A
Dry powder holding flavor and aroma components and process for producing the same
WO2003068007A1