Method for producing granules, and granule

Abstract

To provide a method for producing granules of a functional material having a high moisture content, which can be obtained by spray-drying under a low temperature condition and exhibits excellent dispersibility in a solvent at room temperature to low temperature.SOLUTION: A method for producing granules comprises: a step in which at least one raw material selected from the group consisting of crystalline sugars and crystalline sugar alcohols is mixed with a functional material to obtain a spray liquid that contains the raw material and the functional material, and in which part of the raw material is contained in a crystalline state; and a step in which the spray liquid is spray-dried under a low temperature condition, wherein the functional material is a functional material having a high moisture content.SELECTED DRAWING: None

Description

Technical Field

[0001] The present invention relates to a method for producing granules and to the granules.

Background Art

[0002] When providing a functional material that is liable to deteriorate due to factors such as light, heat, moisture, oxygen, and time-dependent changes as a raw material for food and pharmaceuticals, it is very important to maintain the quality of the functional material over a long period in consideration of the deterioration factors (light, temperature, humidity, oxygen, time-dependent changes, etc.) during the storage period until it is used as a raw material. As a method for improving the stability of such a functional material, there is drying and powdering, and as one method of drying and powdering, there is spray drying (also referred to as spray drying, SD).

[0003] Spray drying is a method of spraying a solution or suspension containing a functional material into a drying gas and rapidly drying it to obtain a dry powder or granule. Generally, hot air heated to about 100 to 200°C is used as the drying gas. However, there are cases where it is desired to avoid using a 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 a low temperature together with a crystal suspension in which a part of a crystalline sugar and / or sugar alcohol is contained in a crystalline state, and an invention of granules produced by the method are disclosed (Patent Document 1 and Patent Document 2).

Prior Art Documents

Patent Documents

[0004]

Patent Document 1

Patent Document 2

Summary of the Invention

Problems to be Solved by the Invention

[0005] The methods disclosed in Patent Document 1 and Patent Document 2 first produce a crystal suspension in which a part of the crystalline sugar and / or sugar alcohol is contained in a crystalline state, and then mix this crystal suspension with a functional material to prepare a spray liquid. At this time, in order to enable the production of a dry powder (granules) by spray drying under low-temperature conditions, it is necessary to maintain a state in which a part of the crystalline sugar and / or sugar alcohol is contained in a crystalline state in the spray liquid.

[0006] For this reason, in the methods disclosed in Patent Document 1 and Patent Document 2, in the case of functional materials with a high water content (for example, liquid eggs in which about 75% is water, creamers (such as coffee creamers) in which about 50 to 70% is water, and liquid milk materials such as whole milk in which about 88% is water, as well as fruit juices and vegetable juices in which more than 90% is water), when attempting to obtain granules sufficiently containing components other than water (solids, etc.), it is necessary to increase the blending ratio of the functional material, and inevitably the ratio of water also increases. Therefore, it has sometimes been difficult to obtain a spray liquid in which a part of the crystalline sugar and / or sugar alcohol is contained in a crystalline state.

[0007] On the other hand, in a composition prepared in powder or granule form from a functional material with a high water content such as powdered eggs, powdered milk, pressed juice powder of fruits, pressed juice powder of vegetables, coffee creamer powder, etc., using a general spray drying method, it is known that lumps (undissolved powder) are generated when the composition is dissolved in a solvent at normal temperature to low temperature. The need for a technique to make it less likely to form lumps (undissolved powder) in the dissolution operation in a solution at normal temperature to low temperature has been increasing even when such a functional material with a high water content is spray dried.

[0008] In view of the above-mentioned problems of the prior art, an object of the present invention is to provide a method for producing granules of a functional material with a high water content that can be obtained by spray drying under low-temperature conditions and has excellent dispersibility in a solvent at normal temperature to low temperature. Another object of the present invention is to provide granules obtained by the method.

Means for Solving the Problems

[0009] The present invention relates to a method for producing granules, comprising: a step 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 and having a part of the raw material contained in a crystalline state; and a step of spray-drying the spray liquid under low-temperature conditions, wherein the functional material is a functional material having a high water content.

[0010] The present invention also relates to a method for producing granules, comprising: a step 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 without using a solvent and having a part of the raw material contained in a crystalline state; and a step of 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 crystal suspension of the at least one raw material, to obtain a spray liquid containing the raw material and the functional material and having a part of the raw material contained in a crystalline state, and further spray-drying the spray liquid under low-temperature conditions. Thereby, even a functional material having a high water content can be used to produce granules by spray-drying under low-temperature conditions, and the resulting granules have excellent dispersibility in solvents at normal temperature to low temperature.

[0012] In the above 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. Thereby, the effects of the present invention described above can be more significantly achieved.

[0013] In the above production method, the spray-drying may be performed, for example, under conditions where the inlet temperature is 0 to 60°C.

[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 the solid content of a functional material having a high water content, wherein part of the sugar and / or the sugar alcohol is in a crystalline state and the other part is in an amorphous state.

[0015] The granules may be those in which 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.

[0016] The sugar and the sugar alcohol may be, for example, monosaccharides, disaccharides, trisaccharides, and their sugar alcohols. Further, the sugar and the sugar alcohol may be at least one selected from the group consisting of, for example, palatinose, sucrose, and trehalose.

[0017] The functional material may be, for example, liquid egg, creamer, fruit juice, vegetable juice, or liquid milk material.

[0018] The present invention includes, for example, the following inventions. [1] A step of mixing at least one raw material selected from the group consisting of crystalline sugars and crystalline sugar alcohols and a functional material to obtain a spray liquid containing the raw material and the functional material and having a part of the raw material in a crystalline state, A step of spray-drying the spray liquid under low-temperature conditions, and A method for producing granules, wherein the functional material is a functional material having a high water content. [2] A step of mixing at least one raw material selected from the group consisting of crystalline sugars and crystalline sugar alcohols and a functional material to obtain a spray liquid containing the raw material and the functional material without using a solvent and having a part of the raw material in a crystalline state, A step of spray-drying the spray liquid under low-temperature conditions, and [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 one of [1] to [3], wherein the sugar and the sugar alcohol are monosaccharides, disaccharides, trisaccharides, and sugar alcohols thereof. [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 production method according to any one of [1] to [5], wherein the spray drying is performed under the condition that the inlet temperature is 0 to 60°C. [7] The production method according to any one of [1] to [6], wherein the functional material is liquid egg, creamer, fruit juice, vegetable juice, or liquid milk material. [8] Containing at least one selected from the group consisting of crystalline sugar and crystalline sugar alcohol, and the solid content of the functional material with a high water content, The sugar and / or the sugar alcohol is a granule in which a part is in a crystalline state and the other part is in an amorphous state. [9] The granule according to [8], wherein the amorphous sugar and / or sugar alcohol and the solid content are retained in the gaps formed between the crystalline sugar and / or sugar alcohol.

[10] The granule according to [8] or [9], wherein the sugar and the sugar alcohol are monosaccharides, disaccharides, trisaccharides, and sugar alcohols thereof.

[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 granule according to any one of [8] to

[11] , wherein the functional material with a high water content is liquid egg, creamer, fruit juice, vegetable juice, or liquid milk material.

Advantages of the Invention

[0019] According to the present invention, it is possible to provide a method for producing granules of a functional material with a high water content, which can be obtained by spray drying under low-temperature conditions and has excellent dispersibility in a normal-temperature to low-temperature solution. According to the present invention, it is also possible to provide granules obtained by the method.

[0020] The present inventors added 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 prepared a spray liquid (crystal suspension) by utilizing the water originally contained in the functional material without newly adding water. As a result, it was found that spray drying is possible under low-temperature conditions, and the granules obtained by spray drying have excellent dispersibility in a normal-temperature to low-temperature solvent. The present invention is based on this finding.

[0021] The granules according to the present invention contain crystalline sugars and / or sugar alcohols, so irregularities are formed on the surface of the granule particles, and the contact surface between the granule particles becomes small, resulting in excellent fluidity. Therefore, the granules according to the present invention are excellent in operability. The granules according to the present invention contain crystalline sugars and / or sugar alcohols, so the granule particles are less likely to deteriorate or break due to physical or mechanical stimuli, and the stability and storage properties of the particle structure are also excellent.

[0022] In addition, when the granules according to the present invention are returned to a solution containing a functional material using a normal-temperature to low-temperature solvent (for example, water), the formation of lumps (undissolved powder) is suppressed, and they exhibit the property of quickly dispersing in the solution. Therefore, for example, when a food material is adopted as the functional material, it does not impair the usability of food processors and consumers.

[0023] When the granules according to the present invention are blended in a powder mix product eaten with a normal-temperature to low-temperature solution (for example, a solution such as water, milk, or carbonated water), they can be prepared in a normal-temperature to low-temperature temperature range suitable for eating from the beginning, so they do not require operations such as mixing with ice, maintaining at room temperature or under refrigeration, and temporarily heating to a high temperature for dissolution and then cooling.

[0024] In addition, since the granules according to the present invention are obtained by spray drying under low-temperature conditions, the functions of the functional materials contained therein are less likely to be lost due to heat. That is, in the granules according to the present invention, the functions of the functional materials are well maintained. Usually, when obtaining granules by spray drying, it is difficult to obtain suitable granules unless spray drying is performed under higher-temperature conditions. However, since the granules according to 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 under low-temperature conditions. For example, in fruit juices and vegetable juices, in the conventional method, discoloration and deterioration in terms of taste and aroma occurred during spray drying, whereas in the method according to the present invention, it is possible to powderize (granulate) while maintaining the color, taste, and aroma of the functional materials.

[0025] Moreover, the method for producing the 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, it is not necessary to separately prepare a crystal suspension of at least one raw material selected from the group consisting of sugar and sugar alcohol, and the steps of completely dissolving the raw material and crystallizing the raw material can be omitted. Therefore, it is possible to produce granules by a method that is simpler than the conventional method.

[0026] The method for producing the granules according to the present invention can perform spray drying of a functional material with a high water content at a low temperature, so that low-stability components contained in liquid eggs, liquid dairy materials, fruit juices / vegetable juices, extracts of fruits / vegetables, creamers, etc. can be made into dry-state granules without being deteriorated. Therefore, considering the factors causing deterioration (light, temperature, humidity, oxygen, time-dependent changes, etc.) during the storage period of the functional material, the quality of the functional material can be maintained over a long period.

Brief Description of the Drawings

[0027]

Figure 1

Figure 2

Figure 3

Figure 4

Embodiments for Carrying Out the Invention

[0028] Hereinafter, embodiments for carrying out the present invention will be described in detail. However, the present invention is not limited to the following embodiments.

[0029] 〔Method for Producing Granules〕 One aspect of the present invention is to mix at least one raw material selected from the group consisting of crystalline sugar and crystalline sugar alcohol with a functional material to obtain a spray liquid containing the raw material and the functional material and having a part of the raw material contained in a crystalline state (mixing step A), and a step of spray-drying the spray liquid under low-temperature conditions (spray-drying step), and relates to a method for producing granules, wherein the functional material is a functional material having a high water content.

[0030] One aspect of the present invention also relates to a method for producing granules, which comprises mixing at least one raw material selected from the group consisting of crystalline sugar and crystalline sugar alcohol with a functional material to obtain a spray liquid containing the raw material and the functional material without using a solvent and having a part of the raw material contained in a crystalline state (mixing step B), and a step of spray-drying the spray liquid under low-temperature conditions (spray-drying step).

[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 sugar and crystalline sugar alcohol (hereinafter, also simply referred to as "raw material") and a functional material, and a part of the raw material is contained in a crystalline state.

[0032] The spray liquid may contain other components in addition to the raw materials and functional materials, as long as the effects according to the present invention are not impaired. Examples of the other components include components that can be tolerated as foods or pharmaceuticals. Specifically, for example, preservatives, high-intensity sweeteners, fragrances, thickeners, lubricants (e.g., calcium stearate), components for protecting proteins and live bacteria (e.g., proteins such as casein, antioxidants such as vitamin C, phosphate buffer solutions), 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), and the like can be mentioned.

[0033] One aspect of the mixing step may be a step (mixing step A) of obtaining a spray liquid in which at least one raw material selected from the group consisting of crystalline sugars and crystalline sugar alcohols is mixed with a functional material having a high water content, and a part of the raw material is contained in a crystalline state. In mixing step A, other components may be mixed in addition to the raw materials and functional materials, if necessary. Also, as long as the above-described spray liquid is obtained, a solvent may be mixed. The mixing can be carried out, for example, by stirring or the like. Mixing step A can be carried out, for example, by stirring for 10 minutes to 3 hours while maintaining the temperature at 25 to 35°C. The rotation speed during stirring may be, for example, 250 to 400 rpm.

[0034] Another aspect of the mixing process may be a step (Mixing Process 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 in which a part of the raw material is contained in a crystalline state without using a solvent. In Mixing Process B, other components may be mixed in addition to the raw materials and the functional material, if necessary. Mixing Process B can be carried out, for example, by mixing the raw materials, the functional material, etc. Mixing can be performed, for example, by stirring or the like. Mixing Process B can be carried out, for example, by stirring for 10 minutes to 3 hours while maintaining the temperature at 25 to 35°C. The rotation speed during stirring may be, for example, 250 to 400 rpm. The functional material used in Mixing Process B may be a functional material with a high water content or may not be a functional material with a high water content, but since no solvent is used, it is preferably a functional material with a high water content.

[0035] In the mixing process (Mixing Process A and Mixing Process B), a spray liquid in which a part of the raw material is contained in a crystalline state may be obtained without dissolving all of the raw materials, or after dissolving all of the raw materials, precipitation of the raw material crystals and / or recrystallization of the raw materials may be carried out to obtain a spray liquid in which a part of the raw material is contained in a crystalline state. The fact that a part of the raw material is contained in a crystalline state can be confirmed, for example, visually. Other methods for confirming that a part of the raw material is contained in a crystalline state include, for example, observing crystallization induction with a microscope. When the spray liquid dropped on a slide glass is observed with a microscope at room temperature of 25°C for 5 minutes, if the presence of crystals is confirmed, it can be determined that a part of the raw material is contained in a crystalline state.

[0036] Precipitation of the raw material crystals and / or recrystallization of the raw materials after dissolving all of the raw materials can be carried out by known methods. Methods for precipitating the raw material crystals and / or recrystallizing the raw materials after dissolving all of the raw materials include a method of cooling the raw material solution (cooling crystallization method), a method of adding a non-solvent such as ethanol to the mixed solution (non-solvent crystallization), and a reaction crystallization method, etc.

[0037] As used herein, the term "crystalline sugar and / or sugar alcohol" means a solid sugar and / or sugar alcohol in which the constituent atoms form a three-dimensionally regular repeat. As used herein, the term "non-crystalline sugar and / or sugar alcohol" means a solid or liquid sugar and / or sugar alcohol that does not have such a regular repeat.

[0038] Crystalline sugars and crystalline sugar alcohols are preferably monosaccharides, disaccharides, trisaccharides, and sugar alcohols thereof, from the viewpoint of enhancing the operability in the mixing step.

[0039] Examples of monosaccharides include glucose, galactose, mannose, fructose, allose, altrose, etc. Examples of disaccharides include isomaltulose, sucrose, lactulose, lactose, maltose, trehalose, cellobiose, etc. Examples of trisaccharides include nigero triose, maltotriose, raffinose, etc. Note that isomaltulose is a disaccharide trademarked by DM Mitsui Sugar Co., Ltd. as "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. Note that reduced palatinose is a mixture of 1,1-GPM and 1,6-GPS trademarked 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, two or more crystalline sugar alcohols, or a combination of crystalline sugars and crystalline sugar alcohols in two or more.

[0042] The content of the crystalline sugar and / or sugar alcohol contained in the spray liquid can be appropriately set according to the type of functional material to be used and the like. For example, the content of the crystalline sugar and / or sugar alcohol contained in the spray liquid can be set so that the crystallization rate in the spray liquid falls within the range described later. Also, for example, although not limited thereto, the content of the crystalline sugar and / or sugar alcohol contained in the spray liquid is, based on the total amount of the spray liquid, 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, 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 as long as it is a material or component that exhibits some function in a composition (such as food, pharmaceuticals, 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 rays, electrical interaction, physical stimulation, or a material that loses its function by heating.

[0044] The method for producing the granules according to the present embodiment can obtain granules by spray drying under low-temperature conditions even when the functional material contains a large amount of moisture, and the granules have the effect of being excellent in dispersibility in a solvent at normal temperature to low temperature. Therefore, as the functional material, a functional material with a high moisture content can be used.

[0045] In this specification, the "functional material with a high moisture content" means a functional material whose moisture content is 20% or more on a mass basis based on the total amount of the functional material. The moisture content is, 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 on a mass basis based on the total amount of the functional material. The moisture content can be measured by appropriately selecting a known method such as a heat drying method, a Karl Fischer method, or a distillation method according to the type of the functional material.

[0046] Examples of functional materials with a high water content include, but are not limited to, liquid milk materials such as liquid eggs, creamers, whole milk, whey, and fresh cream, fruit juices, vegetable juices, and extracts of fruits and vegetables.

[0047] The technique of powdering liquid eggs by spray drying has been known for a long time, and techniques of adding additives such as saccharides and casein during spray drying for the purpose of preventing deterioration and improving quality have also been known. However, powdered eggs obtained by spray drying liquid eggs (whole egg liquid, egg white liquid, egg yolk liquid, etc.) by conventional methods have problems such as difficulty in dissolution operations because lumps (undissolved powder) are formed during dissolution operations in solvents at normal to low temperatures (for example, water), and the texture is affected. According to the method for producing granules according to this embodiment, these problems of the prior art can be solved.

[0048] Non-dairy coffee creamers in which vegetable oil is emulsified with casein, dairy coffee creamers in which milk fat is emulsified with casein, etc., cream powder obtained by drying creamers prepared by a method of emulsifying oil in water, or powdered products obtained by spray drying liquid milk materials such as whole milk, whey, and fresh cream by conventional methods have problems with solubility in solvents at normal to low temperatures (for example, water). To improve solubility in cold water, a method of coating the surface of the powder with a composition such as fats and oils and fatty acids has been known. However, this method has problems such as a complicated manufacturing process and the need to use additives such as fats and oils and fatty acids. According to the method for producing granules according to this embodiment, these problems of the prior art can be solved.

[0049] Powdered products obtained by spray drying fruit juices, vegetable juices, and extracts of fruits and vegetables by conventional methods have problems such as deterioration of color, taste, and aroma. According to the method for producing granules according to this embodiment, these problems of the prior art can be solved.

[0050] The content of the functional material contained in the spray liquid can be appropriately set according to the type of the functional material used and the like. 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 falls within the range described later. Also, for example, although not limited thereto, the content of the functional material contained in the spray liquid is, based on the total amount of the spray liquid, 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, 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] Since the crystallization rate in the spray liquid can more significantly exhibit the effects according to the present invention, it 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. 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 put into a 1.5 mL Eppendorf tube, and centrifuged at 16,000 rpm for 3 minutes using a centrifuge (for example, Sakuma Seisakusho Co., Ltd., M150IV), and it is a value calculated by applying the remaining crystal mass when the supernatant is removed and the mass of the spray liquid to the following formula. Crystallization rate (% by mass) = Remaining crystal mass (g) / Mass of spray liquid (g) × 100

[0052] The crystallization rate in the spray liquid can be adjusted by adjusting the usage ratio of at least one raw material selected from the group consisting of crystalline sugar and crystalline sugar alcohol and the functional material. Also, the crystallization rate in the spray liquid can be adjusted, for example, by performing operations such as physically or chemically adding or removing crystals, such as filter filtration, centrifugation, gravitational sedimentation, dissolution by adding water and / or heating, and adjustment of consumption of crystal components accompanying chemical reactions. Furthermore, it can also be adjusted by operations such as increasing crystals, such as input and mixing of crystal components.

[0053] The spray liquid contains a part of the raw materials in a crystalline state. The spray liquid only needs to contain crystal nuclei, and the size of the crystal nuclei is not particularly limited as long as it is equal to or larger than the size that can stably exist in the spray liquid. The size of the crystal nuclei may be, for example, equal to or larger than the critical crystal nuclei.

[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 operations such as addition and removal of solvents or solutes, solvent temperature, dissolution time, change of stirring time, crushing by a stirrer or grinder, fractionation by filtration, etc., and crystallization operations such as hydrolysis of sugar.

[0056] The "average particle size of the crystalline sugar and / or sugar alcohol" in this specification can be measured by a digital microscope. For measurement, for example, SKM-S31B-PC manufactured by Saito Optical Co., Ltd. can be used. Specifically, for example, it can be measured by the following method. Drop the spray liquid onto a slide glass, place a cover glass on it, and measure at a magnification of 1000 times. The method for measuring the average particle size is to take the average of the particle sizes of any 10 or more crystals using a digital microscope (for example, Saito Optical Co., Ltd., SKM-S31B-PC). For 10 or more particles to be measured in the spray liquid, when the distance in the first direction and the distance in the second direction orthogonal to the first direction intersect at their respective midpoints, the distance in the first direction and the distance in the second direction are taken as the lateral width and the longitudinal width, respectively. The first direction is the same direction for all the particles to be measured. Among the measured lateral width and longitudinal width, the longer one is taken as the major axis, and the shorter one is taken as the minor axis, and the average in the particles to be measured is taken as the average major axis and the average minor axis.

[0057] The standard deviation of the average particle size of 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 a small variation in the average particle size. The standard deviation of the average particle size of 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 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" is the unbiased standard deviation obtained by the STDEV.S function of Microsoft (registered trademark) Excel.

[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 (not derived from the functional material but added water). When the functional material is a functional material with a high water content, the spray liquid can be obtained by using the water originally contained in the functional material without adding a new solvent, so it is not necessarily required 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 process> The spray drying process is a process of spray drying the above-described spray liquid under low-temperature conditions. Spray drying can be performed, for example, using a spray drying device (spray dryer). As the spray drying device, for example, OC-16 manufactured by Okawara Kako Co., Ltd. can be used.

[0062] The low-temperature conditions mean that the temperature is lower than the temperature (for example, higher than 60°C) at which conventional spray drying has been performed (for example, 60°C or lower). In the present embodiment, since a spray liquid containing a part of sugar and / or sugar alcohol in a crystalline state is used, suitable granules can be obtained even when spray drying is performed under lower-temperature conditions than before. The low-temperature conditions may be temperature conditions such that the functions of the functional material are not lost.

[0063] Performing spray drying under low-temperature conditions means that the inlet temperature (inlet air temperature) in the spray drying device is performed under the temperature conditions as described above.

[0064] In one embodiment, the inlet temperature in the spray drying process is, for example, 60°C or lower, 55°C or lower, 50°C or lower, 45°C or lower, 40°C or lower, 35°C or lower, 30°C or lower, 25°C or lower, 20°C or lower, or 15°C or lower. The inlet temperature may be, for example, 0°C or higher, 5°C or higher, or 10°C or higher. That is, the inlet temperature in the spray drying process may be, for example, 0 to 60°C, or may be 0 to 50°C.

[0065] The outlet temperature (exhaust air temperature) in the spray drying device may be, for example, 50°C or lower, 40°C or lower, 35°C or lower, 30°C or lower, 25°C or lower, 20°C or lower, or 15°C or lower, and may be 0°C or higher, 5°C or higher, or 10°C or higher.

[0066] In the spray drying process, the liquid temperature of the spray liquid may be, for example, 60°C or lower, 50°C or lower, or 45°C or lower, and may be 10°C or higher, 15°C or higher, or 20°C or higher.

[0067] In spray drying, other conditions such as the supply amount of the spray liquid, the atmospheric temperature, and the atmospheric humidity may be appropriately adjusted respectively.

[0068] For example, the atomizer rotation speed in spray drying may be 3000 rpm or higher, 5000 rpm or higher, or 10000 rpm or higher, and may be 25000 rpm or lower, 20000 rpm or lower, or 18000 rpm or lower.

[0069] In the spray drying process, for example, for the purpose of adjusting the moisture content of the granules, a further post-drying process may be provided. The post-drying process may be, for example, blowing air for a predetermined time to the granules adhering to the can wall in the spray dryer to further volatilize the moisture of the granules. Alternatively, it may be to store the granules obtained by spray drying in a desiccator containing silica gel for a predetermined time.

[0070] <Granules> The granules according to this embodiment contain at least one selected from the group consisting of crystalline sugar and crystalline sugar alcohol and the solid content of a functional material with a high moisture content, and the crystalline sugar and / or sugar alcohol is partially in a crystalline state and partially in an amorphous state. The granules can be obtained, for example, by the above-described method for producing granules.

[0071] The "granules" in this specification are an aggregate of particles, and the particles (granule particles) constituting the granules contain one or more selected from the group consisting of crystalline sugar and sugar alcohol.

[0072] The "solid content of the functional material" in this specification is the solid content remaining after removing moisture from the functional material. The removal of moisture is carried out, for example, by the above-described spray drying.

[0073] The granules may contain two or more crystalline sugars, two or more crystalline sugar alcohols, or a combination of two or more crystalline sugars and crystalline sugar alcohols.

[0074] The granules according to one embodiment are composed of granule particles in which part of the crystalline sugar and / or sugar alcohol is in a crystalline state and the crystalline sugars and / or sugar alcohols in this crystalline state aggregate with each other. In this case, it is preferable that the other part (the other part) of the crystalline sugar and / or sugar alcohol is in an amorphous state and is held in the gaps formed between the aggregated crystalline sugars and / or sugar alcohols. It is also preferable that the functional material is held in the gaps formed between the crystalline sugars and / or sugar alcohols.

[0075] The aggregation of the crystalline sugars and / or sugar alcohols with each other can be confirmed by observing the appearance of the granule particles or the cross-section of the granule particles by a scanning electron microscope (SEM) or a digital microscope. The fact that the amorphous sugar and / or sugar alcohol and the functional material are held in the above gaps can be confirmed by the following method. (1) Observe the morphology of the granules during heating with a differential scanning calorimeter (DSC, for example, the RealView DSC (TA7000) manufactured by Hitachi High-Tech Science Corporation). Thereby, it can be visually confirmed that the amorphous sugar and sugar alcohol undergo a glass transition upon heating. (2) Observe the difference in polarization properties between the crystalline state and the amorphous state with a polarizing microscope (for example, the polarizing microscope (MT9200L) manufactured by Mage Techno Co., Ltd.).

[0076] The number of crystalline sugars and / or sugar alcohols (the number of crystals) contained in the particles constituting the granules may be, for example, 10 or more, 50 or more, or 100 or more. The number of crystals may be 1000 or less. The number of crystals can be measured visually by observing with a scanning electron microscope.

[0077] The shape of the particles constituting the granules may be substantially ellipsoidal or substantially spherical. The particles constituting the granules may have irregularities on their surfaces.

[0078] The average particle size of the particles 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 also 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 particles may be, for example, 20.00 to 118.00 μm.

[0079] The "average particle size of the particles" in this specification can be measured by an electron microscope. For the measurement, for example, MiniscopeTM3030 manufactured by Hitachi High-Technologies Corporation can be used. Specifically, for example, it can be measured by the following method. Measure the crystal diameter of the particles constituting the particles using an electron microscope. Observe 10 or more particles, measure the major axis and minor axis of each particle, and obtain the average value of the particle size.

[0080] The standard deviation of the average particle size of the particles may be, for example, 40 μm or less, or 30 μm or less, and may be 5 μm or more or 10 μm or more.

[0081] The average minor axis of the particles may be, for example, 80 μm or more, or 95 μm or more, and may be 150 μm or less, or 130 μm or less. The average major axis of the particles may be, for example, 75 μm or more, or 95 μm or more, and may be 200 μm or less, or 150 μm or less.

[0082] The ratio of the average major axis to the average minor axis of the particles 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 fluidity of the particles are better. The standard deviation of the ratio of the average major axis to the average minor axis of the particles may be 0.20 or less, or 0.12 or less, and may be 0.01 or more, since the particles are more easily dried, less likely to caking, and have better fluidity.

[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 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, and 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 may be 30.0 μm or less, 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 may be 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, for example, 3.1 or less, 2.8 or less, 2.5 or less, 2.2 or less, or 1.9 or less, and may be 0.5 or more, 1.0 or more, or 1.4 or more, since the stability and fluidity of the granules are better. 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, and may be more than 0.0, or 0.1 or more.

[0087] From the viewpoint that the effect of suppressing the formation of lumps (powdery state) and rapidly dispersing in the solution is more remarkable when the loose bulk density of the particles constituting the granules is returned to a solution containing a functional material using a solvent at normal temperature to low temperature (for example, water), for example, 0.700 (g / cm 3 ) or less, 0.600 (g / cm 3 ) or less, 0.500 (g / cm 3 ), or 0.400 (g / cm 3) may be as follows: 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 ) or more. The loose bulk density of the particles constituting the granules may be, for example, 0.393 (g / cm 3 ) to 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] From the viewpoint that the effect of suppressing the formation of lumps (powdery masses) and rapidly dispersing in the solution when returning to a solution containing the functional material using a solvent at normal temperature to low temperature (for example, water) is more prominent, the tapped bulk density of the particles constituting the granules may be, for example, 1.000 (g / cm 3 ) or less, 0.900 (g / cm 3 ) or less, 0.800 (g / cm 3 ), or 0.700 (g / cm 3 ) or less, and may be 0.300 (g / cm 3 ) or more, 0.400 (g / cm 3 ) or more, 0.500 (g / cm 3 ) or more, or 0.600 (g / cm 3 ) or more. The tapped bulk density of the particles constituting the granules may be, for example, 0.6979 (g / cm 3 ) to 0.704 (g / cm 3 ). The tapped bulk density of the particles constituting the granules can be measured by the method described in the examples below.

[0089] From the viewpoint that the effect of suppressing the formation of lumps (powdery masses) and rapidly dispersing in the solution when returning to a solution containing the functional material using a solvent at normal temperature to low temperature (for example, water) is more prominent, the dynamic bulk density of the particles constituting the granules may be, for example, 0.700 (g / cm 3 ) or less, 0.600 (g / cm 3 ) or less, or 0.500 (g / cm 3 ), and may be 0.200 (g / cm3 ) Above, 0.300 (g / cm 3 ) Above, 0.400 (g / cm 3 ) Above, or 0.500 (g / cm 3 ) Above may be sufficient. The dynamic bulk density of the particles constituting the granules is, for example, 0.530 (g / cm 3 ) ~ 0.545 (g / cm 3 ) may be sufficient. The dynamic bulk density of the particles constituting the granules can be measured by the method described in the examples below.

[0090] Since the granules according to this embodiment have the above-described configuration, they are excellent in dispersibility in solvents at normal temperature to low temperature.

[0091] The granules according to one embodiment have a simple sedimentation index of 2. That is, 200 mL of water (4°C) was poured into a 200 mL beaker, and after 6 g of the granules according to this embodiment were added, while maintaining the temperature at 4°C, the state was observed at 1 minute, 5 minutes, and 10 minutes after the addition. Regardless of the time, the entire amount settled. 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, and specifically, it can be evaluated by the following method. 200 mL of water (4.0°C) was poured into a 200 mL beaker containing 6 g of granules, and the mixture was stirred with a magnetic stirrer (300 rpm) for 30 seconds. After the stirring was completed, the contents of the beaker were immediately poured onto a sieve with a mesh size of 1000 μm, and the weight of the contents remaining on the sieve was 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, for example, as materials to be added to foods, food additives, pharmaceuticals, cosmetics, quasi-drugs, animal feeds, fertilizers, fragrances, antibiotics, soil conditioners, and the like.

Examples

[0094] Hereinafter, the present invention will be described more specifically with reference to examples. However, the present invention is not limited to the following examples.

[0095] 〔Test method〕 In each of the following test examples, common procedures and the like will be described first.

[0096] <Optical microscope observation> The spray liquid was dropped onto a slide glass, covered with a cover glass, and observed with 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, centrifuged at 16,000 rpm for 3 minutes using a centrifuge (Sakuma Seisakusho Co., Ltd., M150IV), and the residual crystal mass when the supernatant was removed and the mass of the spray liquid were calculated by applying them to the following formula. Crystallization rate (mass %) = Residual crystal mass (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 (Okawara Chemical Machinery Co., Ltd., OC-16 (dry type)) · Spray liquid supply device: Mono pump (Heishin Sobi Co., Ltd., 3NTL08PUL) · Spray method: Atomizer disk method The settings of the spray dryer are as follows. · Hot air inlet temperature setting: 30°C · Blower frequency setting: 60.0 Hz · Exhaust fan frequency setting: 37.0 Hz · Static pressure inside the tower setting: Slightly negative pressure to slightly positive pressure (MPa) · Atomizer disk frequency setting: 60 Hz · Pump frequency setting: 11.0 Hz · Raw material temperature setting: Not set (room temperature)

[0099] <Measurement of spray liquid supply rate> The liquid delivery tube connected to the spray dryer was removed and placed in a 100 mL graduated cylinder, and the spray liquid was supplied. The spray liquid flowing out from the liquid delivery tube was collected in the graduated cylinder for 60 seconds, and the spray liquid supply rate (mL / min) was measured.

[0100] <Measurement of moisture content of dry powder (loss on drying method)> 10 g of the recovered dry powder was weighed, and the moisture content was measured using an infrared moisture meter (Kett Science Laboratory Co., Ltd.) under the conditions of 105 °C for 15 minutes.

[0101] <Measurement of moisture content of dry powder (water activity method)> The water activity (Aw) was measured using 5 g or 10 mL of the dry powder with a water activity measuring device (METER, Dew Point water activity Meter AquaLAb Series4TE).

[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-Tech Corporation, MiniscopeTM3030).

[0103] <Evaluation of fluidity of dry powder> For the dry powders of the examples and comparative examples, the "flowability index" proposed by R.L. Carr was calculated. (Carr, R.L. "Evaluating flow properties of solids." Chem. Eng. (1965) 72 (163 - 168)). Using a multifunctional powder physical property measuring instrument (Seishin Enterprise Co., Ltd., Multi - tester MT - 02), the angle of repose (°), spatula angle (°), compressibility (%) and homogeneity (-) of the dry powder were determined, and based on Carr's theory, the index corresponding to each measured value was obtained. By summing up the indices of each measured value, the flowability index was obtained. The temperature and humidity during the measurement were 25°C and 50%. Next, the fluidity of the granules was evaluated based on the following Carr's evaluation criteria. Evaluation criteria for fluidity Flowability index value Degree of fluidity 90 - 100 Best 80 - 89 Good 70 - 79 Quite good 60 - 69 Normal 40 - 59 Not very good 0 - 19 Very poor

[0104] <Evaluation of the bulk density of the dry powder> For the dry powders of the examples and comparative examples, the bulk density (loose bulk density, tapped bulk density, dynamic bulk density) was determined using a multifunctional powder physical property measuring instrument (Seishin Enterprise Co., Ltd., Multi - tester MT - 02).

[0105] <Evaluation of the cold water dispersibility of the dry powder> For the dry powders of the examples and comparative examples, the cold water dispersibility (simple sedimentation index, dispersibility index) was evaluated according to the method described in International Publication No. WO 2020 / 095663.

[0106] (Evaluation of the simple sedimentation index) 200 mL of water (at 4 °C) was poured into a 200 mL beaker. After adding 6 g of dry powder, the state of the powder was observed while maintaining it in a refrigerator at 4 °C. The time elapsed since the addition was measured with a stopwatch, and the degree to which the powder on the liquid surface of the cold water settled in the water was evaluated at the 1-minute, 5-minute, and 10-minute time points based on the following simple sedimentation index. Simple sedimentation index 2: Regardless of time, the entire amount settles. 1: Approximately half of the amount sinks, but the entire amount does not settle. 0: It does not settle at all.

[0107] (Evaluation of dispersibility index) 200 mL of water (at 4.0 °C) was poured into a 200 mL beaker containing 6 g of dry powder, and it was stirred with a magnetic stirrer (300 rpm) for 30 seconds. After the stirring ended, the contents of the beaker were immediately poured onto a sieve with a mesh size of 1000 μm, 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 material] (Preparation of spray liquid) 4000 g of frozen whole eggs (Kewpie Corporation, frozen whole eggs (for confectionery)) was thawed by maintaining it at room temperature of 25 °C overnight to obtain 4000 g of whole egg liquid. After transferring the obtained 4000 g of whole egg liquid to a 10 L volume stainless steel pot, 4000 g of trehalose (Hayashibara Co., Ltd., Treha fine powder) was gradually added while stirring at 350 rpm using a stirrer (Shinto Corporation, Three One Motor, BL-1200) to obtain 8000 g of trehalose-containing whole egg liquid in total. This was used as the spray liquid.

[0109] Optical microscope observation and measurement of the crystallization rate were performed on the obtained spray liquid, and it was confirmed that a part of the trehalose was contained in a crystalline state. An example of the optical microscope image (magnification 500 times) of the spray liquid is shown in Figure 1. The spray liquid obtained above contained trehalose crystals with a particle size of 20 - 80 μm. Also, the crystallization rate of the spray liquid obtained above was 40%. From these facts, it was confirmed that the obtained spray liquid contained trehalose in a crystalline state.

[0110] (Spray drying) Using the entire amount of the obtained spray liquid, spray drying was carried out for 90 minutes under the following conditions using a spray dryer. ·Ambient temperature: 34.3 °C ·Ambient humidity: 54.5% RH ·Temperature of the spray liquid: 29.0 °C ·Inlet temperature: 35.0 °C ·Outlet temperature: 29.7 °C ·Supply rate of the spray liquid: 68 mL / min ·Atomizer rotation speed: 25500 rpm ·Air volume of the blower: 60 Hz ·Air volume of the exhaust: 38 Hz ·Temperature of the dried product: 29.0 °C After the spraying was completed, without changing the operating conditions of the spray dryer, the drying air was continuously sent for 30 minutes as it was to dry the inside of the dryer. Then, the dried powder was scraped off and collected. The obtained dried powder was used as the dried powder of Example 1-1.

[0111] (Evaluation of the dried powder) The dried powder of Example 1-1 was evaluated. As comparative subjects, dried egg white (Kewpie Corporation) (Comparative Example 1-1) and dried whole egg No. 1 (Kewpie Corporation) (Comparative Example 1-2) were used to conduct the same evaluation.

[0112] Regarding the dried powder of Example 1-1, the moisture content was confirmed by the moisture activity method and the loss on drying method. The moisture activity (Aw) measured by the moisture activity method was 0.6244. The moisture content measured by the loss on drying method was 9.80%.

[0113] Regarding the dried powder of Example 1-1, electron microscope observation was carried out. Fig. 2 shows an example of the electron microscope image of the dried powder of Example 1-1. Fig. 2(A) is an electron microscope image at a magnification of 1000 times, and Fig. 2(B) is an electron microscope image at a magnification of 500 times. As shown in Fig. 2, it was confirmed that the dried powder of Example 1-1 is granules wrapped in trehalose crystals.

[0114] The cold water dispersibility of the dry powders of Example 1-1 and Comparative Examples 1-1 to 1-2 was evaluated. Table 1 shows the evaluation results of the simple sedimentation index and the dispersibility index. [Table 1]

[0115] As a result of the evaluation of the simple sedimentation index, all of the dry powder of Example 1-1 immediately settled, while 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 had a small amount of lumps (remaining powder) formed and a small amount of content remaining on the sieve, while the dry powders of Comparative Examples 1-1 and 1-2 had a large amount of lumps (remaining powder) formed and a large amount of content remaining on the sieve. As is clear from these results, the dry powder of Example 1-1 was excellent in dispersibility in cold water.

[0116] The fluidity of the dry powders of Example 1-1 and Comparative Examples 1-1 to 1-2 was evaluated. Table 2 shows the evaluation results of the fluidity. [Table 2]

[0117] The bulk density of the dry powders of Example 1-1 and Comparative Examples 1-1 to 1-2 was evaluated. Table 3 shows the evaluation results of the bulk density. [Table 3]

[0118] 〔Test Example 2: Production and Evaluation of Granules Using Coffee Creamer as a Functional Material〕 (Preparation of Spray Liquid) The liquid coffee creamer (Ajinomoto AGF Inc., Marie) was opened and transferred to a 10 L stainless pot, and 2500 g of the liquid coffee creamer was collected. While stirring at 350 rpm using a stirrer (Shinto Co., Ltd., Three One Motor, BL-1200), 2500 g of lactose (Shoei Food Industry Co., Ltd., Ala, 100 mesh ON) was gradually added to obtain 5000 g of lactose-containing coffee creamer in total. This was used as the spray liquid.

[0119] Optical microscope observation and measurement of the crystallization rate were performed on the obtained spray liquid, and it was confirmed that a part of the lactose was contained in a crystalline state. Fig. 3 shows an example of an optical microscope image (magnification 500 times) of the spray liquid. The spray liquid obtained above contained lactose crystals with a particle size of 20 to 80 μm. Also, the crystallization rate of the spray liquid obtained above was 40%. From these facts, it was confirmed that the obtained spray liquid contained lactose in a crystalline state.

[0120] (Spray drying) Using the entire amount of the obtained spray liquid, spray drying was carried out 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: 25500 rpm · Blower air volume: 60 Hz · Exhaust air volume: 38 Hz · Dry product temperature: 29.0 °C After the spraying was completed, without changing the operating conditions of the spray dryer, drying air was continuously sent for 30 minutes as it was to dry the inside of the dryer. Then, the dried powder was scraped off and collected. The obtained dried powder was used as the dried powder of Example 2-1.

[0121] (Evaluation of dried powder) The dry powder of Example 2-1 was evaluated. As comparative objects, the same evaluation was carried out using a creaming powder (Nestle Japan Ltd., Bright) (Comparative Example 2-1), a powder cream (Morinaga Milk Industry Co., Ltd., Creap) (Comparative Example 2-2), and a powdered oil and fat (Nisshin Oillio Group Ltd., Nisshin MCT Powder) (Comparative Example 2-3).

[0122] Regarding the dry powder of Example 2-1, the moisture content 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] Regarding the dry powder of Example 2-1, electron microscope observation was carried out. An example of the electron microscope image of the dry powder of Example 2-1 is shown in Fig. 4. Fig. 4(A) is an electron microscope image at a magnification of 1000 times, and Fig. 4(B) is an electron microscope image at a magnification of 500 times. As shown in Fig. 4, it was confirmed that the dry powder of Example 2-1 was granules wrapped in lactose crystals.

[0124] Regarding the dry powders of Example 2-1 and Comparative Examples 2-1 to 2-3, evaluation of cold water dispersibility was carried out. The evaluation results of the simple sedimentation index and the dispersibility index are shown in Table 4.

Table 4

[0125] As a result of the evaluation of the simple sedimentation index, the dry powder of Example 2-1 immediately settled in full amount, 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 had a small amount of lumps (remaining powder) formed and a small amount of content remaining on the sieve, while the dry powders of Comparative Examples 2-1 to 2-3 had a large amount of lumps (remaining powder) formed and a large amount of content remaining on the sieve. As is clear from these results, the dry powder of Example 2-1 was excellent in dispersibility in cold water.

[0126] Regarding the dry powders of Example 2-1 and Comparative Examples 2-1 to 2-3, evaluation of fluidity was carried out. The evaluation results of fluidity are shown in Table 5.

Table 5

[0127] For the dry powders of Example 2-1 and Comparative Examples 2-1 to 2-3, the bulk density was evaluated. The evaluation results of the bulk density are shown in Table 6.

Table 6

Claims

1. A step of mixing at least one raw material selected from the group consisting of crystalline sugar and crystalline sugar alcohol with a functional material to obtain a spray liquid containing the raw material and the functional material and having a part of the raw material contained in a crystalline state; A step of spray-drying the spray liquid under low-temperature conditions, and a method for producing granules, wherein the functional material is a functional material having a high water content.

2. A step of mixing at least one raw material selected from the group consisting of crystalline sugar and crystalline sugar alcohol with a functional material to obtain a spray liquid containing the raw material and the functional material without using a solvent and having a part of the raw material contained in a crystalline state; A step of spray-drying the spray liquid under low-temperature conditions, and a method for producing granules.

3. The production method according to claim 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 claim 1 or 2, wherein the sugar and the sugar alcohol are monosaccharides, disaccharides, trisaccharides, and sugar alcohols thereof.

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 production method according to claim 1 or 2, wherein the spray-drying is performed under the condition that the inlet temperature is 0 to 60°C.

7. The production method according to claim 1 or 2, wherein the functional material is liquid egg, creamer, fruit juice, vegetable juice, or liquid milk material.

8. Granules containing at least one selected from the group consisting of crystalline sugar and crystalline sugar alcohol and a solid content of a functional material having a high water content, wherein the sugar and / or the sugar alcohol is partially in a crystalline state and partially in an amorphous state.

9. The granules according to claim 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 granules according to claim 8 or 9, wherein the sugar and the sugar alcohol are monosaccharides, disaccharides, trisaccharides, and sugar alcohols thereof.

11. The granules according to claim 8 or 9, wherein the sugar and the sugar alcohol are at least one selected from the group consisting of palatinose, sucrose, and trehalose.

12. ​ ​ The granule according to claim 8 or 9, wherein the functional material with a high water content is liquid egg, creamer, fruit juice, vegetable juice, or liquid milk material.

Images