Acid resistant powder, food product, chewable tablet and method for producing acid resistant powder

Abstract

To provide an acid resistant powder excellent in processing stability, acid resistance, pressure resistance, storage stability, and palatability.SOLUTION: An acid-resistant powder includes primary coating particles that encapsulate powder particles of a core material (A) as multiple nuclei and coated with a primary coating material (B) as a continuous phase, and secondary coating particles that have a structure coated with a secondary coating material (C) using the primary coating particles as a single nucleus, the core material (A) contains a powder (A1) with a bulk density of 0.2 to 0.7 that includes viable microbes, and an excipient (A2) with a bulk density of 0.7 to 1.0 and water activity of 0.30 or less, the primary coating material (B) contains lipids with a melting point of 40°C to 70°C, and the secondary coating material (C) contains lipids with a melting point of 40°C to 100°C, an average particle diameter of the primary coating particles ranges from 50 μm to 500 μm, and the ratio of the average particle diameter of the secondary coating particles to that of the primary coating particles is between 1.05 and 2.00.SELECTED DRAWING: Figure 2

Description

[Technical field]

[0001] The present invention relates to an acid-resistant powder, a food product, a chewable tablet, and a method for producing the acid-resistant powder, which include coated particles that contain a powder containing live bacteria as a core material. [Background technology]

[0002] Live bacteria such as bifidobacteria and lactic acid bacteria suppress the proliferation of bad bacteria in the intestines and improve the intestinal flora, thereby exerting beneficial effects on the host. In addition, the live bacteria have an intestinal regulating effect, such as improving constipation and diarrhea. In recent years, these live bacteria have been known as probiotics and are food ingredients used in medicines, foods for specified health uses, and health foods. However, these live bacteria cannot fully exert their effects unless they reach the intestinal tract after oral ingestion without being killed by gastric acid, bile acid, etc. In addition, they are vulnerable to physical shocks when processing medicines and foods, and are easily killed. Furthermore, when stored for a long period of time at room temperature, especially when stored for a long period of time in close proximity to raw materials with high water activity, the bacteria are easily killed, so they cannot fully exert their effects. Therefore, coatings have been invented to process and store bifidobacteria and lactic acid bacteria alive in foods.

[0003] A typical form of medicines and health foods is a solid preparation formed by compressing powder, which is called a tablet or tableted product. Other typical forms of medicines and health foods include soft capsules and hard capsules, but tableted products are easy to process and are widely used. Among tableted products, the demand for chewable tablets has been particularly high in recent years. This is a form in which the tablet is chewed in the mouth, enjoyed the taste, and then swallowed, and the active ingredients can be taken in the same way as with luxury foods, so there is a high demand from consumers. Conventional tableted products that are swallowed without chewing do not require consideration of texture such as roughness after chewing, and excipients with low water activity such as baked starch can be used. On the other hand, if baked starch is used in chewable tablets, the baked starch does not dissolve easily in saliva, so the active ingredients cannot be taken in the same way as with luxury foods. In addition, sugars such as glucose and maltitol, which are commonly used to improve texture, have high water activity, and high technology is required to compound active ingredients that deteriorate when coexisting with water.

[0004] For example, JP 2018-158947 A proposes a preparation containing live bacteria, particularly a solid preparation formed by tableting. This is a method for producing a solid preparation containing starch with a specific drying loss value, useful intestinal bacteria, and additives. This technology achieves a solid preparation with a high survival rate of bacteria after storage, but it cannot be used for tablet products that are chewed and tasted, such as chewable tablets, because it feels rough. [Prior art documents] [Patent documents]

[0005] [Patent Document 1] JP 2018-158947 A Summary of the Invention [Problem to be solved by the invention]

[0006] In light of this, there is a demand for reducing the death of live bacteria when powdered raw materials containing live bacteria such as lactic acid bacteria and bifidobacteria are processed into an acid-resistant powder (processing stability). Next, there is a demand for an acid-resistant powder that can suppress the death of live bacteria when they come into contact with gastric acid (acid resistance) so that the live bacteria can be delivered alive to the intestines after ingestion, that can reduce the death of live bacteria even when subjected to tableting pressure when the acid-resistant powder is compressed into a chewable tablet (pressure resistance), that can reduce the death of live bacteria when this chewable tablet is stored (storage stability), and that can be chewed and eaten without feeling rough (palatability).

[0007] An object of the present invention is to provide an acid-resistant powder that is excellent in processing stability, acid resistance, pressure resistance, storage stability, and palatability. [Means for solving the problem]

[0008] As a result of intensive research into solving the above problems, the present inventors have found that the above problems can be solved by primary coated particles having a specific average particle size, which contain a powder containing live bacteria and an excipient having a specific bulk density and water activity as multiple cores, and which are coated with a primary coating material containing a lipid with a specific melting point and have a specific average particle size, and these primary coated particles are coated with a secondary coating material containing a lipid with a specific melting point and have a specific average particle size, thereby completing the present invention. That is, the present invention is as follows: [1] to [6].

[0009] [1] An acid-resistant powder comprising primary coated particles in which powder particles of a core substance (A) are encapsulated as multiple nuclei and coated with a primary coating material (B) as a continuous phase, and secondary coated particles having a structure in which the primary coated particles are coated with a secondary coating material (C) as a single nucleus, The core material (A) comprises a powder (A1) containing live bacteria having a bulk density of 0.2 to 0.7 and an excipient (A2) having a bulk density of 0.7 to 1.0 and a water activity of 0.30 or less, The primary coating material (B) contains a lipid having a melting point of 40°C to 70°C, The secondary coating material (C) contains a lipid having a melting point of 40°C to 100°C, The average particle size of the primary coated particles is 50 μm to 500 μm, An acid-resistant powder, characterized in that the ratio of the average particle size of the secondary coated particles to the average particle size of the primary coated particles (average particle size of secondary coated particles / average particle size of primary coated particles) is 1.05 to 2.00. [2] a mass ratio of the core material (A) to a total mass of the core material (A) and the primary coating material (B) is 0.65 to 0.90; The acid-resistant powder according to [1], characterized in that a mass ratio of the primary coated particles (B) to a total mass of the primary coated particles and the secondary coating material (C) is preferably 0.60 to 0.85. [3] The acid-resistant powder according to [1] or [2], preferably having an average particle size of 50 μm to 500 μm. [4] A food product comprising the acid-resistant powder according to any one of [1] to [3]. [5] A chewable tablet comprising the acid-resistant powder according to any one of [1] to [3] and a water-soluble saccharide. [6] A method for producing an acid-resistant powder according to any one of [1] to [3], A step of mixing the core material (A) and the primary coating material (B) to obtain the primary coated particles; A method for producing an acid-resistant powder, which preferably comprises a step of mixing the primary coated particles with a powdery secondary coating material (C) to obtain the secondary coated particles. Effect of the Invention

[0010] According to the present invention, it is possible to provide an acid-resistant powder in which the death of live bacteria is reduced when a powdered raw material containing live bacteria is processed into an acid-resistant powder (processing stability), the death of live bacteria is inhibited when the powdered raw material comes into contact with gastric acid (acid resistance), there is little death even when the acid-resistant powder is subjected to tableting pressure when being compressed into a chewable tablet (pressure resistance), there is little death of live bacteria when the chewable tablet is stored (storage stability), and there is little sense of roughness when the chewable tablet is chewed and eaten (palatability). [Brief description of the drawings]

[0011] [Figure 1] FIG. 2 is a schematic explanatory diagram showing the structure of a primary coated particle constituting the acid-resistant powder of the present invention. [Diagram 2] FIG. 2 is a schematic explanatory diagram showing the structure of a secondary coated particle constituting the acid-resistant powder of the present invention. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0012] In this specification, when a preferred numerical range (e.g., mass %) is described stepwise, each lower limit and upper limit can be independently combined. For example, in the description "preferably 10 or more, more preferably 20 or more, and preferably 100 or less, more preferably 90 or less," "preferably lower limit: 10" and "more preferably upper limit: 90" can be combined to "10 or more and 90 or less."

[0013] [Acid-resistant powder] The acid-resistant powder of the present invention is an acid-resistant powder comprising primary coated particles encapsulating powder particles of a core substance (A) as multiple nuclei and coated with a primary coating material (B) as a continuous phase, and secondary coated particles having a structure in which the primary coated particles serve as single nuclei and are coated with a secondary coating material (C), characterized in that the core substance (A) comprises a powder (A1) containing live bacteria having a bulk density of 0.2 to 0.7 and an excipient (A2) having a bulk density of 0.7 to 1.0 and a water activity of 0.3 or less, the primary coating material (B) comprises a lipid having a melting point of 40°C to 70°C, the secondary coating material (C) comprises a lipid having a melting point of 40°C to 100°C, the average particle diameter of the primary coated particles is 50 μm to 500 μm, and the average particle diameter of the secondary coated particles relative to the average particle diameter of the primary coated particles (average particle diameter of secondary coated particles / average particle diameter of primary coated particles) is 1.05 to 2.0.

[0014] FIG. 1 shows a schematic diagram of the structure of a primary coated particle constituting the acid-resistant powder of the present invention, and FIG. 2 shows a schematic diagram of the structure of a secondary coated particle contained in the acid-resistant powder of the present invention. 1, primary coated particle 10 is a coated granule in which a core substance (A) is encapsulated as multiple nuclei inside a primary coating material (B) that is a continuous phase. Although not shown, the core substance (A) contains a powder (A1) containing live bacteria with a bulk density of 0.2 to 0.7 and an excipient (A2) with a bulk density of 0.7 to 1.0 and a water activity of 0.3 or less. 2, the secondary coated particles 20 have a structure in which the primary coated particles 10 serve as a single core and are coated with a particulate secondary coating material (C). By using the particulate secondary coating material (C), it is possible to produce secondary coated particles 20 having the primary coated particles 10 as a single core. The presence of a single primary coated particle 10 within the secondary coated particles 20 makes the secondary coated particles 20 less likely to crumble even when subjected to tableting pressure during processing into a chewable tablet, resulting in a live bacteria-containing powder from which chewable tablets with excellent processing stability, acid resistance, pressure resistance, storage stability, and palatability can be produced.

[0015] The average particle diameter of the primary coated particles 10 is 50 μm to 500 μm. The lower limit is preferably 100 μm or more. The upper limit is preferably 400 μm or less, more preferably 300 μm or less. When the average particle diameter is less than 50 μm, the surface area of ​​the primary coated particles becomes large and sufficient coating with the secondary coating material cannot be achieved, resulting in reduced coating performance and failure to obtain acid resistance and storage stability. When the average particle diameter exceeds 500 μm, the secondary coating material is easily peeled off and the coating state of the secondary coated particles deteriorates, resulting in failure to obtain processing stability, acid resistance, and storage stability.

[0016] The average particle diameter of the secondary coated particles 20 is not particularly limited, but is, for example, 50 μm to 500 μm. The lower limit is preferably 100 μm or more. The upper limit is preferably 400 μm or less, more preferably 300 μm or less. When the average particle diameter is less than 50 μm, the particle diameter of the primary coated particles is also less than 50 μm, and as described above, sufficient coating with the secondary coating material is not possible, the coating performance is reduced, and acid resistance and storage stability cannot be obtained. By setting the average particle diameter to 500 μm or less, the secondary coating material is less likely to peel off, and the coating state of the secondary coated particles is improved, so that processing stability, acid resistance, and storage stability can be obtained.

[0017] The ratio of the average particle size of the secondary coated particles 20 to the average particle size of the primary coated particles 10 (average particle size of the secondary coated particles / average particle size of the primary coated particles) is 1.05 to 2.00. The upper limit is preferably 1.60 or less, more preferably 1.40 or less. When this ratio exceeds 2.00, the amount of the secondary coating material is too much, and processing stability, acid resistance, pressure resistance, storage stability, and palatability cannot be obtained, and the content of useful components is reduced. When this ratio is less than 1.05, the secondary coating layer does not have a sufficient thickness or the primary coated particles are broken into small particles, so that processing stability, acid resistance, pressure resistance, storage stability, and palatability cannot be obtained.

[0018] In the primary coated particles, the mass ratio of the core substance (A) to the primary coating material (B) is not particularly limited, but for example, the mass ratio of the core substance (A) to the total mass of the core substance (A) and the primary coating material (B) is 0.65 to 0.90. The lower limit is preferably 0.70 or more, more preferably 0.75 or more. The upper limit is preferably 0.85 or less. When the mass ratio is 0.65 or more, the content of the core substance (A) can be increased. On the other hand, when the mass ratio is 0.90 or less, the content of the primary coating material (B) increases, the coating performance is improved, and the acid resistance, pressure resistance, and storage stability are improved.

[0019] In the primary coated particles, the mass ratio of the powder (A1) containing live bacteria with a bulk density of 0.2 to 0.7 and the excipient (A2) with a bulk density of 0.7 to 1.0 in the core material (A) is not particularly limited, but for example, when the mass of the powder (A1) containing live bacteria is taken as 1, the mass of the excipient (A2) is 0.2 to 0.8. The lower limit is preferably 0.3 or more, more preferably 0.4 or more. The upper limit is preferably 0.7 or less. When the mass ratio is 0.2 or more, there is an effect that the coating performance is improved, and the pressure resistance and storage stability are improved. Also, when it is 0.8 or less, the content of the powder (A1) containing live bacteria can be increased, and the palatability is also improved.

[0020] In the secondary coated particles, the mass ratio of the primary coated particles to the secondary coating material (C) is not particularly limited, but for example, the mass ratio of the primary coated particles (B) to the total mass of the primary coated particles and the secondary coating material (C) is 0.60 to 0.85. The lower limit is preferably 0.65 or more, more preferably 0.70 or more. The upper limit is preferably 0.80 or less. When the mass ratio is 0.60 or more, the content of the core substance (A) contained in the secondary coated particles can be increased. Also, when the mass ratio is 0.85 or less, the content of the secondary coating material (C) increases, which has the effect of improving the coating performance and improving the pressure resistance.

[0021] The processing stability of the acid-resistant powder of the present invention is, for example, such that the processing survival rate in the processing stability of the present invention is 70% or more, preferably 80% or more, and more preferably 90% or more.

[0022] The acid resistance of the acid-resistant powder of the present invention is, for example, such that the viable cell survival rate in the acid resistance test of the present invention is 10% or more, preferably 20% or more, more preferably 30% or more, even more preferably 32% or more, and most preferably 35% or more.

[0023] The pressure resistance of the acid-resistant powder of the present invention is, for example, such that the viable cell survival rate in the pressure resistance test of the present invention is 75% or more, preferably 85% or more, and more preferably 95% or more.

[0024] The storage stability of the acid-resistant powder of the present invention is, for example, such that the viable cell survival rate in the storage stability test of the present invention is 50% or more, preferably 60% or more, and more preferably 70% or more.

[0025] The oil content of the acid-resistant powder of the present invention is not particularly limited, but is, for example, 20 to 70% by mass or more. The lower limit is preferably 30% by mass or more, more preferably 35% by mass or more. The upper limit is preferably 60% by mass or less, more preferably 50% by mass or less, and even more preferably 45% by mass or less. The oil content is measured according to the "ether extraction method". When the oil content is 20% by mass or more, the water repellency of the acid-resistant powder is high, and therefore, the storage stability is excellent. When the oil content is 70% by mass or less, the content of live bacteria can be increased.

[0026] Each component of the present invention will be described in detail below. [Powder containing live bacteria (A1)] The powder (A1) containing live bacteria of the core material (A) of the present invention is not particularly limited as long as it is a powder containing live bacteria. Examples of live bacteria include bifidobacteria and lactic acid bacteria.

[0027] The powder (A1) containing the live bacteria of the core material (A) has a bulk density of 0.2 to 0.7. It is preferably 0.3 or more, more preferably 0.4 or more, and most preferably 0.5 or more. If the bulk density is less than 0.2, the chewable tablet made using the live bacteria-containing powder of the present invention does not have palatability or storage stability. If the bulk density is more than 0.7, the chewable tablet made using the live bacteria-containing powder of the present invention can have palatability and storage stability even without applying the present invention. The average particle size of the powder (A1) containing the live bacteria of the present invention is not particularly limited as long as it is within the range in which the effects of the present invention can be obtained, and is, for example, 10 to 200 μm. The upper limit is preferably 150 μm or less, more preferably 100 μm or less, and even more preferably 80 μm or less. If the average particle size of the core material (A) is small, there is an advantage that the size of the primary coated particles can be easily adjusted.

[0028] [Excipient (A2)] The excipient (A2) of the core substance (A) of the present invention has a bulk density of 0.7 to 1.0, preferably 0.7 to 0.9, and more preferably 0.75 to 0.85. If the bulk density is less than 0.7 and more than 1.0, storage stability cannot be obtained.

[0029] The excipient (A2) of the core substance (A) of the present invention is not particularly limited as long as it is within the range in which the effects of the present invention can be achieved, but the average particle size is preferably 20 μm to 100 μm. More preferably, it is 30 μm to 100 μm, and most preferably, it is 40 μm to 70 μm. By making it 20 μm or more, the coating performance is improved and the pressure resistance and storage stability are improved. By making it 100 μm or less, the coating performance is improved and the storage stability is improved.

[0030] The excipient (A2) of the core substance (A) of the present invention has a water activity of 0 to 0.30. It is preferably 0.20 or less, more preferably 0.15 or less, and most preferably 0.10 or less. If it is more than 0.3, the target storage stability cannot be obtained.

[0031] Examples of the excipient (A2) for the core substance (A) of the present invention include powders of lactose, starch, calcined starch, sucrose, maltitol, sorbitol, dextrin, trehalose, crystalline cellulose, etc., but other substances whose particle size, bulk density, water activity have been adjusted by processing such as pulverization or granulation, sieving or classification, calcined or dried may also be used. Of these, calcined starch is the most preferred. The powder (A1) containing the live bacteria of the present invention has a bulk density of 0.2 to 0.7 and is lighter than the excipient (A2), while the excipient (A2) of the present invention has a bulk density of 0.7 to 1.0 and is heavier than the powder (A1) containing the live bacteria. If the core material (A) of the present invention is only the powder (A1) containing the live bacteria, the particle size of the primary coated particles will vary, the efficiency of the secondary coating will decrease, and the coating performance of the secondary coated particles will not reach the target, and the chewable tablet made using the live bacteria-containing powder of the present invention will not have palatability or storage stability. However, by primary coating the powder (A1) containing the live bacteria of the present invention together with the excipient (A2), that is, a powder that is heavier than the powder (A1) containing the live bacteria with a bulk density of 0.7 to 1.0, the particle size of the primary coated particles can be made uniform, the efficiency of the secondary coating will be improved, and the coating performance of the secondary coated particles will be good, and the chewable tablet made using the live bacteria-containing powder of the present invention can have storage stability. One of the possible factors that may cause the chewable tablet to have poor texture (palatability) when chewed, which is the subject of the present invention, is the excipient (A2) as the core material (A). The excipient (A2) of the present invention has a bulk density of 0.7 to 1.0 and a water activity of 0.30 or less, but an excipient with such properties causes roughness, that is, a powdery feeling in the mouth when chewing the chewable tablet. By incorporating this excipient (A2) into the secondary coated particles, the powdery feeling in the mouth when chewing the chewable tablet can be eliminated, so that palatability can be obtained. The second possible factor is the excipient as a raw material other than the secondary coated particles to be mixed into the chewable tablet. In order to improve the storage stability of the live bacteria contained in the chewable tablet, an excipient with low water activity is desirable, but many of these excipients cause a powdery feeling in the mouth when chewing the chewable tablet. On the other hand, many excipients that do not feel powdery have high water activity, so if such excipients are used as raw materials for chewable tablets without using the secondary coated particles of the present invention, the live bacteria will come into direct contact with the excipient with high water activity, and storage stability will not be obtained. However, by coating the live bacteria with the secondary coated particles, the live bacteria will not come into direct contact with the excipient with high water activity, and storage stability will be obtained.

[0032] [Primary covering material (B)] The primary coating material (B) of the present invention contains an edible lipid having a melting point of 40° C. to 70° C. The lower limit of the melting point of the lipid in the primary coating material (B) is preferably 50° C. or higher, more preferably 55° C. or higher. When the melting point of the lipid in the primary coating material (B) is 40° C. or higher, the coating performance is improved, and pressure resistance and storage stability are excellent. On the other hand, when the melting point of the lipid in the primary coating material (B) is 70° C. or lower, the primary coating material (B) can be softened without exposing the core substance (A) to high temperatures during the formation of the primary coated particles.

[0033] The lipid of the primary covering material (B) may be any lipid having a melting point of 40° C. to 70° C., and examples thereof include fatty acid esters, higher alcohols, and waxes, and one or more of these may be used. Examples of fatty acid esters include triglycerides, which are typical edible fats and oils, and have a structure in which three molecules of fatty acid are ester-bonded to glycerin, and originate from, for example, soybean oil, rapeseed oil, cottonseed oil, rice oil, corn oil, sesame oil, peanut oil, sunflower oil, safflower oil, camellia oil, olive oil, coconut oil, palm oil, palm kernel oil, cacao butter, perilla oil, perilla oil, lard, beef tallow, chicken oil, whale oil, and fish oil. The melting point is adjusted by transesterification, hydrogenation, or the like. Other fatty acid esters include so-called emulsifiers, such as glycerin fatty acid esters, sorbitan fatty acid esters, propylene glycol fatty acid esters, sucrose fatty acid esters, and lecithin. Examples of higher alcohols include linear or branched alcohols having 20 to 36 carbon atoms. Specific examples include eicosanol (20 carbon atoms), docosanol (26 carbon atoms), octacosanol (28 carbon atoms), triacontanol (=myricyl alcohol, 30 carbon atoms), and hexatriacontanol (36 carbon atoms). Examples of waxes include carnauba wax, candelilla wax, and rice wax. Of these, triglycerides are most preferred.

[0034] The lipid of the primary coating material (B) may be in powder form or in liquid form melted by heating. When using a lipid of the powdered primary coating material (B), primary coated particles can be formed quickly and easily by spraying the liquid primary coating material (B) onto the mixed core substance (A).

[0035] [Secondary covering material (C)] The secondary coating material (C) of the present invention contains an edible lipid having a melting point of 40°C to 100°C. The lower limit of the melting point of the lipid of the secondary coating material (C) is preferably 50°C or higher, more preferably 55°C or higher, and even more preferably 60°C or higher. On the other hand, the upper limit of the melting point of the lipid of the secondary coating material (C) is preferably 90°C or lower, more preferably 80°C or lower, and even more preferably 75°C or lower. When the melting point of the lipid of the secondary coating material (C) is high, the secondary coating materials (C) are less likely to adhere to each other when the primary coating particles and the secondary coating material (C) are mixed, and are more likely to be arranged on the surfaces of the primary coating particles. On the other hand, when the melting point of the lipid of the secondary coating material (C) is lowered, the primary coating particles collide with each other when the primary coating particles and the secondary coating material (C) are mixed, so that the secondary coating material (C) arranged on the surfaces of the primary coating particles spreads, thereby improving the coating performance.

[0036] The lipid of the secondary coating material (C) may be any lipid having a melting point of 40° C. to 100° C., and examples thereof include fatty acid esters, higher alcohols, and waxes, and one or more of these may be used. Examples of fatty acid esters include triglycerides, which are typical edible fats and oils, and have a structure in which three molecules of fatty acid are ester-bonded to glycerin, and originate from, for example, soybean oil, rapeseed oil, cottonseed oil, rice oil, corn oil, sesame oil, peanut oil, sunflower oil, safflower oil, camellia oil, olive oil, coconut oil, palm oil, palm kernel oil, cacao butter, perilla oil, perilla oil, lard, beef tallow, chicken oil, whale oil, and fish oil. The melting point is adjusted by transesterification, hydrogenation, or the like. Other fatty acid esters include so-called emulsifiers, such as glycerin fatty acid esters, sorbitan fatty acid esters, propylene glycol fatty acid esters, sucrose fatty acid esters, and lecithin. Examples of higher alcohols include linear or branched alcohols having 20 to 36 carbon atoms. Specific examples include eicosanol (20 carbon atoms), docosanol (26 carbon atoms), octacosanol (28 carbon atoms), triacontanol (=myricyl alcohol, 30 carbon atoms), and hexatriacontanol (36 carbon atoms). Examples of waxes include carnauba wax, candelilla wax, and rice wax. Of these, triglycerides are most preferred.

[0037] The lipid of the secondary coating material (C) is in powder form. By using the lipid of the powdered secondary coating material (C), the secondary coating material (C) adheres to the surface of the primary coated particle, and a secondary coated particle having the primary coated particle as a single nucleus can be formed. If the lipid of the secondary coating material (C) in liquid form is used, the secondary coating material (C) becomes a coated granule containing the primary coated particles as multiple nuclei with the secondary coating material (C) as a continuous phase, and the effect of the present invention cannot be obtained.

[0038] The average particle size of the lipid in the secondary coating material (C) is, for example, 5 to 100 μm. The upper limit is preferably 80 μm or less, more preferably 60 μm or less, and further preferably 40 μm or less. When the average particle size of the lipid in the secondary coating material (C) is small, the secondary coating material (C) is densely arranged on the surface of the primary coating particles, thereby improving the coating performance.

[0039] [Processing method (manufacturing method)] The method for producing an acid-resistant powder containing secondary coated particles of the present invention includes, for example, a step of mixing the core material (A) and the primary coating material (B) to obtain the primary coated particles, and a step of mixing the primary coated particles and a powdery secondary coating material (C) to obtain the secondary coated particles. More specifically, a powder (A1) containing live bacteria as the core material (A) and an excipient (A2) are put into a stirring layer, and the lipid of the primary coating material (B) is melted at a temperature higher than the melting point and prepared as a liquid. Then, while mixing and stirring the core material (A), the liquid primary coating material (B) is sprayed into the stirring layer. At this time, the temperature of the primary coating material (B) drops below the melting point and solidifies, so that the powder (A1) containing live bacteria as multiple core materials (A) and the excipient (A2) are both bound to the primary coating material (B) and granulated, and primary coated. Next, the lipid of the secondary coating material (C) is added to the primary coated particles in the stirring layer and put in, and secondary coating is performed by stirring at high speed. At this time, the lipid powder collides with the lipid of the primary coating material (B) on the surface of the primary coated particle and adheres to it, and by repeating this process, a secondary coating layer is formed, completing the secondary coated particle. The secondary coating is preferably performed at a temperature lower than the melting point of the lipid of the secondary coating material (C). Under these conditions, the primary coated particles and the secondary coating material are stirred at high speed to cause the powder particles to collide with each other, and the lipid of the secondary coating material is layered around the primary coated particles, forming a coating.

[0040] [Chewable tablets] The food containing the secondary coated particles of the present invention can be used in a wide range of applications, but chewable tablets are preferred due to their effectiveness. Chewable tablets can contain excipients, lubricants, flow agents, sweeteners, flavor powders, and fruit juice powders in addition to the secondary coated particles of the present invention. The excipients are preferably water-soluble carbohydrates in order to reduce the roughness of the chewable tablets, and examples of such excipients include glucose, fructose, sucrose, lactose, maltose, trehalose, isomaltulose, isomaltulose (palatinose), oligosaccharides (galactooligosaccharides, fructooligosaccharides), starch hydrolysates (dextrin, maltodextrin), erythritol, xylitol, sorbitol, reduced isomaltulose, and maltitol (reduced maltose). Among these, glucose, maltose, isomaltulose (palatinose), maltodextrin, erythritol, reduced isomaltulose, and maltitol are preferred, with maltose and maltitol being the most preferred. EXAMPLES

[0041] The present invention will be described in more detail below with reference to examples and comparative examples, but the present invention is not limited thereto.

[0042] (Examples 1 to 19, Comparative Examples 1 to 11) Acid-resistant powders were prepared according to the following methods for preparing primary coated particles and secondary coated particles. The obtained acid-resistant powders were evaluated for "survival rate of live bacteria after processing" (processing stability), "survival rate of live bacteria after acid resistance test" (acid resistance), "survival rate of live bacteria after tableting" (pressure resistance), "storage stability of live bacteria in chewable tablets" (storage stability), and "roughness by sensory evaluation" (preference), and the evaluation results are shown in Tables 1, 2, and 3.

[0043] (About ingredients) The raw materials used in the examples are as follows. In the present invention, the average particle size is measured using a laser diffraction particle size distribution analyzer "SALD-2100" (manufactured by Shimadzu Corporation). The melting point in the present invention is measured in accordance with the Standard Methods for the Analysis of Fats, Oils and Related Materials, "2.2.4.2 Melting Point (Slip Melting Point)." The bulk density in the present invention is defined as the loose bulk density (g / cm 3 ) and is calculated by pouring an excess of sample into a 100 mL cylindrical container until it overflows, and then measuring the mass of the powder when the excess powder is scraped off from the top of the container. In the present invention, the water activity is measured using a water activity measuring device "HygroLab" (manufactured by Rotronic).

[0044] <Powder (A1) containing live bacteria of the core substance (A)> Bifidobacteria A: "Bifidobacteria Powder BB536" (Morinaga Milk Industry Co., Ltd.), average particle size 29.0 μm, bulk density 0.64 Bifidobacteria B: "Bifidobacteria Powder M63" (Morinaga Milk Industry Co., Ltd.), average particle size 26.0 μm, bulk density 0.62 Lactic acid bacteria A: average particle size 32.1 μm, bulk density 0.45

[0045] <Excipient (A2) for core substance (A)> ST Starch P: Calcined starch (manufactured by Nippon Starch Chemical Co., Ltd.), average particle size 42.1 μm, bulk density 0.83, water activity 0.002 or less (below detection limit) Ceolas ST-100: Crystalline cellulose (manufactured by Asahi Kasei Corporation), average particle size 81.6 μm, bulk density 0.20, water activity 0.26 Ceolas UF-F711: Crystalline cellulose (manufactured by Asahi Kasei Corporation), average particle size 88.0 μm, bulk density 0.26, water activity 0.40

[0046] <Primary covering material (B)> Hardened rapeseed oil: (NOF Corp.), melting point 67°C Hardened palm oil: (NOF Corp.), melting point 57°C Hardened rapeseed oil 1: (NOF Corp.), melting point 50°C Hardened palm oil: (NOF Corp.), melting point 42°C Carnauba wax: (manufactured by Toa Kasei Co., Ltd.), melting point 86°C

[0047] <Secondary coating material (C)> The lipids described below were powdered by spray cooling or pulverization, and then subjected to secondary pulverization until the average particle size became 50 μm or less, to prepare secondary coating materials. Hardened rapeseed oil: (NOF Corp.), melting point 67°C, average particle size 6.8μm Hardened palm oil: (NOF Corporation), melting point 57°C, average particle size 14.6μm Glycerol fatty acid ester: (manufactured by Danisco Japan Co., Ltd.), melting point 62°C, average particle size 18.2 μm Hardened palm oil: (NOF Corporation), melting point 42°C, average particle size 42.5μm Rice wax: (manufactured by Toa Kasei Co., Ltd.), melting point 78°C, average particle size 14.5 μm Hardened rapeseed oil 2: (NOF Corp.), melting point 36°C, average particle size 40.4μm

[0048] (Regarding the production of acid-resistant powder) The primary coated particles and secondary coated particles constituting the acid-resistant powders of the Examples and Comparative Examples were prepared as follows. [Preparation method of primary coated particles] In Example 1, 200 g of powder (A1) "Bifidobacterium BB536" containing live bacteria as the core material (A) and 100 g of excipient (A2) "ST Starch P" were placed in a high-speed stirring mixer. While stirring the high-speed stirring mixer, the primary coating material (B) of extremely hardened rapeseed oil was adjusted to its melting point +10°C and melted, and 75 g of this was sprayed inside the high-speed stirring mixer to coat the core material (A) with the primary coating material (B). Next, the product was cooled to a product temperature of 20°C in the high-speed stirring mixer to obtain the primary coated particles of Example 1.

[0049] [Preparation method of secondary coated particles] 75 g of rapeseed hardened oil, which is the secondary coating material (C), was added to the primary coated particles of Example 1 in a high-speed stirring mixer. Stirring and mixing were performed with the jacket temperature of the high-speed stirring mixer cooled, and the secondary coating material was attached to the surface of the primary coated particles in a powder state. By continuing to stir and mix further, the powder of the secondary coating material was evenly distributed on the surface of the primary coated particles, and the secondary coated particles of Example 1 were prepared.

[0050] In Examples 2 to 19 and Comparative Examples 1 to 11, the primary coated particles and secondary coated particles were prepared according to the formulations in Tables 1 to 3. Moreover, Examples 2 to 10, 13 to 19 and Comparative Examples 3 to 4, 8 to 9, and 11 were prepared under the same production conditions as Example 1.

[0051] Example 11 was prepared by increasing the stirring speed and slowing the spraying speed of the primary coating material (B) when preparing the primary coated particles so that the particle diameter of the primary coated particles would be small. Example 12 was prepared by decreasing the stirring speed and speeding up the spraying speed of the primary coating material (B) when preparing the primary coated particles so that the particle diameter of the primary coated particles would be large. Comparative Example 1 was performed only with the primary coating material (C) without secondary coating. Comparative Example 2 was performed only with secondary coating as in Example 1 without primary coating the core material (A). Comparative Example 5 was prepared by increasing the stirring speed and slowing the spraying speed of the primary coating material (B) when preparing the primary coated particles so that the particle diameter of the primary coated particles would be small. Comparative Example 6 was prepared by decreasing the stirring speed and speeding up the spraying speed of the primary coating material (B) when preparing the primary coated particles so that the particle diameter of the primary coated particles would be large. In Comparative Example 7, the secondary coated particles were prepared by heating and melting the secondary coating material (C) at a melting point of +10°C and spraying it onto the primary coated particles. In Comparative Example 10, the powder (A1) itself containing live bacteria was evaluated. The rest of the evaluation was performed under the same manufacturing conditions as in Example 1. The secondary coated particles thus obtained were used as acid-resistant powder and were evaluated.

[0052] (Evaluation method for acid-resistant powder) <Method for measuring live bacteria> In the method for measuring the viable bacteria of the present invention, 100 mg of a specimen was added to 100 mL of physiological saline and homogenized to extract the viable bacteria. This solution was appropriately diluted, and 1 mL of the diluted solution was mixed with 20 mL of BL agar medium (manufactured by Nissui Pharmaceutical Co., Ltd.) and subjected to anaerobic culture (37°C, 72 hours). After the culture was completed, the number of viable bacteria per 1 g of specimen was calculated from the number of colonies that grew on the medium.

[0053] <Processing stability: survival rate of live bacteria after processing (survival rate after processing)> The survival rate of live bacteria after processing was calculated using the following formula and evaluated according to the following criteria. Viable bacteria count before processing: The viable bacteria count of the powder containing viable bacteria as the raw material is measured and multiplied by the blending ratio. Viable bacteria count after processing: Viable bacteria count of secondary coated particles produced by processing Processing survival rate (%) = Number of viable bacteria after processing / Number of viable bacteria before processing × 100 [Standards for processing survival rate] ◎: 90% or more, 〇: less than 90%, 80% or more, △: less than 80%, 70% or more, ×: less than 70%

[0054] <Vitamin survival rate after acid resistance test (acid resistance survival rate)> (Acid resistance test) In the present invention, the acid resistance evaluation is carried out by placing 100 mL of a hydrochloric acid aqueous solution of pH 3.0 in a 200 mL capacity beaker and adjusting the temperature to 37°C. Next, 100 mg of secondary coated particles are added and stirred for 1 hour at 100 rpm with a magnetic stirrer. After stirring is completed, the mixture is neutralized with a sodium hydroxide aqueous solution of pH 13 and the viable cell count is measured. When calculating the viable cell count, the amount of the sodium hydroxide aqueous solution added is corrected. Acid resistance survival rate (%) = number of viable bacteria after acid resistance test / number of viable bacteria before acid resistance test × 100 [Acid resistance survival rate standard] ◎: 30% or more, 〇: less than 30%, 20% or more, △: less than 20%, 10% or more, ×: less than 10%

[0055] <Pressure resistance: Viable bacteria survival rate after tableting (survival rate after tableting)> (Pressure resistance test) In the present invention, the pressure resistance evaluation was carried out by preparing tablets (chewable tablets) containing acid-resistant powders with the following formulation and compression conditions, and measuring the number of viable bacteria before and after compression. The measurement of viable bacteria in the tablets was carried out by grinding the tablets in a mortar to obtain a powder, which was used as a sample for the viable bacteria measurement method. The maltitol used was "Amalty MR-50" (manufactured by Mitsubishi Corporation Life Sciences Co., Ltd.), the calcined starch used was "ST Starch P" (manufactured by Nippon Starch Chemical Co., Ltd.), the silicon dioxide used was "Silopage 720" (manufactured by Fuji Silysia Chemical Co., Ltd.), and the calcium stearate used was "Calcium stearate (vegetable)" (manufactured by Taihei Chemical Industry Co., Ltd.). The pressure resistance of the viable bacteria was evaluated by the following formula. Tablet survival rate (%) = Number of viable bacteria after tableting / Number of viable bacteria before tableting × 100 [Tablet survival rate criteria] ◎: 95% or more, 〇: less than 95%, 85% or more, △: less than 85%, 75% or more, ×: less than 75% [Tablet composition] Acid-resistant powder of the examples or comparative examples 20% by mass Maltitol 67% by weight Silicon dioxide 1% by mass Calcium stearate 2% by weight Flavor materials (flavoring, acidulant, sweetener) 10% by mass Total 100% by mass

[0056] However, Comparative Example 11 was carried out with the following composition. Acid-resistant powder of Comparative Example 11 16% by mass Calcined starch "ST Starch P" 4% by mass Maltitol 67% by weight Silicon dioxide 1% by mass Calcium stearate 2% by weight Flavor materials (flavoring, acidulant, sweetener) 10% by mass Total 100% by mass

[0057] [Tableting conditions for tablet production] Model: Rotary tablet press Collect 12HU (manufactured by Kikusui Seisakusho Co., Ltd.) Tableting pressure: 15kN Pestle size: diameter 15mmφ Tablet weight: 1g

[0058] <Storage stability: Viable bacteria survival rate after storage of chewable tablets (storage survival rate)> (Storage stability test) The chewable tablets were sealed in aluminum bags and subjected to a storage test for 6 months at 25° C. The survival rate of live bacteria after storage was calculated using the following formula and evaluated according to the following criteria. Preservation survival rate (%) = Number of viable bacteria after storage / Number of viable bacteria before storage × 100 [Criteria for survival rate] ◎: 70% or more, 〇: less than 70%, 60% or more, △: less than 60%, 50% or more, ×: less than 50%

[0059] <Preference: Sensory evaluation of texture (roughness)> Roughness was evaluated based on the powdery texture felt in the mouth when chewing the chewable tablet. The evaluation was performed by six panelists A to F, aged 20 to 50 years old. The powdery texture felt in the mouth may be due to the excipient (A2) contained in the double-coated particles when the coating performance of the double-coated particles is insufficient, or it may be due to raw materials other than the double-coated particles used to make the chewable tablet. No roughness or powdery feeling at all 5 points Slightly rough or powdery feeling: 3 points 1 point: Feels strongly rough or powdery

[0060] The roughness was evaluated as follows based on the average score of the six panelists, with the following "x" being the failure criterion. Over 4.0 points and 5.0 points or less Good roughness ◎ Over 3.0 points and 4.0 points or less Roughness acceptable Over 2.0 points and 3.0 points or less: Slightly rough △ 1.0 or more, 2.0 or less: Poor roughness ×

[0061] [Table 1-1] [Table 1-2]

[0062] [Table 2-1] [Table 2-2]

[0063] [Table 3-1] [Table 3-2]

[0064] In Examples 1 to 19, the core material (A) was a powder (A1) containing live bacteria with a bulk density of 0.2 to 0.7 and an excipient (A2) with a bulk density of 0.7 to 1.0 and a water activity of 0.30 or less, and a lipid with a melting point of 40°C to 70°C was used as the primary coating material (B) to form primary coated particles with an average particle size of 50 μm to 500 μm, and the surface of the obtained primary coated particles was coated with a lipid with a melting point of 40°C to 100°C as the secondary coating material (C), and the secondary coated particles were formed so that the average particle size of the secondary coated particles relative to the average particle size of the primary coated particles was 1.05 to 2.0, resulting in excellent results in all evaluations of processing stability, acid resistance, pressure resistance, storage stability, and palatability. In addition, the obtained acid-resistant powder had an average particle size of about 50 μm to 500 μm, so it was suitable as a raw material for other dosage forms such as tableting and soft capsules.

[0065] On the other hand, in Comparative Example 1, the primary coated particles were not coated with the secondary coating material (C), so the effects of acid resistance, pressure resistance, and storage stability were not obtained. Also, since the amount of the primary coating material (B) was large during the primary coating process, the particles were exposed to heat for a long time during coating with the primary coating material, and a tendency for processing stability to decrease was observed. In Comparative Example 2, since the primary coating process using the primary coating material was not performed, the coating with the secondary coating material was insufficient, and the effect of storage stability was not obtained. In Comparative Example 3, a primary coating material with a high melting point was used, so that during coating with the primary coating material, live bacteria were killed by contact with the high-temperature primary coating material, and processing stability was poor. In Comparative Example 4, a lipid having a melting point of less than 40° C. was used as the secondary coating material, so that the effects of acid resistance, pressure resistance, and storage stability were not obtained, and the palatability was also poor. In Comparative Example 5, the average particle size of the primary coated particles was less than 50 μm, so that the effects of acid resistance and storage stability were not obtained. In Comparative Example 6, the average particle size of the primary coated particles exceeded 500 μm, so that the processing stability was poor and the effects of acid resistance and storage stability were not obtained. In Comparative Example 7, the secondary coating material was melted and the secondary coated particles were formed using the melted secondary coating material, so that the heat killed the live bacteria and the processing stability was reduced. Also, the average particle size of the secondary coated particles relative to the average particle size of the primary coated particles exceeded 2.0, and a granulated product of the primary coated particles with the secondary coating material as the continuous phase was formed, so acid resistance, storage stability, and palatability were not obtained. In Comparative Examples 8 and 9, the excipient (A2) with a low bulk density and high water activity was used, and therefore the chewable tablets did not have sufficient storage stability. In Comparative Example 10, the live bacteria was not processed and the chewable tablets were made, so the acid resistance, pressure resistance, and storage stability were poor. In Comparative Example 11, the excipient (A2) was not used and the chewable tablets were made from baked starch alone, not from acid-resistant powder, but from baked starch alone, but from a rough texture and poor palatability. [Industrial Applicability]

[0066] A chewable tablet using the acid-resistant powder of the present invention has little viable bacteria killed even when subjected to the tableting pressure during processing into a chewable tablet, and has little roughness while still having little viable bacteria killed when stored as a chewable tablet, so that an excellent viable bacteria-containing chewable tablet can be provided.

Claims

1. An acid-resistant powder comprising primary coated particles which contain powder particles of a core substance (A) as a plurality of nuclei and are coated with a primary coating material (B) as a continuous phase, and secondary coated particles which have a structure in which the primary coated particles are coated with a secondary coating material (C) as a single nucleus, the core material (A) comprises a powder (A1) containing live bacteria having a bulk density of 0.2 to 0.7 and an excipient (A2) having a bulk density of 0.7 to 1.0 and a water activity of 0.30 or less; The primary coating material (B) contains a lipid having a melting point of 40° C. to 70° C., The secondary coating material (C) contains a lipid having a melting point of 40° C. to 100° C., The average particle size of the primary coated particles is 50 μm to 500 μm, The ratio of the average particle size of the secondary coated particles to the average particle size of the primary coated particles (average particle size of the secondary coated particles / average particle size of the primary coated particles) is 1.05 to 2.

00.

2. a mass ratio of the core material (A) to a total mass of the core material (A) and the primary coating material (B) is 0.65 to 0.90; 2. The acid-resistant powder according to claim 1, wherein a mass ratio of the primary coated particles to a total mass of the primary coated particles and the secondary coating material (C) is 0.60 to 0.

85.

3. 3. The acid-resistant powder according to claim 1, having an average particle size of 50 μm to 500 μm.

4. A food product comprising the acid-resistant powder according to claim 1 or 2.

5. A chewable tablet comprising the acid-resistant powder according to claim 1 or 2 and a water-soluble carbohydrate.

6. A method for producing the acid-resistant powder according to claim 1 or 2, A step of mixing the core material (A) and the primary coating material (B) to obtain the primary coated particles; A method for producing an acid-resistant powder, comprising: a step of mixing the primary coated particles with a powdery secondary coating material (C) to obtain the secondary coated particles.

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