Powder composition
A β-caryophyllene-starch hydrolysate powder composition without Tween 80 achieves improved dispersibility and stability, addressing autoxidation and aggregation issues, suitable for pharmaceutical and food uses.
Patent Information
- Application Number
- PCT/JP2025/008717
- Authority / Receiving Office
- WO · WO
- Patent Type
- Applications
- Current Assignee / Owner
- Priority Date
- 2024-09-17
- Filing Date
- 2025-03-10
- Publication Date
- 2025-09-18
AI Technical Summary
Existing methods for developing β-caryophyllene into powders face challenges with water dispersibility and stability, particularly due to autoxidation and aggregation issues, and compositions using Tween 80 are not stable for industrial use.
A powder composition comprising β-caryophyllene mixed with a starch hydrolysate having a specific degree of decomposition (R = 5≦R≦100) and without Tween 80 or certain polysorbates, combined with optional emulsifiers, is produced through emulsification and spray drying to enhance dispersibility and stability.
The resulting powder composition exhibits excellent water dispersibility and storage stability, with β-caryophyllene remaining stable, suitable for pharmaceutical and food applications.
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Abstract
Description
powder composition
[0001] The present invention relates to a powder composition, and more particularly to a powder composition containing the following components (A) and (B): (A) β-caryophyllene and (B) a starch hydrolysate, but not Tween 80, wherein R, the value of the degree of decomposition of the starch hydrolysate (B), satisfies the range of 5≦R≦100; and a powder composition containing the following components (A), (B), and (C): (A) β-caryophyllene, (B) a starch hydrolysate, and (C) an emulsifier (excluding (B) the starch hydrolysate and Tween 80), wherein R, the value of the degree of decomposition of the starch hydrolysate (B), satisfies the range of 5≦R≦100.
[0002] β-Caryophyllene (CAS registration number 87-44-5, molecular formula C15H24, molecular weight 204.35 or 204.36) is a terpene compound found in essential oils such as black pepper, basil, oregano, cinnamon, hops, rosemary, hemp, and cloves, and has been approved by the U.S. Food and Drug Administration (FDA) as a food flavoring agent. β-Caryophyllene is also a selective agonist of the cannabinoid receptor type 2 (CB2), and has been reported to exhibit antioxidant, anti-inflammatory, analgesic, sleep-promoting, hormone-stabilizing, stress-relieving, and anticonvulsant effects (see, for example, Non-Patent Document 1 listed below).
[0003] As described above, β-caryophyllene has excellent effects, and therefore it is conceivable that it could be developed into foods and pharmaceuticals, such as health foods and pharmaceuticals in the form of tablets, powders, or liquids. However, because β-caryophyllene is an oily component with high fat solubility, it is difficult to develop it as is, particularly as a powder or liquid, and ingenuity was required.
[0004] When a highly fat-soluble oil component is made into a powder or liquid, examples of methods that can be used include (i) a method of emulsifying the fat-soluble component to make a liquid, (ii) a method of combining the fat-soluble component with an excipient to make a powder, and (iii) a method of dispersing the powder in an aqueous solution to make a liquid. However, when using method (ii), by making the component into a powder and dividing it into small portions, the powder can be dissolved or dispersed in water when needed and taken, which is expected to be highly convenient when carrying it when going out, and therefore, the development of a powder using method (ii) is desired.
[0005] On the other hand, when developing a powder product, if the powder floats or aggregates when added to water, it is undesirable in terms of administration and appearance. Furthermore, because β-caryophyllene has a double bond in its molecule, it is prone to autoxidation due to the influence of air, etc., and there are problems with stability, such as deterioration over long-term storage. For these reasons, there is a need for the development of a powder containing β-caryophyllene that is highly dispersible in water and stable, and there is a need for the development of a powder composition for this purpose.
[0006] For example, Patent Document 1 discloses a composition containing β-caryophyllene and a pharmaceutically effective carrier for use in treating psychosis, and cites a powder formulation for oral administration. Non-Patent Document 2 describes the spray-drying and powdering of an emulsion containing fenugreek seed oil, a surfactant (i.e., emulsifier) Tween 80, and maltodextrin, and that the powder could be a candidate for a new health food. Non-Patent Document 3 describes that fenugreek seed oil contains β-caryophyllene.
[0007] Special Publication No. 2015-510926
[0008] Ilaria Ceccarelli et al. , Frontiers in Neuroscience, 14:P1-11, 2020 Mohona Munshi et al. , J. Food Process Preserve. 2022, 46: e16294 Theysshana Visuvanathan et al. , Plants, 2022, 11, 1450
[0009] However, Patent Document 1 does not disclose any specific powders or powder compositions. Furthermore, the powder compositions conceivable from Non-Patent Documents 2 and 3 contain Tween 80 as an emulsifier, but these studies only examine emulsion stability, not the stability of β-caryophyllene. Furthermore, the present inventors have demonstrated that β-caryophyllene is not stable in powder compositions containing Tween 80, and furthermore, the resulting powder compositions are difficult to recover, making them unsuitable for industrial use.
[0010] Therefore, an object of the present invention is to provide a powder composition containing β-caryophyllene, which has excellent water dispersibility and storage stability, and in which the β-caryophyllene contained therein is stable.
[0011] As a result of extensive research, the present inventors have found that a powder composition obtained by mixing β-caryophyllene with a starch hydrolysate has excellent water dispersibility and storage stability, and that the β-caryophyllene contained therein is stabilized, and have completed the following inventions.
[0012] (1) A powder composition containing the following components (A) and (B): (A) β-caryophyllene, and (B) a starch hydrolysate, but not containing Tween 80, wherein (B) the starch hydrolysate has a degree of decomposition, R, in the range of 5≦R≦100.
[0013] (2) A powder composition containing the following components (A) and (B): (A) β-caryophyllene, and (B) a starch hydrolysate, and not containing one or more polysorbates selected from the group consisting of Tween 20, Tween 60, Tween 65, and Tween 80, wherein (B) the starch hydrolysate has a degree of decomposition, R, in the range of 5≦R≦100.
[0014] (3) A powder composition containing the following components (A), (B), and (C): (A) β-caryophyllene, (B) a starch hydrolysate, and (C) an emulsifier (excluding (B) the starch hydrolysate and Tween 80), wherein R, which is a value of the degree of decomposition of (B) the starch hydrolysate, is 5≦R≦100.
[0015] (4) A powder composition containing the following components (A), (B), and (C): (A) β-caryophyllene, (B) a starch hydrolyzate, and (C) an emulsifier (excluding (B) the starch hydrolyzate and one or more polysorbates selected from the group consisting of Tween 20, Tween 60, Tween 65, and Tween 80), wherein R, which is a value of the degree of decomposition of (B) the starch hydrolyzate, is 5≦R≦100.
[0016] (5) The powder composition according to any one of (1) to (4), which is a β-caryophyllene-stabilized powder composition.
[0017] (6) The powder composition according to any one of (1) to (4), wherein the content of (A) β-caryophyllene in the powder composition is 1 to 50 parts by weight per 100 parts by weight of the powder composition.
[0018] (7) A powder composition according to any one of (1) to (4), wherein the content of (B) the starch hydrolysate in the powder composition is 5 to 80 parts by weight per 100 parts by weight of the powder composition.
[0019] (8) A powder composition described in any one of (1) to (4), which is a pharmaceutical composition or a food or beverage composition.
[0020] (9) A method for producing a powder composition, comprising: a step of preparing a starch hydrolysate solution; a step of mixing the prepared starch hydrolysate solution with β-caryophyllene to prepare a mixed solution; a step of emulsifying the prepared mixed solution to prepare an emulsion; a step of preparing a spray slurry from the prepared emulsion; and a step of drying the prepared spray slurry, the method not comprising a step of adding Tween 80.
[0021] (10) A method for producing a powder composition, comprising: a step of preparing a starch hydrolysate solution; a step of mixing the prepared starch hydrolysate solution with β-caryophyllene to prepare a mixed liquid; a step of emulsifying the prepared mixed liquid to prepare an emulsion; a step of preparing a spray slurry from the prepared emulsion; and a step of drying the prepared spray slurry, the method not comprising a step of adding one or more polysorbates selected from the group consisting of Tween 20, Tween 60, Tween 65, and Tween 80.
[0022] (11) A method for producing a powder composition, comprising: preparing a starch hydrolysate solution; mixing the prepared starch hydrolysate solution with β-caryophyllene and an emulsifier (excluding starch hydrolysates and Tween 80) to prepare a mixture; emulsifying the prepared mixture to prepare an emulsion; preparing a spray slurry from the prepared emulsion; and drying the prepared spray slurry.
[0023] (12) A method for producing a powder composition, comprising: preparing a starch hydrolysate solution; mixing the prepared starch hydrolysate solution with β-caryophyllene and an emulsifier (excluding starch hydrolysates and one or more polysorbates selected from the group consisting of Tween 20, Tween 60, Tween 65, and Tween 80) to prepare a mixture; emulsifying the prepared mixture to prepare an emulsion; preparing a spray slurry from the prepared emulsion; and drying the prepared spray slurry.
[0024] (13) A method for improving the water dispersibility of a powder composition containing β-caryophyllene, the method comprising the step of mixing β-caryophyllene with a starch hydrolyzate, and not including the step of adding Tween 80.
[0025] (14) A method for improving the water dispersibility of a powder composition containing β-caryophyllene, the method comprising a step of mixing β-caryophyllene with a starch hydrolysate, and not including a step of adding one or more polysorbates selected from the group consisting of Tween 20, Tween 60, Tween 65, and Tween 80.
[0026] (15) A method for improving the water dispersibility of a powder composition containing β-caryophyllene, the method comprising the step of mixing β-caryophyllene, a starch hydrolysate, and an emulsifier (excluding starch hydrolysates and Tween 80).
[0027] (16) A method for improving the water dispersibility of a powder composition containing β-caryophyllene, the method comprising the step of mixing β-caryophyllene, a starch hydrolysate, and an emulsifier (excluding starch hydrolysates and one or more polysorbates selected from the group consisting of Tween 20, Tween 60, Tween 65, and Tween 80).
[0028] (17) A method for stabilizing β-caryophyllene contained in a powder composition, the method comprising a step of mixing β-caryophyllene with a starch hydrolyzate, and not including a step of adding Tween 80.
[0029] (18) A method for stabilizing β-caryophyllene contained in a powder composition, comprising a step of mixing β-caryophyllene with a starch hydrolysate, and not comprising a step of adding one or more polysorbates selected from the group consisting of Tween 20, Tween 60, Tween 65, and Tween 80.
[0030] (19) A method for stabilizing β-caryophyllene contained in a powder composition, comprising a step of mixing β-caryophyllene, a starch hydrolyzate, and an emulsifier (excluding starch hydrolyzate and Tween 80).
[0031] (20) A method for stabilizing β-caryophyllene contained in a powder composition, comprising a step of mixing β-caryophyllene, a starch hydrolyzate, and an emulsifier (excluding starch hydrolyzate and one or more polysorbates selected from the group consisting of Tween 20, Tween 60, Tween 65, and Tween 80).
[0032] According to the present invention, it is possible to provide a powder composition that has excellent water dispersibility and storage stability, and in which the β-caryophyllene contained therein is stabilized.
[0033] The powder composition according to the present invention, its production method, a method for improving the water dispersibility of a powder composition containing β-caryophyllene, and a method for stabilizing β-caryophyllene contained in a powder composition will be described in detail below. The powder composition according to the present invention comprises the following components (A) and (B): (A) β-caryophyllene, (B) a starch hydrolysate, and is free of Tween 80, or one or more polysorbates selected from the group consisting of Tween 20, Tween 60, Tween 65, and Tween 80, wherein R, which is a value of the degree of degradation of the starch hydrolysate, is 2<R≦100; and the following components (A), (B), and (C): (A) β-caryophyllene, (B) a starch hydrolysate, and (C) an emulsifier (with the proviso that (B) the starch hydrolysate and Tween 80, or one or more polysorbates selected from the group consisting of Tween 20, Tween 60, Tween 65, and Tween 80). 80, excluding one or more polysorbates selected from the group consisting of (A) and (B), wherein R, the value of the degree of decomposition of the starch decomposition product, is 2<R≦100.
[0034] As described above, β-caryophyllene used in the present invention is an essential oil component contained in black pepper, basil, oregano, cinnamon, hops, rosemary, cannabis, hemp, cloves, and the like. Therefore, β-caryophyllene can be extracted and purified from these materials by a method appropriately selected by a person skilled in the art and used. Alternatively, commercially available β-caryophyllene can also be used.
[0035] The β-caryophyllene that can be used in the present invention can be appropriately selected within a range that does not impair the characteristics of the present invention, and is not particularly limited. From the viewpoint of the stability of β-caryophyllene in the powder composition, however, the purity of β-caryophyllene is preferably 50% or more, more preferably 60% or more, even more preferably 70% or more, still more preferably 80% or more, and particularly preferably 90% or more.
[0036] The content of β-caryophyllene in the powder composition according to the present invention is 1 to 70 parts by weight, preferably 1 to 55 parts by weight, more preferably 2 to 54 parts by weight, more preferably 3 to 53 parts by weight, more preferably 5 to 50 parts by weight, more preferably 7 to 48 parts by weight, even more preferably 8 to 47 parts by weight, still more preferably 10 to 45 parts by weight, and particularly preferably 13 to 40 parts by weight, per 100 parts by weight of the powder composition. In this specification, numerical ranges expressed using "to" or "from" mean ranges that include the numerical values before and after "to" or "from" as the lower and upper limits.
[0037] In the present invention, the term "starch hydrolysate" refers to starch hydrolysed to an appropriate molecular weight using an acid and / or an enzyme, and the degree of hydrolysis (Dextrose Equivalent: DE) is used as an indicator. The starch hydrolysate that can be used in the present invention is not particularly limited as long as it does not impair the characteristics of the present invention, but such starch hydrolysates have a degree of hydrolysis (DE value) R of 2<R≦100, preferably a DE value R of 5≦R≦100, more preferably a DE value R of 7≦R≦100, more preferably a DE value R of 9≦R≦100, more preferably a DE value R of 11≦R≦100, more preferably a DE value R of 11≦R<100, more preferably a DE value R of 11≦R≦50, even more preferably a DE value R of 11≦R≦40, and even more preferably a DE value R of 11≦R≦25. Specific DE values of starch hydrolysates that can be used in the present invention include 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, and 49. , 50, 51, 52, 53, 54, 55, 56, 57, 58, 59, 60, 61, 62, 63, 64, 65, 66, 67, 68, 69, 70, 71, 72, 73, 74, 75, 76, 77, 78, 79, 80, 81, 82, 83, 84, 85, 86, 87, 88, 89, 90, 91, 92, 93, 94, 95, 96, 97, 98, 99, 100 can be mentioned. Note that these DE values are also values obtained by rounding off the decimal point of the DE value having a decimal point. Specific examples of starch hydrolysates include dextrin, maltodextrin, maltooligosaccharide, powdered candy, etc., and these may be used alone or in combination of two or more kinds. In the present invention, the starch hydrolysate may be a mixture of starch hydrolysates or starches having different DE values. In this case, the DE value is calculated as a weighted average based on the blending amounts and DE values of the starch hydrolysates and starches.Furthermore, the starch hydrolysate can function as a powdering base or an emulsifier in the powder composition according to the present invention.
[0038] The content of the starch hydrolysate in the powder composition according to the present invention is preferably 5 to 80 parts by weight, preferably 10 to 75 parts by weight, more preferably 10 to 70 parts by weight, even more preferably 10 to 65 parts by weight, still more preferably 15 to 60 parts by weight, and particularly preferably 20 to 47 parts by weight, relative to 100 parts by weight of the powder composition.
[0039] The powder composition according to the present invention may be prepared using Tween 80 (CAS No.: 9005-65-6, English name: Polyoxyethylene (20) Sorbitan Monooleate or Polysorbate 80), Tween 20 (CAS No.: 9005-64-5, English name: Polyoxyethylene (20) Sorbitan Monolaurate or Polysorbate 20), or Tween 60 (CAS No.: 9005-67-8, English name: Polyoxyethylene (20) Sorbitan Monostearate or Polysorbate 60), Tween 65 (CAS No.: 9005-71-4, English name: Polyoxyethylene (20) Sorbitan Tristearate or Polysorbate 65), and Tween 80. This is because, as in the case where Tween 80 is contained in the powder composition of the present invention, an unstable powder composition of the present invention may be produced.
[0040] In the powder composition according to the present invention, "β-caryophyllene is stable" refers to a powder composition that shows only a small change in oxidative odor and has both good aqueous dispersion speed and aqueous dispersion stability. Among powder compositions according to the present invention in which "β-caryophyllene is stable," those with a relatively high residual rate of β-caryophyllene are powder compositions in which "β-caryophyllene is more stable." In the present specification, the change in oxidative odor is confirmed by a sensory test, the aqueous dispersion speed and aqueous dispersion stability by a water dispersibility test, recoverability by determining whether or not the β-caryophyllene can be recovered by peeling off and dropping from the wall of a chamber upon application of vibration, and the residual rate of β-caryophyllene by headspace analysis.
[0041] The powder composition according to the present invention is preferably a powder composition in which β-caryophyllene is stabilized, that is, a β-caryophyllene-stabilized powder composition.
[0042] The powder composition according to the present invention may or may not contain an emulsifier other than starch hydrolysates and Tween 80. The emulsifier that can be used in the present invention is an emulsifier other than starch hydrolysates and Tween 80, and is not particularly limited as long as it does not impair the characteristics of the present invention. Examples of such emulsifiers include polyglycerol fatty acid esters, phospholipids, sucrose fatty acid esters, modified starches, etc., and these may be used alone or in combination.
[0043] The polyglycerol fatty acid esters that can be used in the present invention can be selected within a range that does not impair the characteristics of the present invention, and are not particularly limited. For example, they include esters of polyglycerol having an average degree of polymerization of 2 or more with, for example, citric acid, caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid, stearic acid, oleic acid, linoleic acid, pentastearic acid, monoisostearic acid, diisostearic acid, pentaisostearic acid, and pentaoleic acid. More specifically, they include polyglyceryl caprylate, tetraglyceryl monostearate, hexaglyceryl monolaurate, hexaglyceryl monomyristate, hexaglyceryl monopalmitate, hexaglyceryl monostearate, hexaglyceryl monooleate, hexaglyceryl tristearate, hexaglyceryl isostearate, decaglyceryl monolaurate, decaglyceryl monomyristate, decaglyceryl monopalmitate, and the like. Examples of suitable polyglycerol fatty acid esters include glyceryl stearate, glyceryl monostearate, glyceryl monooleate, glyceryl monolinoleate, glyceryl stearate citrate, tetraglyceryl tristearate, glyceryl distearate, glyceryl isostearate, glyceryl trioleate, glyceryl tristearate, glyceryl pentastearate, glyceryl monoisostearate, glyceryl diisostearate, glyceryl pentaisostearate, glyceryl pentaoleate, and the like. These polyglycerol fatty acid esters may include one or more polyglycerol fatty acid esters selected from the group consisting of glyceryl monomyristate, glyceryl monolaurate, and glyceryl caprylate. These polyglycerol fatty acid esters may be commercially available products.
[0044] The phospholipids that can be used in the present invention can be selected within a range that does not impair the characteristics of the present invention, and are not particularly limited. Examples of phospholipids that can be used in the present invention include glycerophospholipids such as phosphatidic acid, bisphosphatidic acid, lecithin (phosphatidylcholine), phosphatidylethanolamine, phosphatidylmethylethanolamine, phosphatidylserine, phosphatidylinositol, phosphatidylglycerin, and diphosphatidylglycerin (cardiolipin), as well as hydrogenated or hydroxylated versions of these; lysolecithin, lysophosphatidic acid, lysophosphatidylcholine, and glycerophospholipids such as lecithin, ... Examples of phospholipids include lyso compounds such as lysoglycerin, lysophosphatidylinositol, lysophosphatidylethanolamine, lysophosphatidylmethylethanolamine, lysophosphatidylcholine (lysolecithin), lysophosphatidylserine; various lecithins derived from plants such as soybean, corn, peanut, rapeseed, wheat, etc., from animals such as egg yolk, cow, and from microorganisms such as Escherichia coli; sphingophospholipids such as sphingomyelin, etc., and can include one or more phospholipids selected from the group consisting of these phospholipids, but lecithin is preferred.In addition, these phospholipids can be commercially available products.
[0045] The sucrose fatty acid ester that can be used in the present invention can be selected within a range that does not impair the characteristics of the present invention, and is not particularly limited. For example, sucrose fatty acid esters in which a fatty acid having 6 to 22 carbon atoms is ester-bonded to one or more hydroxyl groups of sucrose can be used. Specific examples of such sucrose fatty acid esters include sucrose laurate, sucrose myristate, sucrose palmitate, sucrose stearate, and sucrose oleate. The sucrose fatty acid ester may be either a monoester or a diester, and specific examples thereof include sucrose monolaurate, sucrose monomyristate, sucrose monopalmitate, sucrose monostearate, sucrose monooleate, sucrose dilaurate, sucrose dimyristate, sucrose dipalmitate, sucrose distearate, and sucrose dioleate. One or more sucrose fatty acid esters selected from the group consisting of these sucrose fatty acid esters may be included, with sucrose monolaurate, sucrose monomyristate, sucrose monopalmitate, sucrose monostearate, and sucrose monooleate being preferred, and sucrose monolaurate, sucrose monomyristate, and sucrose monostearate being more preferred. Commercially available sucrose fatty acid esters may be used.
[0046] The modified starch referred to in the present invention is also called chemically modified starch, and is starch that has been enzymatically and / or chemically and / or physically modified (Food Safety Commission Additives Evaluation Report "Modified Starch," issued November 2007). It is a food additive. Currently, 12 types of modified starch are available in Japan, specifically acetylated adipate cross-linked starch, acetylated oxidized starch, acetylated phosphate cross-linked starch, acetylated starch (starch acetate), oxidized starch, sodium octenyl succinate starch, hydroxypropyl starch, hydroxypropylated phosphate cross-linked starch, phosphated starch, phosphate monoesterified phosphate cross-linked starch, phosphate cross-linked starch, and sodium starch glycolate. These may be used alone or in combination. Preferred modified starches include oxidized starch, sodium octenyl succinate starch, and hydroxypropyl starch. In addition, commercially available modified starches can be used, and they can also function as a powdering base in the powder composition of the present invention.
[0047] The content of the emulsifier, excluding the starch hydrolysate and Tween 80, in the powder composition according to the present invention is preferably 5 to 50 parts by weight, preferably 5 to 40 parts by weight, preferably 5 to 35 parts by weight, more preferably 8 to 30 parts by weight, even more preferably 10 to 25 parts by weight, still more preferably 10 to 20 parts by weight, and particularly preferably 12 to 16 parts by weight, relative to 100 parts by weight of the powder composition.
[0048] The powder composition of the present invention may contain any substance, or may be used together with any substance by mixing, etc., as long as the characteristics of the present invention are not impaired. Such substances can be selected within the range that does not impair the characteristics of the present invention, and are not particularly limited, but examples thereof include antioxidants, other powdering bases, inorganic excipients, etc.
[0049] The antioxidant that can be used in the present invention is not particularly limited as long as it does not impair the characteristics of the present invention. Examples of such antioxidants include ascorbic acid or ascorbic acid derivatives or salts thereof, such as L-ascorbic acid, sodium L-ascorbate, potassium L-ascorbate, calcium L-ascorbate, L-ascorbic acid phosphate, magnesium L-ascorbic acid phosphate, L-ascorbic acid sulfate, disodium L-ascorbic acid sulfate, L-ascorbyl palmitate, and L-ascorbic acid 2-glucoside; tocopherols, such as tocopherol, tocotrienol, and mixed tocopherol; flavonoids (catechin, anthocyanin, flavones, isoflavones, flavans, and flava); Examples of antioxidants include polyphenols such as erythorbic acid, sodium erythorbate, potassium erythorbate, calcium erythorbate, erythorbic acid phosphate, and erythorbic acid sulfate, or salts thereof; ubiquinone, glutathione, lipoic acid, uric acid, urobilinogen, and bilirubin, which may be used alone or in combination. Preferred antioxidants include tocopherols, ascorbic acid or ascorbic acid derivatives or salts thereof, flavonoids, and phenolic acids.
[0050] The content of the antioxidant in the powder composition according to the present invention can be appropriately set within a range that does not impair the characteristics of the present invention, and is not particularly limited. For example, the content is preferably 10 parts by weight or less, more preferably 1 to 8 parts by weight, and even more preferably 1 to 5 parts by weight, relative to 100 parts by weight of the powder composition.
[0051] In the present invention, carrageenan, tamarind seed gum, tara gum, karaya gum, guar gum, locust bean gum, tragacanth gum, pullulan, gellan gum, native gellan gum, gum arabic, xanthan gum, and the like may be used. These can function as powdering bases in the powder composition of the present invention. The content of these in the powder composition of the present invention can be appropriately set within a range that does not impair the characteristics of the present invention, and is not particularly limited. However, the content is preferably 5 to 70 parts by weight, more preferably 10 to 50 parts by weight, even more preferably 10 to 30 parts by weight, and even more preferably 15 to 25 parts by weight per 100 parts by weight of the powder composition.
[0052] In the present invention, inorganic excipients such as talc, fine silicon dioxide, light anhydrous silicic acid, and hydrous silicon dioxide may also be used. These can function as powdering bases in the powder composition of the present invention. The content of these excipients in the powder composition of the present invention can be appropriately set within a range that does not impair the characteristics of the present invention, and is not particularly limited, but is 0.5 to 70 parts by weight, preferably 0.5 to 50 parts by weight, more preferably 0.5 to 30 parts by weight, and even more preferably 0.5 to 25 parts by weight, per 100 parts by weight of the powder composition.
[0053] The powder composition according to the present invention is preferably a pharmaceutical composition or a food or drink composition. When the powder composition according to the present invention is a food or drink composition, it is preferably used in health foods.
[0054] The powder composition of the present invention can be dissolved / dispersed in water and then taken. The amount of water used in such cases can be appropriately determined within a range that does not impair the characteristics of the present invention, and is not particularly limited. For example, the amount of water used can be 5 to 20 times the amount of the powder composition of the present invention.
[0055] Next, the method for producing the powder composition according to the present invention comprises, for example, the following steps: (i) a step of preparing a starch hydrolysate solution (starch hydrolysate solution preparation step): for example, a step of heating water to 40 to 70°C, and adding, mixing, and dissolving a starch hydrolysate, an emulsifier (excluding starch hydrolysates and Tween 80, or one or more polysorbates selected from the group consisting of Tween 20, Tween 60, Tween 65, and Tween 80) and other substances as required to prepare a starch hydrolysate solution; (ii) a step of mixing the starch hydrolysate solution prepared in the starch hydrolysate solution preparation step (i) with β-caryophyllene to prepare a mixture (mixture preparation step); (iii) a step of emulsifying the mixed liquid prepared in the mixed liquid preparation step (ii) to prepare an emulsion (mixed liquid emulsification step): for example, a step of emulsifying the mixed liquid prepared in the mixed liquid preparation step (ii) using a commercially available homogenizer; (iv) a step of preparing a spray slurry from the emulsion prepared in the mixed liquid emulsification step (iii) (spray slurry preparation step); (v) a step of drying the spray slurry prepared in the spray slurry preparation step (iv) (powder composition preparation step): for example, a step of drying the spray slurry prepared in the spray slurry preparation step (iv) using a commercially available spray dryer to prepare a powder composition.
[0056] In the present invention, the starch hydrolysate solution refers to a solution or suspension in which a starch hydrolysate is dissolved in an aqueous solvent. Examples of aqueous solvents include water such as ion-exchanged water and ultrapure water, and mixed solvents of water and water-soluble organic solvents (e.g., ethyl alcohol, ethylene glycol), but the present invention is not limited to these, and any solvent containing water or moisture will suffice.
[0057] The mixed solution preparation step (ii) may be a step of preparing a mixed solution by mixing the starch hydrolysate solution prepared in the starch hydrolysate solution preparation step (i), β-caryophyllene, and an emulsifier (excluding starch hydrolysates, and Tween 80, or one or more polysorbates selected from the group consisting of Tween 20, Tween 60, Tween 65, and Tween 80).
[0058] The method for producing a powder composition according to the present invention may include not only the above-mentioned "starch hydrolysate solution preparation step (i)," "mixed liquid preparation step (ii)," "mixed liquid emulsification step (iii)," "spray slurry preparation step (iv)," and "powder composition preparation step (v)," but also other steps as long as the features of the present invention are not impaired. Furthermore, the method may not include a specific step as long as the features of the present invention are not impaired, for example, "not including the step of adding Tween 80."
[0059] In addition to the above-mentioned production method, the powder composition according to the present invention can also be produced by commonly known methods such as freeze-drying, agitation granulation, and fluidized bed granulation.
[0060] Next, the method for improving the water dispersibility of a powder composition containing β-caryophyllene according to the present invention includes, for example, the following steps: (vi) a step of mixing β-caryophyllene with a starch hydrolyzate (mixing step).
[0061] The mixing step (vi) may be a step of mixing β-caryophyllene, a starch hydrolysate, and an emulsifier (excluding the starch hydrolysate and Tween 80, or one or more polysorbates selected from the group consisting of Tween 20, Tween 60, Tween 65, and Tween 80).
[0062] Next, the method for stabilizing β-caryophyllene contained in the powder composition according to the present invention includes, for example, the following steps: (vi) a step of mixing β-caryophyllene with a starch hydrolyzate (mixing step).
[0063] The mixing step (vi) may be a step of mixing β-caryophyllene, a starch hydrolysate, and an emulsifier (excluding the starch hydrolysate and Tween 80, or one or more polysorbates selected from the group consisting of Tween 20, Tween 60, Tween 65, and Tween 80).
[0064] The method of improving the water dispersibility of a powder composition containing β-caryophyllene and the method of stabilizing β-caryophyllene contained in the powder composition according to the present invention may include not only the above-mentioned "mixing step (vi)," but also other steps as long as the features of the present invention are not impaired. Furthermore, the method may not include a specific step as long as the features of the present invention are not impaired, for example, "the step of adding Tween 80 is not included."
[0065] In the following examples, the present invention will be described in more detail using test examples, but the technical scope of the present invention is not limited to the following examples.
[0066] [1-1] Preparation of Powder Composition of Test Example 1 Water was heated to 60°C, and 20.0 parts by weight of a starch hydrolysate and a commercially available emulsifier other than Tween 80, and 66.8 parts by weight of other substances (antioxidants, other powder bases, inorganic excipients, etc.) were added, mixed, and dissolved to prepare Liquid I. 13.2 parts by weight of β-caryophyllene was heated to 60°C and mixed with the prepared Liquid I, followed by emulsification using a commercially available homogenizer. A spray slurry was prepared from the resulting emulsion. The prepared spray slurry was dried using a commercially available spray dryer, yielding the powder composition of Test Example 1.
[0067] [1-2] Preparation of Powder Composition of Test Example 2 Water was heated to 60°C, and 20.0 parts by weight of starch, 12.3 parts by weight of a starch hydrolysate, and a commercially available emulsifier other than Tween 80, and 54.5 parts by weight of other substances (antioxidants, other powder bases, inorganic excipients, etc.) were added, mixed, and dissolved to prepare Liquid I. 13.2 parts by weight of β-caryophyllene was heated to 60°C and mixed with the prepared Liquid I. The mixture was then emulsified using a commercially available homogenizer, and a spray slurry was prepared from the resulting emulsion. The prepared spray slurry was dried using a commercially available spray dryer, to obtain the powder composition of Test Example 2.
[0068] [1-3] Preparation of Powder Composition of Test Example 3 Water was heated to 60°C, and 47.0 parts by weight of starch, 15.3 parts by weight of a starch hydrolysate, and a commercially available emulsifier other than Tween 80, and 24.5 parts by weight of other substances (antioxidants, other powder bases, inorganic excipients, etc.) were added, mixed, and dissolved to prepare Liquid I. 13.2 parts by weight of β-caryophyllene was heated to 60°C and mixed with the prepared Liquid I. The mixture was then emulsified using a commercially available homogenizer, and a spray slurry was prepared from the resulting emulsion. The prepared spray slurry was dried using a commercially available spray dryer, to obtain the powder composition of Test Example 3.
[0069] [1-4] Preparation of Powder Composition of Test Example 4 Water was heated to 60°C, and 20.8 parts by weight of a starch hydrolysate (DE2), 15.3 parts by weight of a commercially available emulsifier other than the starch hydrolysate and Tween 80, and 24.5 parts by weight of other substances (antioxidants, other powder bases, inorganic excipients, etc.) were added, mixed, and dissolved to prepare Liquid I. 39.4 parts by weight of β-caryophyllene was heated to 60°C and mixed with the prepared Liquid I, followed by emulsification using a commercially available homogenizer. A spray slurry was prepared from the resulting emulsion. The prepared spray slurry was dried using a commercially available spray dryer to obtain the powder composition of Test Example 4.
[0070] [1-5] Preparation of Powder Composition of Test Example 5 Water was heated to 60°C, and 47.0 parts by weight of a starch hydrolysate (DE2), 15.3 parts by weight of a commercially available emulsifier other than the starch hydrolysate and Tween 80, and 24.5 parts by weight of other substances (antioxidants, other powder bases, inorganic excipients, etc.) were added, mixed, and dissolved to prepare Liquid I. 13.2 parts by weight of β-caryophyllene was heated to 60°C and mixed with the prepared Liquid I, followed by emulsification using a commercially available homogenizer. A spray slurry was prepared from the resulting emulsion. The prepared spray slurry was dried using a commercially available spray dryer to obtain the powder composition of Test Example 5.
[0071] [1-6] Preparation of Powder Composition of Test Example 6 Water was heated to 60°C, and 47.0 parts by weight of a starch hydrolysate (DE5), 15.3 parts by weight of a commercially available emulsifier other than the starch hydrolysate and Tween 80, and 24.5 parts by weight of other substances (antioxidants, other powder bases, inorganic excipients, etc.) were added, mixed, and dissolved to prepare Liquid I. 13.2 parts by weight of β-caryophyllene was heated to 60°C and mixed with the prepared Liquid I. The mixture was then emulsified using a commercially available homogenizer, and a spray slurry was prepared from the resulting emulsion. The prepared spray slurry was dried using a commercially available spray dryer to obtain the powder composition of Test Example 6. The starch hydrolysate (DE5) used was prepared by mixing 23.5 g of a starch hydrolysate with a DE value of 11 and 23.5 g of starch with a DE value of 0.
[0072] [1-7] Preparation of Powder Composition of Test Example 7 Water was heated to 60°C, and 47.0 parts by weight of a starch hydrolysate (DE7), 15.3 parts by weight of a commercially available emulsifier other than the starch hydrolysate and Tween 80, and 24.5 parts by weight of other substances (antioxidants, other powder bases, inorganic excipients, etc.) were added, mixed, and dissolved to prepare Liquid I. 13.2 parts by weight of β-caryophyllene was heated to 60°C and mixed with the prepared Liquid I. The mixture was then emulsified using a commercially available homogenizer, and a spray slurry was prepared from the resulting emulsion. The prepared spray slurry was dried using a commercially available spray dryer to obtain the powder composition of Test Example 7. The starch hydrolysate (DE7) used was a mixture of 28.2 g of a starch hydrolysate with a DE value of 11 and 18.8 g of a starch hydrolysate with a DE value of 2.
[0073] [1-8] Preparation of Powder Composition of Test Example 8 Water was heated to 60°C, and 47.0 parts by weight of a starch hydrolysate (DE9), 15.3 parts by weight of a commercially available emulsifier other than the starch hydrolysate and Tween 80, and 24.5 parts by weight of other substances (antioxidants, other powder bases, inorganic excipients, etc.) were added, mixed, and dissolved to prepare Liquid I. 13.2 parts by weight of β-caryophyllene was heated to 60°C and mixed with the prepared Liquid I. The mixture was then emulsified using a commercially available homogenizer, and a spray slurry was prepared from the resulting emulsion. The prepared spray slurry was dried using a commercially available spray dryer to obtain the powder composition of Test Example 8. The starch hydrolysate (DE9) used was prepared by mixing 23.5 g of a starch hydrolysate with a DE value of 19 with 23.5 g of starch with a DE value of 0.
[0074] [1-9] Preparation of Powder Composition of Test Example 9 Water was heated to 60°C, and 20.0 parts by weight of a starch hydrolysate (DE11), 12.3 parts by weight of a commercially available emulsifier other than the starch hydrolysate and Tween 80, and 54.5 parts by weight of other substances (antioxidants, other powder bases, inorganic excipients, etc.) were added, mixed, and dissolved to prepare Liquid I. 13.2 parts by weight of β-caryophyllene was heated to 60°C and mixed with the prepared Liquid I, followed by emulsification using a commercially available homogenizer. A spray slurry was prepared from the resulting emulsion. The prepared spray slurry was dried using a commercially available spray dryer to obtain the powder composition of Test Example 9.
[0075] [1-10] Preparation of Powder Composition of Test Example 10 Water was heated to 60°C, and 20.0 parts by weight of a starch hydrolysate (DE11), 12.3 parts by weight of Tween 80, and 54.5 parts by weight of other substances (antioxidants, other powder bases, inorganic excipients, etc.) were added, mixed, and dissolved to prepare Liquid I. 13.2 parts by weight of β-caryophyllene was heated to 60°C and mixed with the prepared Liquid I. The mixture was then emulsified using a commercially available homogenizer, and a spray slurry was prepared from the resulting emulsion. The prepared spray slurry was dried using a commercially available spray dryer, and the resulting powder adhering to the wall of the chamber was removed using a commercially available brush, thereby obtaining the powder composition of Test Example 10.
[0076] [1-11] Preparation of Powder Composition of Test Example 11 Water was heated to 60°C, and 20.0 parts by weight of a starch hydrolysate (DE11), 6.6 parts by weight of Tween 80, and 60.2 parts by weight of other substances (antioxidants, other powder bases, inorganic excipients, etc.) were added, mixed, and dissolved to prepare Liquid I. 13.2 parts by weight of β-caryophyllene was heated to 60°C and mixed with the prepared Liquid I. The mixture was then emulsified using a commercially available homogenizer, and a spray slurry was prepared from the resulting emulsion. The prepared spray slurry was dried using a commercially available spray dryer, and the resulting powder adhering to the wall of the chamber was removed using a commercially available brush, thereby obtaining the powder composition of Test Example 11.
[0077] [1-12] Preparation of Powder Composition of Test Example 12 Water was heated to 60°C, and 80.2 parts by weight of a starch hydrolysate (DE11) and 6.6 parts by weight of Tween 80 were added, mixed, and dissolved to prepare Liquid I. 13.2 parts by weight of β-caryophyllene was heated to 60°C and mixed with the prepared Liquid I, followed by emulsification using a commercially available homogenizer. A spray slurry was prepared from the resulting emulsion. The prepared spray slurry was dried using a commercially available spray dryer, and the resulting powder adhering to the wall of the chamber was removed using a commercially available brush, thereby obtaining the powder composition of Test Example 12.
[0078] [1-13] Preparation of Powder Composition of Test Example 13 Water was heated to 60°C, and 85.0 parts by weight of a starch hydrolysate (DE11) and 5.0 parts by weight of Tween 80 were added, mixed, and dissolved to prepare Liquid I. 10.0 parts by weight of β-caryophyllene was heated to 60°C and mixed with the prepared Liquid I, followed by emulsification using a commercially available homogenizer. A spray slurry was prepared from the resulting emulsion. The prepared spray slurry was dried using a commercially available spray dryer, and the resulting powder adhering to the wall of the chamber was removed using a commercially available brush, thereby obtaining the powder composition of Test Example 13.
[0079] [1-14] Preparation of Powder Composition of Test Example 14 Water was heated to 60°C, and 20.8 parts by weight of a starch hydrolysate (DE11), 15.3 parts by weight of a commercially available emulsifier other than the starch hydrolysate and Tween 80, and 24.5 parts by weight of other substances (antioxidants, other powder bases, inorganic excipients, etc.) were added, mixed, and dissolved to prepare Liquid I. 39.4 parts by weight of β-caryophyllene was heated to 60°C and mixed with the prepared Liquid I, followed by emulsification using a commercially available homogenizer. A spray slurry was prepared from the resulting emulsion. The prepared spray slurry was dried using a commercially available spray dryer to obtain the powder composition of Test Example 14.
[0080] [1-15] Preparation of Powder Composition of Test Example 15 Water was heated to 60°C, and 20.8 parts by weight of a starch hydrolysate (DE11), 19.7 parts by weight of Tween 80, and 20.1 parts by weight of other substances (antioxidants, other powder bases, inorganic excipients, etc.) were added, mixed, and dissolved to prepare Liquid I. 39.4 parts by weight of β-caryophyllene was heated to 60°C and mixed with the prepared Liquid I. The mixture was then emulsified using a commercially available homogenizer, and a spray slurry was prepared from the resulting emulsion. The prepared spray slurry was dried using a commercially available spray dryer, and the resulting powder adhering to the wall of the chamber was removed using a commercially available brush, thereby obtaining the powder composition of Test Example 15.
[0081] [1-16] Preparation of Powder Composition of Test Example 16 Water was heated to 60°C, and 40.9 parts by weight of a starch hydrolysate (DE11) and 19.7 parts by weight of Tween 80 were added, mixed, and dissolved to prepare Liquid I. 39.4 parts by weight of β-caryophyllene was heated to 60°C and mixed with the prepared Liquid I, followed by emulsification using a commercially available homogenizer. A spray slurry was prepared from the resulting emulsion. The prepared spray slurry was dried using a commercially available spray dryer, and the resulting powder adhering to the wall of the chamber was removed using a commercially available brush, thereby obtaining the powder composition of Test Example 16.
[0082] [1-17] Preparation of Powder Composition of Test Example 17 Water was heated to 60°C, and 33.9 parts by weight of a starch hydrolysate (DE11), 15.3 parts by weight of a commercially available emulsifier other than the starch hydrolysate and Tween 80, and 24.5 parts by weight of other substances (antioxidants, other powder bases, inorganic excipients, etc.) were added, mixed, and dissolved to prepare Liquid I. 26.3 parts by weight of β-caryophyllene was heated to 60°C and mixed with the prepared Liquid I, followed by emulsification using a commercially available homogenizer. A spray slurry was prepared from the resulting emulsion. The prepared spray slurry was dried using a commercially available spray dryer to obtain the powder composition of Test Example 17.
[0083] [1-18] Preparation of Powder Composition of Test Example 18 Water was heated to 60°C, and 40.5 parts by weight of a starch hydrolysate (DE11), 15.3 parts by weight of a commercially available emulsifier other than the starch hydrolysate and Tween 80, and 24.5 parts by weight of other substances (antioxidants, other powder bases, inorganic excipients, etc.) were added, mixed, and dissolved to prepare Liquid I. 19.7 parts by weight of β-caryophyllene was heated to 60°C and mixed with the prepared Liquid I, followed by emulsification using a commercially available homogenizer. A spray slurry was prepared from the resulting emulsion. The prepared spray slurry was dried using a commercially available spray dryer to obtain the powder composition of Test Example 18.
[0084] [1-19] Preparation of Powder Composition of Test Example 19 Water was heated to 60°C, and 47.0 parts by weight of a starch hydrolysate (DE11), 15.3 parts by weight of a commercially available emulsifier other than the starch hydrolysate and Tween 80, and 24.5 parts by weight of other substances (antioxidants, other powder bases, inorganic excipients, etc.) were added, mixed, and dissolved to prepare Liquid I. 13.2 parts by weight of β-caryophyllene was heated to 60°C and mixed with the prepared Liquid I. The mixture was then emulsified using a commercially available homogenizer, and a spray slurry was prepared from the resulting emulsion. The prepared spray slurry was dried using a commercially available spray dryer, to obtain the powder composition of Test Example 19.
[0085] [1-20] Preparation of Powder Composition of Test Example 20 Water was heated to 60°C, and 33.9 parts by weight of a starch hydrolysate (DE 15), 15.3 parts by weight of a commercially available emulsifier other than the starch hydrolysate and Tween 80, and 24.5 parts by weight of other substances (antioxidants, other powder bases, inorganic excipients, etc.) were added, mixed, and dissolved to prepare Liquid I. 26.3 parts by weight of β-caryophyllene was heated to 60°C and mixed with the prepared Liquid I. The mixture was then emulsified using a commercially available homogenizer, and a spray slurry was prepared from the resulting emulsion. The prepared spray slurry was dried using a commercially available spray dryer to obtain the powder composition of Test Example 20.
[0086] [1-21] Preparation of Powder Composition of Test Example 21 Water was heated to 60°C, and 47.0 parts by weight of a starch hydrolysate (DE 15), 15.3 parts by weight of a commercially available emulsifier other than the starch hydrolysate and Tween 80, and 24.5 parts by weight of other substances (antioxidants, other powder bases, inorganic excipients, etc.) were added, mixed, and dissolved to prepare Liquid I. 13.2 parts by weight of β-caryophyllene was heated to 60°C and mixed with the prepared Liquid I. The mixture was then emulsified using a commercially available homogenizer, and a spray slurry was prepared from the resulting emulsion. The prepared spray slurry was dried using a commercially available spray dryer, yielding the powder composition of Test Example 21.
[0087] [1-22] Preparation of Powder Composition of Test Example 22 Water was heated to 60°C, and 47.0 parts by weight of a starch hydrolysate (DE 19), 15.3 parts by weight of a commercially available emulsifier other than the starch hydrolysate and Tween 80, and 24.5 parts by weight of other substances (antioxidants, other powder bases, inorganic excipients, etc.) were added, mixed, and dissolved to prepare Liquid I. 13.2 parts by weight of β-caryophyllene was heated to 60°C and mixed with the prepared Liquid I. The mixture was then emulsified using a commercially available homogenizer, and a spray slurry was prepared from the resulting emulsion. The prepared spray slurry was dried using a commercially available spray dryer, yielding the powder composition of Test Example 22.
[0088] [1-23] Preparation of Powder Composition of Test Example 23 Water was heated to 60°C, and 40.5 parts by weight of a starch hydrolysate (DE 25), 15.3 parts by weight of a commercially available emulsifier other than the starch hydrolysate and Tween 80, and 24.5 parts by weight of other substances (antioxidants, other powder bases, inorganic excipients, etc.) were added, mixed, and dissolved to prepare Liquid I. 19.7 parts by weight of β-caryophyllene was heated to 60°C and mixed with the prepared Liquid I. The mixture was then emulsified using a commercially available homogenizer, and a spray slurry was prepared from the resulting emulsion. The prepared spray slurry was dried using a commercially available spray dryer, yielding the powder composition of Test Example 23.
[0089] [1-24] Preparation of Powder Composition of Test Example 24 Water was heated to 60°C, and 47.0 parts by weight of a starch hydrolysate (DE 25), 15.3 parts by weight of a commercially available emulsifier other than the starch hydrolysate and Tween 80, and 24.5 parts by weight of other substances (antioxidants, other powder bases, inorganic excipients, etc.) were added, mixed, and dissolved to prepare Liquid I. 13.2 parts by weight of β-caryophyllene was heated to 60°C and mixed with the prepared Liquid I. The mixture was then emulsified using a commercially available homogenizer, and a spray slurry was prepared from the resulting emulsion. The prepared spray slurry was dried using a commercially available spray dryer to obtain the powder composition of Test Example 24.
[0090] [1-25] Preparation of Powder Composition of Test Example 25 Water was heated to 60°C, and 47.0 parts by weight of a starch hydrolysate (DE25), 15.3 parts by weight of Tween 80, and 24.5 parts by weight of other substances (antioxidants, other powder bases, inorganic excipients, etc.) were added, mixed, and dissolved to prepare Liquid I. 13.2 parts by weight of β-caryophyllene was heated to 60°C and mixed with the prepared Liquid I. The mixture was then emulsified using a commercially available homogenizer, and a spray slurry was prepared from the resulting emulsion. The prepared spray slurry was dried using a commercially available spray dryer, and the resulting powder adhering to the wall of the chamber was removed using a commercially available brush, thereby obtaining the powder composition of Test Example 25.
[0091] [1-26] Preparation of Powder Composition of Test Example 26 Water was heated to 60°C, and 71.5 parts by weight of a starch hydrolysate (DE25) and 15.3 parts by weight of Tween 80 were added, mixed, and dissolved to prepare Liquid I. 13.2 parts by weight of β-caryophyllene was heated to 60°C and mixed with the prepared Liquid I, followed by emulsification using a commercially available homogenizer. A spray slurry was prepared from the resulting emulsion. The prepared spray slurry was dried using a commercially available spray dryer, and the resulting powder adhering to the wall of the chamber was removed using a commercially available brush, thereby obtaining the powder composition of Test Example 26.
[0092] [1-27] Preparation of Powder Composition of Test Example 27 Water was heated to 60°C, and 47.0 parts by weight of a starch hydrolysate (DE 30), 15.3 parts by weight of a commercially available emulsifier other than the starch hydrolysate and Tween 80, and 24.5 parts by weight of other substances (antioxidants, other powder bases, inorganic excipients, etc.) were added, mixed, and dissolved to prepare Liquid I. 13.2 parts by weight of β-caryophyllene was heated to 60°C and mixed with the prepared Liquid I. The mixture was then emulsified using a commercially available homogenizer, and a spray slurry was prepared from the resulting emulsion. The prepared spray slurry was dried using a commercially available spray dryer to obtain the powder composition of Test Example 27. The starch hydrolysate (DE 30) used was a mixture of 28.2 g of a starch hydrolysate with a DE value of 40 and 18.8 g of a starch hydrolysate with a DE value of 15.
[0093] [1-28] Preparation of Powder Composition of Test Example 28 Water was heated to 60°C, and 47.0 parts by weight of a starch hydrolysate (DE 35), 15.3 parts by weight of a commercially available emulsifier other than the starch hydrolysate and Tween 80, and 24.5 parts by weight of other substances (antioxidants, other powder bases, inorganic excipients, etc.) were added, mixed, and dissolved to prepare Liquid I. 13.2 parts by weight of β-caryophyllene was heated to 60°C and mixed with the prepared Liquid I. The mixture was then emulsified using a commercially available homogenizer, and a spray slurry was prepared from the resulting emulsion. The prepared spray slurry was dried using a commercially available spray dryer to obtain the powder composition of Test Example 28. The starch hydrolysate (DE 35) used was a mixture of 37.6 g of a starch hydrolysate with a DE value of 40 and 9.6 g of a starch hydrolysate with a DE value of 15.
[0094] [1-29] Preparation of Powder Composition of Test Example 29 Water was heated to 60°C, and 47.0 parts by weight of a starch hydrolysate (DE 40), 15.3 parts by weight of a commercially available emulsifier other than the starch hydrolysate and Tween 80, and 24.5 parts by weight of other substances (antioxidants, other powder bases, inorganic excipients, etc.) were added, mixed, and dissolved to prepare Liquid I. 13.2 parts by weight of β-caryophyllene was heated to 60°C and mixed with the prepared Liquid I. The mixture was then emulsified using a commercially available homogenizer, and a spray slurry was prepared from the resulting emulsion. The prepared spray slurry was dried using a commercially available spray dryer to obtain the powder composition of Test Example 29.
[0095] [1-30] Preparation of Powder Composition of Test Example 30 Water was heated to 60°C, and 47.0 parts by weight of a starch hydrolysate (DE 46), 15.3 parts by weight of a commercially available emulsifier other than the starch hydrolysate and Tween 80, and 24.5 parts by weight of other substances (antioxidants, other powder bases, inorganic excipients, etc.) were added, mixed, and dissolved to prepare Liquid I. 13.2 parts by weight of β-caryophyllene was heated to 60°C and mixed with the prepared Liquid I. The mixture was then emulsified using a commercially available homogenizer, and a spray slurry was prepared from the resulting emulsion. The prepared spray slurry was dried using a commercially available spray dryer to obtain the powder composition of Test Example 30. The starch hydrolysate (DE 46) used was prepared by mixing 15.6 g of glucose with a DE value of 100 and 31.4 g of starch hydrolysate with a DE value of 19.
[0096] [1-31] Preparation of Powder Composition of Test Example 31 Water was heated to 60°C, and 47.0 parts by weight of a starch hydrolysate (DE50), 15.3 parts by weight of a commercially available emulsifier other than the starch hydrolysate and Tween 80, and 24.5 parts by weight of other substances (antioxidants, other powder bases, inorganic excipients, etc.) were added, mixed, and dissolved to prepare Solution I. 13.2 parts by weight of β-caryophyllene was heated to 60°C and mixed with the prepared Solution I. The mixture was then emulsified using a commercially available homogenizer, and a spray slurry was prepared from the resulting emulsion. The prepared spray slurry was dried using a commercially available spray dryer to obtain the powder composition of Test Example 31. The starch hydrolysate (DE50) used was a mixture of 23.5 g of glucose with a DE value of 100 and 23.5 g of starch with a DE value of 0.
[0097] [1-32] Preparation of Powder Composition of Test Example 32 Water was heated to 60°C, and 47.0 parts by weight of glucose (DE 100), 15.3 parts by weight of a starch hydrolysate and a commercially available emulsifier other than Tween 80, and 24.5 parts by weight of other substances (antioxidants, other powder bases, inorganic excipients, etc.) were added, mixed, and dissolved to prepare Liquid I. 13.2 parts by weight of β-caryophyllene was heated to 60°C and mixed with the prepared Liquid I. The mixture was then emulsified using a commercially available homogenizer, and a spray slurry was prepared from the resulting emulsion. The prepared spray slurry was dried using a commercially available spray dryer, yielding the powder composition of Test Example 32.
[0098] 2. Sensory Test for Change in Oxidative Odor 3 g of each of the prepared powder compositions of Test Examples 1 to 32 was placed in a 20 mL sample bottle, and the void in each sample bottle was filled with oxygen gas for 30 seconds and then sealed. The sample bottles were stored in a constant temperature bath at 60°C for 7 days, after which 24 people of all ages and genders performed a sensory evaluation of the change in oxidative odor. Specifically, a small change in oxidative odor between the time of placement in the 20 mL sample bottle and the time after storage in the constant temperature bath at 60°C for 7 days was marked with "Good," and a large change in oxidative odor was marked with "Poor."
[0099] 3. Calculation of β-caryophyllene Remaining Rate For the powder compositions of Test Examples 2, 3, 5, 19, and 23, the amount of remaining β-caryophyllene was quantified by headspace analysis using gas chromatography (first quantification), and then 3 g of each was placed in a 20 mL sample bottle. The void space in each sample bottle was filled with oxygen gas for 30 seconds, and the bottle was then sealed. These sample bottles were stored in a constant temperature bath at 60°C for 7 days, and the amount of remaining β-caryophyllene was again quantified by headspace analysis using gas chromatography (second quantification). The remaining rate of β-caryophyllene after oxidative degradation was calculated from the results of the first and second quantifications.
[0100] 4. Evaluation of Water Dispersibility [4-1] Evaluation of Water Dispersion Speed 100 mL of water was placed in a 200 mL beaker, a stirrer bar was placed in the beaker, and the mixture was stirred at 700 rpm. 300 mg of each of the powder compositions of Test Examples 1 to 32 was weighed out onto a medicine wrapping paper and placed in the beaker, and the water dispersion speed of each powder composition was confirmed. Powders that dispersed within 2 minutes were judged to have a water dispersion speed of "○ (good)," and powders that took more than 2 minutes were judged to have a dispersion speed of "× (poor)."
[0101] [4-2] Evaluation of Aqueous Dispersion Stability 100 mL of water was placed in a 200 mL beaker, a stirrer bar was placed in the beaker, and the mixture was stirred at 700 rpm. 300 mg of each of the powder compositions of Test Examples 1 to 32 was weighed out onto a medicine wrapping paper, placed in each beaker, and completely dispersed in water. After that, each dispersion was dispensed into a 20 mL sample bottle, the lid was closed, and the dispersion was allowed to stand at room temperature for 1 hour, after which the appearance of the dispersion was confirmed. If no oil float or oil ring was observed on the liquid surface or at the top of each dispersion, or if any precipitate was observed at the bottom of the 20 mL sample bottle, the aqueous dispersion stability was judged to be "○ (good)." If any precipitate was observed, the aqueous dispersion stability was judged to be "× (poor)."
[0102] 5. Evaluation of Recoverability The powder compositions of Test Examples 1 to 32 were evaluated for recoverability.
[0103] 6. Summary The above "1. Preparation of powder composition" to "5. Recoverability" are summarized in Tables 1 to 3 below.
[0104] [Table 1]
[0105] [Table 2]
[0106] [Table 3]
[0107] [6-1] Changes in Oxidized Odor As shown in Tables 1 to 3, it was revealed that the powder compositions of Test Examples 1 to 5, 10, 12, 13, 15, 16, 25, and 26 showed large changes in oxidized odor, while the powder compositions of the other Test Examples showed small changes in oxidized odor.
[0108] [6-2] Regarding the residual rate of β-caryophyllene As shown in Tables 1 to 3, the residual rate of β-caryophyllene was higher in the powder compositions of Test Examples 19 and 23, which showed only a small change in oxidized odor, compared to the powder compositions of Test Examples 2, 3, and 5, which showed a large change in oxidized odor. This indicates that β-caryophyllene is stable in the powder compositions of Test Examples 19 and 23.
[0109] [6-3] Evaluation of Water Dispersibility As shown in Tables 1 to 3, the powder compositions of Test Examples 1 and 11 had poor water dispersion speeds, the powder compositions of Test Examples 2 to 5 had poor water dispersion stability, and Test Examples 16 and 26 failed both the water dispersion speed test and the water dispersion stability test, but the powder compositions of the other Test Examples showed good results in both water dispersion speed and water dispersion stability. [6-4] Evaluation of Recoverability As shown in Tables 1 to 3, the powder compositions of Test Examples 10 to 13, 15, 16, 25, and 26, which contained Tween 80, all had difficulty in recovering, as the powder that was produced and adhered to the walls of the chamber had to be peeled off using a commercially available brush. [6-5] General The above [6-1] to [6-4] demonstrate that β-caryophyllene is stable in "a powder composition containing the following components (A) and (B): (A) β-caryophyllene and (B) a starch hydrolysate, but not Tween 80, wherein the value R, which represents the degree of decomposition of the starch hydrolysate (B), is 5≦R≦100" and "a powder composition containing the following components (A), (B), and (C): (A) β-caryophyllene, (B) a starch hydrolysate, and (C) an emulsifier (excluding the starch hydrolysate (B) and Tween 80), wherein the value R, which represents the degree of decomposition of the starch hydrolysate (B), is 5≦R≦100."
Claims
1. A powder composition containing the following components (A) and (B): (A) β-caryophyllene, and (B) a starch hydrolysate, but not containing Tween 80, wherein (B) the starch hydrolysate has a degree of decomposition, R, in the range of 5≦R≦100.
2. A powder composition containing the following components (A), (B), and (C): (A) β-caryophyllene, (B) a starch hydrolysate, and (C) an emulsifier (excluding (B) the starch hydrolysate and Tween 80), wherein R, the value of the degree of decomposition of (B) the starch hydrolysate, is 5≦R≦100.
3. The powder composition according to claim 1 or 2, wherein the powder composition is a β-caryophyllene-stabilized powder composition.
4. The powder composition according to claim 1 or 2, wherein the content of (A) β-caryophyllene in the powder composition is 1 to 50 parts by weight per 100 parts by weight of the powder composition.
5. A powder composition according to claim 1 or 2, wherein the content of (B) the starch hydrolysate in the powder composition is 5 to 80 parts by weight per 100 parts by weight of the powder composition.
6. A powder composition according to claim 1 or claim 2, which is a pharmaceutical composition or a food or beverage composition.
7. A method for producing a powder composition, comprising: preparing a starch hydrolysate solution; mixing the starch hydrolysate solution with β-caryophyllene to prepare a mixed solution; emulsifying the mixed solution to prepare an emulsion; preparing a spray slurry from the emulsion; and drying the spray slurry, the method not comprising the step of adding Tween 80.
8. A method for improving the water dispersibility of a powder composition containing β-caryophyllene, comprising the step of mixing β-caryophyllene with a starch hydrolysate, and not including the step of adding Tween 80.
9. A method for stabilizing β-caryophyllene contained in a powder composition, comprising a step of mixing β-caryophyllene with a starch hydrolysate, and not including a step of adding Tween 80.
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Patent Citations
New composition and method for producing the same
JP2004331597A