A high-stability creatine monohydrate composition and a method for preparing the same

Abstract

The application provides a high-stability creatine monohydrate composition and a preparation method thereof, and comprises core material and coating material; the core material comprises modified silicon dioxide 10-50 parts, creatine monohydrate 1-5 parts, a filler 10-50 parts and a binder 1-5 parts; the coating material comprises polyacrylic resin II 1-10 parts and a film-forming aid 1-20 parts; wherein the modified silicon dioxide is a product of KH570 grafted silicon dioxide and copolymerization of methacryloxypropyl double-terminated polydimethylsiloxane. The added modified silicon dioxide has a super large specific surface area, can firmly adsorb creatine monohydrate on the surface and enhance the stability of creatine monohydrate; meanwhile, through copolymerization with methacryloxypropyl double-terminated polydimethylsiloxane, the modified silicon dioxide forms a stable three-dimensional network structure of organic silicon, can wrap the adsorbed creatine monohydrate inside and further enhance the stability of creatine monohydrate.

Description

Technical Field

[0001] This invention relates to the field of feed additives, and in particular to a highly stable creatine monohydrate composition and its preparation method. Background Technology

[0002] Creatine is a nitrogen-containing organic acid that naturally exists in animal muscle and brain tissue. It can enhance muscle elasticity, accelerate protein synthesis, and rapidly provide energy to cells during energy metabolism. In animal husbandry, creatine is widely used as an important feed additive to improve animal muscle strength, increase muscle volume, improve growth performance, and enhance reproductive efficiency.

[0003] In existing technologies, creatine is typically added to feed in powder, granule, or solution form to support muscle strength growth and improve growth performance in animals. However, this process is accompanied by challenges: creatine is prone to absorbing moisture and clumping in humid environments, affecting its uniformity in feed and the efficiency of animal uptake; high temperatures during feed processing may reduce its bioactivity; and it may decompose in acidic or alkaline environments, affecting its stability and efficacy. Therefore, developing a new composition to improve the stability of creatine, allowing it to be stored for a longer period while maintaining its bioactivity, is of great significance to the field of feed additives.

[0004] In conclusion, there is an urgent need to develop a new technical solution to address the problems existing in the current technology and meet the development needs of the current market. Summary of the Invention

[0005] Based on this, the present invention provides a highly stable creatine monohydrate composition and its preparation method. The modified silica added to the highly stable creatine monohydrate composition provided by the present invention can firmly adsorb creatine monohydrate onto its surface, enhancing its stability; simultaneously, through copolymerization with methacryloyloxypropyl dimethylsiloxane, the modified silica forms a stable organosilicon three-dimensional network structure, which can encapsulate the adsorbed creatine monohydrate, further enhancing its stability.

[0006] One object of the present invention is to provide a highly stable creatine monohydrate composition, said highly stable creatine monohydrate composition comprising a core material and a packaging material covering the core material;

[0007] The core material comprises the following components in parts by weight:

[0008]

[0009] The packaging material comprises the following components in parts by weight:

[0010] Polyacrylic resin II 1-10 parts

[0011] 1-20 parts of film-forming aid;

[0012] in,

[0013] The modified silica is a product of KH570 grafted silica copolymerized with methacryloxypropyl dimethylsiloxane.

[0014] Furthermore, in the modified silica, the mass ratio of silica, KH570 and methacryloyloxypropyl dimethylsiloxane is 10:1-10:5-15.

[0015] Furthermore, the mass ratio of the core material to the packaging material is 10:1-3.

[0016] Furthermore, the filler is microcrystalline cellulose.

[0017] Furthermore, the adhesive is water-soluble starch.

[0018] Furthermore, the film-forming aid is polyvinylpyrrolidone.

[0019] Another object of the present invention is to provide a method for preparing the above-mentioned highly stable creatine monohydrate composition, comprising the following steps:

[0020] S1. Silica and KH570 are mixed, heated to react, purified and dried to obtain the intermediate product;

[0021] S2. The intermediate product, methacryloxypropyl dimethylsiloxane and initiator are mixed, heated and reacted, purified and dried to obtain modified silica.

[0022] S3. Dissolve creatine monohydrate in water, adsorb it with the modified silica, then mix it with filler and binder, granulate and dry to obtain core material;

[0023] S4. Mix polyacrylic acid resin II, film-forming aid and ethanol to obtain packaging material solution;

[0024] S5. Coat the core material with the packaging solution and dry it to obtain the highly stable creatine monohydrate composition.

[0025] Furthermore, the initiator is selected from one or more of benzoyl peroxide or azobisisobutyronitrile.

[0026] Furthermore, in step S1, the heating reaction is carried out at a temperature of 60-80°C for 10-20 hours.

[0027] Furthermore, in step S2, the heating reaction is carried out at a temperature of 90-120°C for 4-8 hours.

[0028] The present invention has the following beneficial effects:

[0029] The high-stability creatine monohydrate composition provided by this invention comprises a core material and a packaging material covering the core material. The core material is made of modified silica, creatine monohydrate, fillers, and binders, while the packaging material is made of polyacrylic acid resin II and film-forming aids. The modified silica is first modified using KH570 to introduce unsaturated double bonds on its surface, enhancing its compatibility with organic materials. Then, it is copolymerized with methacryloxypropyl dimethylsiloxane to obtain the modified silica. Adding the modified silica to the core material significantly improves the stability of creatine monohydrate. On the one hand, the modified silica has an extremely large specific surface area, and the large number of introduced siloxy groups have high surface activity and adsorption capacity, which can fully combine with creatine monohydrate and firmly adsorb it on the surface, thus enhancing its stability. On the other hand, through copolymerization with methacryloyloxypropyl double-terminated polydimethylsiloxane, the modified silica forms a stable organosilicon three-dimensional network structure. This network structure can encapsulate the creatine monohydrate bound to the silica, reducing its contact with the external environment and further enhancing its stability. Detailed Implementation

[0030] To more clearly illustrate the technical solution of the present invention, the following embodiments are provided. Unless otherwise stated, the raw materials, reactions, and post-processing methods appearing in the embodiments are all commercially available raw materials and technical methods well known to those skilled in the art.

[0031] The terms "preferred," "more preferably," and "more suitable" used in this invention refer to embodiments of the invention that provide certain beneficial effects under certain circumstances. However, other embodiments may also be preferred under the same or other circumstances. Furthermore, the description of one or more preferred embodiments does not imply that other embodiments are unavailable, nor is it intended to exclude other embodiments from the scope of this invention.

[0032] It should be understood that, except in any operational instance or otherwise indicated, the amounts or all figures representing ingredients used, for example, in the specification and claims, should be understood to be modified by the term "about" in all cases. Therefore, unless otherwise stated, the numerical parameters set forth in the following specification and appended claims are approximate values ​​varying according to the desired performance to be obtained according to the invention.

[0033] The microcrystalline cellulose used in the embodiments and comparative examples of this invention is ZW-301, which was purchased from Huzhou Zhanwang Pharmaceutical Co., Ltd.

[0034] The water-soluble starch used in the embodiments and comparative examples of this invention was purchased from Zhengzhou Dewang Chemical Industry Co., Ltd.

[0035] The polyacrylic acid resin II used in the embodiments and comparative examples of this invention was purchased from Huzhou Zhanwang Pharmaceutical Co., Ltd.

[0036] The methacryloyloxypropyl dimethylsiloxane used in the embodiments and comparative examples of this invention has a molecular weight of 8000-12000 and was purchased from Shanghai Aladdin Biochemical Technology.

[0037] In the embodiments and comparative examples of this invention, the polyvinylpyrrolidone used was K15, which was purchased from Huzhou Shenhua Polymer Materials Co., Ltd.

[0038] In the embodiments of this invention, "parts" refers to parts by mass.

[0039] Example 1

[0040] A highly stable creatine monohydrate composition, comprising a core material and a packaging material covering the core material;

[0041] The core material comprises the following components in parts by weight:

[0042]

[0043] The packaging material comprises the following components in parts by weight:

[0044] Polyacrylic resin II 6 parts

[0045] 9 parts of polyvinylpyrrolidone;

[0046] in,

[0047] The modified silica is a product of KH570 grafted silica copolymerized with methacryloxypropyl dimethylsiloxane.

[0048] The preparation method of the above-mentioned highly stable creatine monohydrate composition includes the following steps:

[0049] S1. Take 100 parts of a mixture of ethanol and water (ethanol:water = 9:1, V / V), add 10 parts of silica, stir for 1 h, adjust the pH to 4 with 1 mol / L hydrochloric acid solution, then add 5 parts of KH570, heat and stir at 70℃ for 12 h, then wash and dry to obtain the intermediate product.

[0050] S2. The intermediate product, 10 parts of methacryloyloxypropyl dimethylsiloxane, 1 part of benzoyl peroxide and 100 parts of toluene are mixed and heated under reflux at 120°C for 5 hours. Then the mixture is washed and dried to obtain modified silica.

[0051] S3. According to the above mass fractions, creatine monohydrate is dissolved in 12 parts of deionized water, the modified silica is added and adsorbed for 2 hours, then it is mixed with microcrystalline cellulose and water-soluble starch, 10 parts of deionized water are added, granulated and dried to obtain the core material.

[0052] S4. Dissolve polyacrylic acid resin II and polyvinylpyrrolidone in 15 parts of anhydrous ethanol, stir evenly, and obtain the packaging material solution.

[0053] S5. Using a fluidized bed coating machine, the core material is bottom-coated with the coating solution, then cooled to room temperature and passed through a 20-mesh sieve to obtain the highly stable creatine monohydrate composition.

[0054] Example 2

[0055] A highly stable creatine monohydrate composition, comprising a core material and a packaging material covering the core material;

[0056] The core material comprises the following components in parts by weight:

[0057]

[0058] The packaging material comprises the following components in parts by weight:

[0059] Polyacrylic resin II 4 parts

[0060] 6 parts of polyvinylpyrrolidone;

[0061] in,

[0062] The modified silica is a product of KH570 grafted silica copolymerized with methacryloxypropyl dimethylsiloxane.

[0063] The preparation method of the above-mentioned highly stable creatine monohydrate composition includes the following steps:

[0064] S1. Take 100 parts of a mixture of ethanol and water (ethanol:water = 9:1, V / V), add 10 parts of silica, stir for 1 h, adjust the pH to 4 with 1 mol / L hydrochloric acid solution, then add 5 parts of KH570, heat and stir at 70℃ for 12 h, then wash and dry to obtain the intermediate product.

[0065] S2. The intermediate product, 10 parts of methacryloyloxypropyl dimethylsiloxane, 1 part of benzoyl peroxide and 100 parts of toluene are mixed and heated under reflux at 120°C for 5 hours. Then the mixture is washed and dried to obtain modified silica.

[0066] S3. According to the above mass fractions, creatine monohydrate is dissolved in 9 parts of deionized water, the modified silica is added and adsorbed for 2 hours, then it is mixed with microcrystalline cellulose and water-soluble starch, 10 parts of deionized water are added, granulated and dried to obtain the core material.

[0067] S4. Dissolve polyacrylic acid resin II and polyvinylpyrrolidone in 10 parts of anhydrous ethanol, stir evenly, and obtain the packaging material solution.

[0068] S5. Using a fluidized bed coating machine, the core material is bottom-coated with the coating solution, then cooled to room temperature and passed through a 20-mesh sieve to obtain the highly stable creatine monohydrate composition.

[0069] Example 3

[0070] A highly stable creatine monohydrate composition, comprising a core material and a packaging material covering the core material;

[0071] The core material comprises the following components in parts by weight:

[0072]

[0073] The packaging material comprises the following components in parts by weight:

[0074] Polyacrylic resin II 8 parts

[0075] 12 parts of polyvinylpyrrolidone;

[0076] in,

[0077] The modified silica is a product of KH570 grafted silica copolymerized with methacryloxypropyl dimethylsiloxane.

[0078] The preparation method of the above-mentioned highly stable creatine monohydrate composition includes the following steps:

[0079] S1. Take 100 parts of a mixture of ethanol and water (ethanol:water = 9:1, V / V), add 10 parts of silica, stir for 1 h, adjust the pH to 4 with 1 mol / L hydrochloric acid solution, then add 5 parts of KH570, heat and stir at 70℃ for 12 h, then wash and dry to obtain the intermediate product.

[0080] S2. The intermediate product, 10 parts of methacryloyloxypropyl dimethylsiloxane, 1 part of benzoyl peroxide and 100 parts of toluene are mixed and heated under reflux at 120°C for 5 hours. Then the mixture is washed and dried to obtain modified silica.

[0081] S3. According to the above mass fractions, creatine monohydrate is dissolved in 15 parts of deionized water, the modified silica is added and adsorbed for 2 hours, then it is mixed with microcrystalline cellulose and water-soluble starch, 15 parts of deionized water are added, granulated and dried to obtain the core material.

[0082] S4. Dissolve polyacrylic acid resin II and polyvinylpyrrolidone in 20 parts of anhydrous ethanol, stir evenly, and obtain the packaging material solution.

[0083] S5. Using a fluidized bed coating machine, the core material is bottom-coated with the coating solution, then cooled to room temperature and passed through a 20-mesh sieve to obtain the highly stable creatine monohydrate composition.

[0084] Comparative Example 1

[0085] A highly stable creatine monohydrate composition is provided. The difference between this comparative example and Example 1 is that step S2 is omitted in the preparation method of the highly stable creatine monohydrate composition, and in step S3, the modified silica and other components are replaced by intermediate products. The other components and preparation methods are the same as in Example 1.

[0086] Comparative Example 2

[0087] A highly stable creatine monohydrate composition. The difference between this comparative example and Example 1 is that step S2 is omitted in the preparation method of the highly stable creatine monohydrate composition. In step S3, a mixture of intermediate product and methacryloyloxypropyl dimethylsiloxane with a mass ratio of 1:1 is used to replace the modified silica by an equal mass. Other components and preparation methods are the same as in Example 1.

[0088] Test case

[0089] Performance comparison tests were conducted on Examples 1-3 and Comparative Examples 1-2.

[0090] Test method: Take the high-stability creatine monohydrate composition samples prepared in Examples 1-3 and Comparative Examples 1-2, spread the samples evenly to ensure uniform thickness, and place them at room temperature (25℃). Samples were taken and tested at 0 days, 1 month, 3 months and 6 months. The specific test method is as follows: Take 5g of sample, dissolve it with deionized water, make up to 50mL, dilute, and use HPLC to determine the content of creatine monohydrate in the sample.

[0091] The calculation method for the content is as follows: the content of creatine monohydrate measured on day 0 is A, and the content measured after standing is B, then,

[0092]

[0093] The test results are shown in Table 1.

[0094] Table 1 Stability test results

[0095]

[0096] The experimental data above show that the high-stability creatine monohydrate compositions of Examples 1-3 maintained a content of over 96% after 6 months of storage, indicating that the high-stability creatine monohydrate compositions of the present invention have good stability. In contrast, Comparative Example 1 used an intermediate product to replace the modified silica, which lacked the high surface activity and adsorption capacity provided by the siloxy groups; Comparative Example 2 used a physical mixture of the intermediate product and methacryloyloxypropyl dimethylsiloxane to replace the modified silica, failing to form a three-dimensional organosilicon structure and thus unable to effectively encapsulate and protect the creatine monohydrate. Therefore, the stability of the prepared compositions was significantly reduced.

[0097] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above, and that the invention can be implemented in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of the invention is defined by the appended claims rather than the foregoing description. Thus, it is intended that all variations falling within the meaning and scope of equivalents of the claims be included within the present invention.

[0098] Furthermore, it should be understood that although this specification describes embodiments, not every embodiment contains only one independent technical solution. This narrative style is merely for clarity. Those skilled in the art should consider the specification as a whole, and the technical solutions in each embodiment can also be appropriately combined to form other embodiments that can be understood by those skilled in the art.

Claims

1. A high-stability creatine monohydrate composition, characterized by, The high-stability creatine monohydrate composition is composed of a core material and a coating material coated outside the core material; The core material comprises ingredients in mass fractions as follows: modified silica 10-50 parts creatine monohydrate 1-5 parts filler 10-50 parts binder 1-5 parts; The coating material comprises ingredients in mass fractions as follows: polyacrylic resin II 1-10 parts film-forming aid 1-20 parts; The modified silica is a product of copolymerization of KH570 grafted silica and methacryloxypropyl double-terminated polydimethylsiloxane; The mass ratio of silica, KH570 and methacryloxypropyl double-terminated polydimethylsiloxane in the modified silica is 10:1-10:5-15; The mass ratio of the core material to the coating material is 10:1-3; The filler is microcrystalline cellulose; The binder is water-soluble starch; The film-forming aid is polyvinylpyrrolidone.

2. The process for the preparation of the high stability creatine monohydrate composition as claimed in claim 1, characterized in that, The preparation method of the high-stability creatine monohydrate composition comprises the following steps: S1, blend silica and KH570, heat and react, purify and dry to obtain an intermediate product; S2, blend the intermediate product, methacryloxypropyl double-terminated polydimethylsiloxane and an initiator, heat and react, purify and dry to obtain modified silica; S3, dissolve creatine monohydrate in water, adsorb with the modified silica, then blend with microcrystalline cellulose and water-soluble starch, granulate and dry to obtain a core material; S4, blend polyacrylic resin II, polyvinylpyrrolidone and ethanol to obtain a coating material solution; S5, use the coating material solution to coat the core material, dry to obtain the high-stability creatine monohydrate composition; The initiator is dibenzoyl peroxide; In step S1, the temperature of the heat reaction is 60-80℃, and the time is 10-20 h; In step S2, the temperature of the heat reaction is 90-120℃, and the time is 4-8 h.

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