Moisture-proof amino acid

By selecting appropriate excipients and formulation methods, moisture-proof and anti-caking amino acids were prepared, solving the problem of water-soluble amino acids easily absorbing moisture and clumping, and achieving high-content, stable and environmentally friendly amino acid products.

WO2026016964A1PCT designated stage Publication Date: 2026-01-22NANJING NUTRABUILDING BIO TECH CO LTD
View PDF 5 Cites 0 Cited by

Patent Information

Application Number
PCT/CN2025/107956
Authority / Receiving Office
WO · WO
Patent Type
Applications
Current Assignee / Owner
Priority Date
2024-07-15
Filing Date
2025-07-10
Publication Date
2026-01-22

AI Technical Summary

Technical Problem

Water-soluble amino acids are prone to absorbing moisture and clumping in the environment, which affects product quality and stability, and causes inconvenience in production and storage.

Method used

By selecting appropriate excipients and formulation methods, moisture-proof amino acids and anti-caking amino acids can be prepared, including coating treatment with excipients such as cellulose, starch, and gums to improve the stability and moisture-proof properties of amino acids.

Benefits of technology

It achieves high moisture-proof and anti-caking effects, improves the stability and applicability of amino acid products, reduces production costs, and is environmentally friendly with no solvent residue.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure PCTCN2025107956-APPB-I100001
    Figure PCTCN2025107956-APPB-I100001
  • Figure PCTCN2025107956-APPB-I100002
    Figure PCTCN2025107956-APPB-I100002
  • Figure PCTCN2025107956-APPB-I100003
    Figure PCTCN2025107956-APPB-I100003
Patent Text Reader

Abstract

The present invention provides a moisture-proof amino acid or an anti-caking amino acid, and a preparation method therefor. By performing auxiliary material selection and applying formulation processing to the moisture-proof amino acid or anti-caking amino acid raw material, the problem of such amino acid raw materials exhibiting extremely strong hygroscopic and deliquescent properties when exposed to air, or such amino acid raw materials either being prone to hardening and caking themselves or prone to caking and hardening upon moisture absorption, is solved, improving the stability of amino acid raw materials, and offering very high applicability to users. Moreover, the preparation process is simple, the production cost is low, and the preparation method is environmentally friendly.
Need to check novelty before this filing date? Find Prior Art

Description

Moisture-proof amino acid TECHNICAL FIELD

[0001] The present application belongs to the technical field of biological chemical industry, and particularly relates to a moisture-proof amino acid and a preparation method thereof. BACKGROUND

[0002] Amino acids are the basic units of proteins and are extremely important substances for the nutrition, survival and development of living organisms. In daily life, some amino acids need to be supplied by exogenous food. However, some water-soluble amino acid substances, such as alanine, aminoisobutyric acid, phenylalanine, tryptophan, methionine, valine, proline, glycine, serine, threonine, cysteine, aspartic acid, lysine, arginine, histidine, glutamic acid, etc. are hygroscopic and easy to cake and harden in the environment, thus bringing limitations to the production, application and preservation of products containing these amino acids, and also affecting the quality and stability of these products, and bringing poor experience to consumers. Water-soluble amino acids, such as malic acid, citrulline malic acid, SAMe, alanine, tryptophan, methionine, valine, proline, glycine, serine, threonine, cysteine, aspartic acid, lysine, arginine, histidine, glutamic acid, etc. are extremely easy to absorb moisture in the air. When producing products containing these amino acids, the absorbed moisture will cause poor weighing and feeding of these amino acids. Too much moisture will also cause the products containing these amino acids to be locally sticky and caked. These influences have a negative impact on the storage and production process of products containing these amino acids, bring many inconveniences, and also affect the quality and stability of these products.

[0003] Therefore, it is urgent to develop a moisture-proof amino acid product to solve the problem that it is extremely easy to absorb moisture, and a product that is anti-caking and has a high loading to solve the problem that it is easy to cake when wet, and the product will have a very broad market prospect. SUMMARY

[0004] In order to solve the above problems, the present application provides a moisture-proof amino acid and a preparation method thereof. By selecting excipients and processing the raw materials of the moisture-proof amino acid through a preparation method, the problem of extremely strong hygroscopicity and deliquescence of the amino acid when exposed to air is solved, excellent moisture-proof and deliquescence resistance effects are achieved, the stability of the hygroscopic amino acid raw material is improved, the demand for high content is met, great convenience is brought to transportation, storage and application scenarios, and high applicability is brought to users. In addition, the preparation process of the present application is simple and the production cost is low; no organic solvent is involved in the production process, which is friendly to the environment, and the product has no risk of residual solvent.

[0005] The application also provides an anti-caking amino acid and a preparation method thereof. By selecting excipients and processing raw materials of the anti-caking amino acid through a preparation method, the problem of easy caking or caking and dampening of the amino acid is solved, the stability of various amino acids is improved, the demand for high content is met, great convenience is brought to transportation, storage and application scenarios, and great applicability is brought to users. In addition, the preparation process is simple, the production cost is low, no organic solvent is involved in the production process, it is friendly to the environment, and there is no risk of residual solvent in the product.

[0006] In one aspect, the application provides a moisture-proof amino acid comprising not less than 50% by weight of amino acid, the amino acid being selected from one or more of malic acid, citrulline malate, SAMe, alanine, tryptophan, methionine, valine, proline, glycine, serine, threonine, cysteine, aspartic acid, lysine, arginine, histidine, glutamic acid.

[0007] In some embodiments, the moisture-proof amino acid comprises not less than 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45%, 50% by weight of amino acid. In some embodiments, the moisture-proof amino acid comprises not less than 51%, 52%, 53%, 54%, 55%, 56%, 57%, 58%, 59%, 60% by weight of amino acid. In some embodiments, the moisture-proof amino acid comprises 10-99%, 15-98%, 20-98%, 25-97%, 30-97%, 35-96%, 40-96%, 45-95%, 50-95% by weight of amino acid. In some embodiments, the moisture-proof amino acid comprises 50-99%, 55-98%, 60-97%, 65-97%, 70-96%, 75-95%, 80-95% by weight of amino acid.

[0008] In some embodiments, the moisture-proof amino acid has a water absorption rate of not higher than 40%, 30%, 25%, 15%, 10%, 5%. In some embodiments, the moisture-proof amino acid has a water absorption rate lower than that of the amino acid raw material.

[0009] In some embodiments, the moisture-proof amino acid further comprises an excipient.

[0010] In some embodiments, the excipient is selected from one or more of the following: hydroxypropyl cellulose, hydroxypropyl methyl cellulose, ethyl cellulose, methyl cellulose, microcrystalline cellulose, gum arabic, carrageenan, guar gum, modified starch, malt dextrin, talc, silicon dioxide, magnesium stearate, calcium silicate, calcium carbonate, calcium sulfate.

[0011] In some embodiments, the moisture resistant amino acid comprises 51-99% amino acid by weight; 1-49% of one or more excipients selected from the group consisting of: hydroxypropyl cellulose, hypromellose, ethyl cellulose, methyl cellulose, microcrystalline cellulose, acacia gum, carrageenan gum, guar gum, modified starch, maltodextrin, talc, silicon dioxide, magnesium stearate, calcium silicate, calcium carbonate, calcium sulfate.

[0012] In some embodiments, the moisture resistant amino acid comprises 55-97% amino acid by weight; 0.5-20% of one or more excipients selected from the group consisting of: microcrystalline cellulose, hydroxypropyl cellulose, methyl cellulose; 0.5-40% of one or more excipients selected from the group consisting of: hypromellose, ethyl cellulose, acacia gum, carrageenan gum, guar gum, modified starch, maltodextrin; 0.5-5% of one or more excipients selected from the group consisting of: magnesium stearate, calcium silicate, calcium carbonate, calcium sulfate, talc, silicon dioxide.

[0013] In some embodiments, the moisture resistant amino acid comprises 75-95% amino acid by weight; 1-8% of one or more excipients selected from the group consisting of: microcrystalline cellulose, hydroxypropyl cellulose, methyl cellulose; 1-15% of one or more excipients selected from the group consisting of: hypromellose, ethyl cellulose, acacia gum, carrageenan gum, guar gum, modified starch, maltodextrin; 1-2% of one or more excipients selected from the group consisting of: magnesium stearate, calcium silicate, calcium carbonate, calcium sulfate, talc, silicon dioxide.

[0014] In some embodiments, the moisture resistant amino acid is in a granular or powder form.

[0015] In some embodiments, the moisture resistant amino acid has a particle size of 5-100 mesh. In some embodiments, the moisture resistant amino acid has a particle size of 10-90 mesh, 15-80 mesh, 20-60 mesh.

[0016] In some embodiments, the moisture resistant amino acid is formulated into a nutritional supplement, a food, a beverage, or an animal feed.

[0017] In some embodiments, the moisture resistant amino acid is prepared as a solid formulation or a liquid formulation.

[0018] In another aspect, the present application provides a method for preparing a moisture resistant amino acid, the method comprising: configuring one or more excipients selected from the group consisting of: hypromellose, ethyl cellulose, acacia gum, carrageenan gum, guar gum, modified starch, maltodextrin into a solution; granulating and coating a formula amount of amino acid with the solution, one or more excipients selected from the group consisting of: microcrystalline cellulose, hydroxypropyl cellulose, methyl cellulose; drying and sieving; adding a formula amount of one or more excipients selected from the group consisting of: magnesium stearate, calcium silicate, calcium carbonate, calcium sulfate, talc, silicon dioxide to obtain the moisture resistant amino acid.

[0019] In some embodiments, the moisture resistant amino acid comprises 75-95% amino acid by weight; 1-8% of one or more excipients selected from microcrystalline cellulose, hydroxypropyl cellulose, methyl cellulose; 1-15% of one or more excipients selected from hydroxypropyl methyl cellulose, ethyl cellulose, gum arabic, carrageenan gum, guar gum, modified starch, maltodextrin; 1-2% of one or more excipients selected from magnesium stearate, calcium silicate, calcium carbonate, calcium sulfate, talc, silicon dioxide.

[0020] In some embodiments, the granulation coating is one of fluidized bed coating, compression coating and roll coating.

[0021] In some embodiments, the moisture resistant amino acid prepared by the method is used to prepare food, beverage, nutritional product, skin care product or cosmetic product.

[0022] In one aspect, the present application provides an anti-caking amino acid comprising not less than 50% amino acid by weight, the amino acid being selected from one or more of beta-alanine, L-citrulline, DL-malic acid, cysteine.

[0023] In some embodiments, the anti-caking amino acid comprises not less than 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45%, 50% amino acid by weight. In some embodiments, the anti-caking amino acid comprises not less than 51%, 52%, 53%, 54%, 55%, 56%, 57%, 58%, 59%, 60% amino acid by weight. In some embodiments, the anti-caking amino acid comprises 10-99%, 15-98%, 20-97%, 25-96%, 30-95%, 35-94%, 40-93%, 45-92%, 50-90% amino acid by weight. In some embodiments, the anti-caking amino acid comprises 50-99%, 51-98%, 52-97%, 55-96%, 58-95%, 60-95%, 65-92%, 70-90% amino acid by weight.

[0024] In some embodiments, the anti-caking amino acid has a sieving pass rate of not less than 80%, 85%, 86%, 87%, 88%, 89%, 90%, 91%. In some embodiments, the anti-caking amino acid has a sieving pass rate of 90% or more, 93% or more, 95% or more, 98% or more, 100% or close to 100%.

[0025] In some embodiments, the anti-caking amino acid has an anti-caking performance higher than the amino acid raw material itself, with an anti-caking rate of higher than 80%, preferably higher than 85%, 90%, or even 95%.

[0026] In some embodiments, the anti-caking amino acid further comprises an excipient.

[0027] In some embodiments, the excipient is selected from one or more of the following: microcrystalline cellulose, soluble starch, gum arabic, lactose, maltodextrin, talc, sodium aluminosilicate, calcium silicate, silicon dioxide, magnesium stearate.

[0028] In some embodiments, the anti-caking amino acid comprises, by weight, 51-98% of amino acid; 1-49% of one or more excipients selected from the following: microcrystalline cellulose, soluble starch, gum arabic, lactose, maltodextrin, talc, sodium aluminosilicate, calcium silicate, silicon dioxide, magnesium stearate.

[0029] In some embodiments, the anti-caking amino acid comprises, by weight, 60-95% of amino acid; 0.5-47% of one or more excipients selected from the following: microcrystalline cellulose, soluble starch, gum arabic, lactose, maltodextrin; 0.5-15% of one or more excipients selected from the following: talc, sodium aluminosilicate, calcium silicate, silicon dioxide, magnesium stearate.

[0030] In some embodiments, the anti-caking amino acid comprises, by weight, 70-90% of amino acid; 1-25% of one or more excipients selected from the following: microcrystalline cellulose, soluble starch, gum arabic, lactose, maltodextrin; 1-10% of one or more excipients selected from the following: talc, sodium aluminosilicate, calcium silicate, silicon dioxide, magnesium stearate.

[0031] In some embodiments, the anti-caking amino acid is in a granular or powdery form.

[0032] In some embodiments, the anti-caking amino acid has a particle size of 5-100 mesh. In some embodiments, the anti-caking amino acid can have a particle size of 15-90 mesh, 20-80 mesh.

[0033] In some embodiments, the anti-caking amino acid is formulated into a nutritional supplement, a food, a beverage, or an animal feed.

[0034] In some embodiments, the anti-caking amino acid is prepared as a solid formulation or a liquid formulation.

[0035] In another aspect, the present application provides a method for preparing an anti-caking amino acid, the method comprising dispersing a formula amount of amino acid, and one or more excipients selected from the following: microcrystalline cellulose, soluble starch, gum arabic, lactose, maltodextrin, talc, sodium aluminosilicate, calcium silicate, silicon dioxide, magnesium stearate in water, drying the resulting mixture, sieving, to obtain the anti-caking amino acid.

[0036] In some embodiments, the anti-caking amino acid comprises 51-98% amino acids by weight; and 1-49% of one or more excipients selected from the following: microcrystalline cellulose, soluble starch, gum arabic, lactose, maltodextrin, talc, sodium aluminosilicate, calcium silicate, silicon dioxide, and magnesium stearate.

[0037] In some embodiments, after sieving, one or more excipients selected from talc, sodium aluminosilicate, calcium silicate, silica, and magnesium stearate are added.

[0038] In some embodiments, the anti-caking amino acid comprises 60-95% amino acids by weight; 0.5-47% of one or more excipients selected from microcrystalline cellulose, soluble starch, gum arabic, lactose, and maltodextrin; and 0.5-15% of one or more excipients selected from talc, sodium aluminosilicate, calcium silicate, silicon dioxide, and magnesium stearate.

[0039] In some embodiments, the drying process is one of spray drying, vacuum drying, atmospheric pressure drying, microwave drying, freeze drying, infrared drying, and fluidized bed drying.

[0040] In some implementations, the anti-caking amino acids prepared by this method are used in the preparation of food, beverages, nutritional products, skin care products, or cosmetics.

[0041] The summary provides a simplified overview of the selected concepts, which will be further described in the detailed description below. This summary is not intended to identify key or essential features of the claimed subject matter, nor is it intended to limit the scope of the claimed subject matter. Detailed Implementation

[0042] The present invention will now be further described with reference to preferred embodiments thereof. While the invention will be described in conjunction with preferred embodiments, it should be understood that they are not intended to limit the invention to these embodiments. Rather, the invention is intended to cover alternatives, modifications, and equivalents that may be included within the spirit and scope of the invention as defined in the claims.

[0043] As used herein, the term “or” is intended to include both “and” and “or”. In other words, the term “or” can also be replaced with “and / or”.

[0044] As used herein, unless the context clearly indicates otherwise, the singular forms “a / an” and “the” are intended to include the plural forms as well.

[0045] As used herein, the terms "comprising" or "including," or variations thereof, are intended to mean that the terms are used in their broadest sense and are not limited to the inclusion of every item listed. It is further intended that the use of the terms "comprising" or "including" or variations thereof, the terms "consisting essentially of" and "consisting of" are also intended to be used in their broadest sense and are not limited to the inclusion of every item listed.

[0046] In the present application, the scientific and technical terms used herein have the meanings commonly understood by one of ordinary skill in the art, unless otherwise indicated. Also, the laboratory procedures set forth herein are in accordance with conventional techniques of the respective field.

[0047] The starting materials or reagents used in the present application are commercially available unless otherwise specified. All reagents are of commercial reagent grade and used according to the standards received.

[0048] The moisture-proof amino acid and the preparation method thereof of the present application realize the preparation of high content moisture-proof amino acid through the screening of suitable excipients and preparation processes, achieve excellent moisture-proof and anti-caking effects, improve the stability of moisture-absorbing amino acid raw materials, and bring very high applicability to users. The amino acid used in the present application can be prepared and obtained by known methods.

[0049] The moisture-proof amino acid and the preparation method thereof of the present application realize the preparation of high content moisture-proof amino acid through the screening of suitable excipients and preparation processes, achieve excellent moisture-proof and anti-caking effects, improve the stability of moisture-absorbing amino acid raw materials, and bring very high applicability to users. The amino acid used in the present application can be prepared and obtained by known methods.

[0050] The following examples are illustrative of selected embodiments of the application, and are not meant to limit the scope of the application.

[0051] Example 1 Preparation of moisture-proof malic acid

[0052] Example 1.1 Moisture-proof malic acid includes the following components by weight percentage: malic acid 50%, microcrystalline cellulose 8%, gum arabic 40%, and magnesium stearate 2%. The malic acid is sieved through a 60-mesh sieve, the prescribed amount of malic acid and microcrystalline cellulose are weighed and placed in a fluidized bed coating machine, a 40% concentration gum arabic solution is added for granulation and coating, hot air drying is performed at 30°C, the granules are sieved through a 20-mesh sieve, and the prescribed amount of magnesium stearate is added to obtain moisture-proof malic acid granules.

[0053] Example 1.2 Moisture-proof malic acid includes the following components by weight percentage: malic acid 51%, microcrystalline cellulose 8%, carrageenan 39%, and magnesium stearate 2%. The malic acid is sieved through a 60-mesh sieve, the prescribed amount of malic acid and microcrystalline cellulose are weighed and placed in a fluidized bed coating machine, a 10% concentration carrageenan solution is added for granulation and coating, hot air drying is performed at 30°C, the granules are sieved through a 20-mesh sieve, and the prescribed amount of magnesium stearate is added to obtain moisture-proof malic acid granules.

[0054] Example 1.3 The moisture-proof malic acid comprises the following components by weight percentage: malic acid 55%, microcrystalline cellulose 8%, carrageenan 35%, magnesium stearate 2%. The malic acid is sieved through a 60-mesh sieve, the malic acid and microcrystalline cellulose of the prescribed amount are weighed into a fluidized bed coating machine, a 10% concentration of carrageenan solution is added for granulation and coating, hot air drying is performed at 30°C, the granules are sieved through a 20-mesh sieve, and the prescribed amount of magnesium stearate is added to obtain the moisture-proof malic acid granules.

[0055] Example 1.4 The moisture-proof malic acid comprises the following components by weight percentage: malic acid 80%, microcrystalline cellulose 8%, modified starch 10%, magnesium stearate 2%. The malic acid is sieved through a 60-mesh sieve, the malic acid and microcrystalline cellulose of the prescribed amount are weighed into a fluidized bed coating machine, a 20% concentration of modified starch solution is added for granulation and coating, hot air drying is performed at 30°C, the granules are sieved through a 20-mesh sieve, and the prescribed amount of magnesium stearate is added to obtain the moisture-proof malic acid granules.

[0056] Example 1.5 The moisture-proof malic acid comprises the following components by weight percentage: malic acid 87%, microcrystalline cellulose 3%, malt dextrin 8%, magnesium stearate 2%. The malic acid is sieved through a 60-mesh sieve, the malic acid and microcrystalline cellulose of the prescribed amount are weighed into a fluidized bed coating machine, a 40% concentration of malt dextrin solution is added for granulation and coating, hot air drying is performed at 30°C, the granules are sieved through a 20-mesh sieve, and the prescribed amount of magnesium stearate is added to obtain the moisture-proof malic acid granules.

[0057] Example 1.6 The moisture-proof malic acid comprises the following components by weight percentage: malic acid 97%, microcrystalline cellulose 1%, hydroxypropyl methyl cellulose 1%, magnesium stearate 1%. The malic acid is sieved through a 60-mesh sieve, the malic acid and microcrystalline cellulose of the prescribed amount are weighed into a fluidized bed coating machine, a 5% concentration of hydroxypropyl methyl cellulose solution is added for granulation and coating, hot air drying is performed at 30°C, the granules are sieved through a 20-mesh sieve, and the prescribed amount of magnesium stearate is added to obtain the moisture-proof malic acid granules.

[0058] Example 1.7 The moisture-proof malic acid comprises the following components by weight percentage: malic acid 96%, microcrystalline cellulose 1%, hydroxypropyl methyl cellulose 2%, calcium sulfate 1%. The malic acid is sieved through a 60-mesh sieve, the malic acid and microcrystalline cellulose of the prescribed amount are weighed into a fluidized bed coating machine, a 5% concentration of hydroxypropyl methyl cellulose solution is added for granulation and coating, hot air drying is performed at 30°C, the granules are sieved through a 20-mesh sieve, and the prescribed amount of calcium sulfate is added to obtain the moisture-proof malic acid granules.

[0059] Example 1.8 The moisture-proof malic acid comprises the following components by weight percentage: malic acid 95%, microcrystalline cellulose 1%, hydroxypropyl methyl cellulose 3%, magnesium stearate 1%. The malic acid is sieved through a 60-mesh sieve, the prescribed amount of malic acid and microcrystalline cellulose are weighed into a fluidized bed coating machine, a 5% concentration hydroxypropyl methyl cellulose solution is added for granulation coating, hot air drying at 30°C, sieving through a 20-mesh sieve to size, and the prescribed amount of magnesium stearate is added to obtain the moisture-proof malic acid granules. The material of this example has good flowability, does not stick to the pot, and has good performance in fluidized bed granulation and coating.

[0060] Example 2 Preparation of moisture-proof citrulline malate

[0061] Example 2.1 The moisture-proof citrulline malate comprises the following components by weight percentage: citrulline malate 50%, microcrystalline cellulose 8%, gum arabic 40%, calcium silicate 2%. The citrulline malate is sieved through a 60-mesh sieve, the prescribed amount of citrulline malate and microcrystalline cellulose are weighed into a fluidized bed coating machine, a 40% concentration gum arabic solution is added for granulation coating, hot air drying at 30°C, sieving through a 20-mesh sieve to size, and the prescribed amount of calcium silicate is added to obtain the moisture-proof citrulline malate granules.

[0062] Example 2.2 The moisture-proof citrulline malate comprises the following components by weight percentage: citrulline malate 75%, microcrystalline cellulose 8%, carrageenan 15%, magnesium stearate 2%. The malic acid is sieved through a 60-mesh sieve, the prescribed amount of citrulline malate and microcrystalline cellulose are weighed into a fluidized bed coating machine, a 10% concentration carrageenan solution is added for granulation coating, hot air drying at 30°C, sieving through a 20-mesh sieve to size, and the prescribed amount of magnesium stearate is added to obtain the moisture-proof citrulline malate granules.

[0063] Example 2.3 The moisture-proof citrulline malate comprises the following components by weight percentage: citrulline malate 80%, microcrystalline cellulose 8%, modified starch 10%, calcium sulfate 2%. The malic acid is sieved through a 60-mesh sieve, the prescribed amount of citrulline malate and microcrystalline cellulose are weighed into a fluidized bed coating machine, a 20% concentration modified starch solution is added for granulation coating, hot air drying at 30°C, sieving through a 20-mesh sieve to size, and the prescribed amount of calcium sulfate is added to obtain the moisture-proof citrulline malate granules.

[0064] Example 2.4 The moisture-proof citrulline malate comprises the following components by weight percentage: citrulline malate 87%, microcrystalline cellulose 3%, malt dextrin 8%, magnesium stearate 2%. The malic acid is sieved through a 60-mesh sieve, the prescribed amount of citrulline malate and microcrystalline cellulose are weighed into a fluidized bed coating machine, a 40% concentration malt dextrin solution is added for granulation coating, hot air drying at 30°C, sieving through a 20-mesh sieve to size, and the prescribed amount of magnesium stearate is added to obtain the moisture-proof citrulline malate granules.

[0065] Example 2.5. Moisture resistant citrulline malate includes the following components by weight percent: citrulline malate 97%, microcrystalline cellulose 1%, hydroxypropyl methylcellulose 1%, magnesium stearate 1%. The malate is sieved through a 60 mesh screen, the prescribed amount of citrulline malate and microcrystalline cellulose are weighed into a fluid bed coater, a 5% solution of hydroxypropyl methylcellulose is added, and the granulation is coated and dried at 30°C with hot air. The granulation is sieved through a 20 mesh screen, and the prescribed amount of magnesium stearate is added to obtain the moisture resistant citrulline malate granulation.

[0066] Example 2.6. Moisture resistant citrulline malate includes the following components by weight percent: citrulline malate 96%, microcrystalline cellulose 1%, hydroxypropyl methylcellulose 2%, calcium carbonate 1%. The malate is sieved through a 60 mesh screen, the prescribed amount of citrulline malate and microcrystalline cellulose are weighed into a fluid bed coater, a 5% solution of hydroxypropyl methylcellulose is added, and the granulation is coated and dried at 30°C with hot air. The granulation is sieved through a 20 mesh screen, and the prescribed amount of calcium carbonate is added to obtain the moisture resistant citrulline malate granulation.

[0067] Example 2.7. Moisture resistant citrulline malate includes the following components by weight percent: citrulline malate 95%, microcrystalline cellulose 1%, hydroxypropyl methylcellulose 3%, magnesium stearate 1%. The malate is sieved through a 60 mesh screen, the prescribed amount of citrulline malate and microcrystalline cellulose are weighed into a fluid bed coater, a 5% solution of hydroxypropyl methylcellulose is added, and the granulation is coated and dried at 30°C with hot air. The granulation is sieved through a 20 mesh screen, and the prescribed amount of magnesium stearate is added to obtain the moisture resistant citrulline malate granulation. The material in this example has good flow properties, does not stick to the pan, and has good fluid bed granulation and coating properties.

[0068] Example 3. Preparation of moisture resistant SAMe

[0069] Example 3.1. Moisture resistant SAMe includes the following components by weight percent: SAMe 50%, microcrystalline cellulose 8%, gum arabic 40%, magnesium stearate 2%. The SAMe is sieved through a 60 mesh screen, the prescribed amount of SAMe and microcrystalline cellulose are weighed into a fluid bed coater, a 40% solution of gum arabic is added, and the granulation is coated and dried at 30°C with hot air. The granulation is sieved through a 20 mesh screen, and the prescribed amount of magnesium stearate is added to obtain the moisture resistant SAMe granulation.

[0070] Example 3.2. Moisture resistant SAMe includes the following components by weight percent: SAMe 75%, microcrystalline cellulose 8%, carrageenan 15%, magnesium stearate 2%. The SAMe is sieved through a 60 mesh screen, the prescribed amount of SAMe and microcrystalline cellulose are weighed into a fluid bed coater, a 10% solution of carrageenan is added, and the granulation is coated and dried at 30°C with hot air. The granulation is sieved through a 20 mesh screen, and the prescribed amount of magnesium stearate is added to obtain the moisture resistant SAMe granulation.

[0071] Example 3.3 The moisture-proof SAMe comprises the following components by weight percentage: SAMe 80%, microcrystalline cellulose 8%, modified starch 10%, calcium carbonate 2%. SAMe is sieved through a 60-mesh sieve, the prescribed amount of SAMe and microcrystalline cellulose are weighed into a fluidized bed coating machine, a 20% concentration of modified starch solution is added for granulation and coating, hot air drying is performed at 30°C, the granules are sized through a 20-mesh sieve, and the prescribed amount of calcium carbonate is added to obtain the moisture-proof SAMe granules.

[0072] Example 3.4 The moisture-proof SAMe comprises the following components by weight percentage: SAMe 87%, microcrystalline cellulose 3%, maltodextrin 8%, silicon dioxide 2%. SAMe is sieved through a 60-mesh sieve, the prescribed amount of SAMe and microcrystalline cellulose are weighed into a fluidized bed coating machine, a 40% concentration of maltodextrin solution is added for granulation and coating, hot air drying is performed at 30°C, the granules are sized through a 20-mesh sieve, and the prescribed amount of silicon dioxide is added to obtain the moisture-proof SAMe granules.

[0073] Example 3.5 The moisture-proof SAMe comprises the following components by weight percentage: SAMe 97%, microcrystalline cellulose 1%, hydroxypropyl methyl cellulose 1%, magnesium stearate 1%. SAMe is sieved through a 60-mesh sieve, the prescribed amount of SAMe and microcrystalline cellulose are weighed into a fluidized bed coating machine, a 5% concentration of hydroxypropyl methyl cellulose solution is added for granulation and coating, hot air drying is performed at 30°C, the granules are sized through a 20-mesh sieve, and the prescribed amount of magnesium stearate is added to obtain the moisture-proof SAMe granules.

[0074] Example 3.6 The moisture-proof SAMe comprises the following components by weight percentage: SAMe 96%, microcrystalline cellulose 1%, hydroxypropyl methyl cellulose 2%, magnesium stearate 1%. SAMe is sieved through a 60-mesh sieve, the prescribed amount of SAMe and microcrystalline cellulose are weighed into a fluidized bed coating machine, a 5% concentration of hydroxypropyl methyl cellulose solution is added for granulation and coating, hot air drying is performed at 30°C, the granules are sized through a 20-mesh sieve, and the prescribed amount of magnesium stearate is added to obtain the moisture-proof SAMe granules.

[0075] Example 3.7 The moisture-proof SAMe comprises the following components by weight percentage: SAMe 95%, microcrystalline cellulose 1%, hydroxypropyl methyl cellulose 3%, calcium silicate 1%. SAMe is sieved through a 60-mesh sieve, the prescribed amount of SAMe and microcrystalline cellulose are weighed into a fluidized bed coating machine, a 5% concentration of hydroxypropyl methyl cellulose solution is added for granulation and coating, hot air drying is performed at 30°C, the granules are sized through a 20-mesh sieve, and the prescribed amount of calcium silicate is added to obtain the moisture-proof SAMe granules. The material in this example has good flowability, does not stick to the pot, and has good performance in fluidized bed granulation and coating.

[0076] Example 4 Preparation of moisture-proof alanine

[0077] Example 4.1 Moisture-proof alanine includes the following components by weight percentage: alanine 50%, microcrystalline cellulose 8%, gum arabic 40%, magnesium stearate 2%. Alanine is passed through a 60 mesh sieve, the prescribed amount of alanine and microcrystalline cellulose are weighed into a fluidized bed coating machine, 40% concentration gum arabic solution is added for granulation coating, 30°C hot air drying, 20 mesh sieve for granulation, and the prescribed amount of magnesium stearate is added to obtain moisture-proof alanine granules.

[0078] Example 4.2 Moisture-proof alanine includes the following components by weight percentage: alanine 75%, microcrystalline cellulose 8%, carrageenan 15%, magnesium stearate 2%. Alanine is passed through a 60 mesh sieve, the prescribed amount of alanine and microcrystalline cellulose are weighed into a fluidized bed coating machine, 10% concentration carrageenan solution is added for granulation coating, 30°C hot air drying, 20 mesh sieve for granulation, and the prescribed amount of magnesium stearate is added to obtain moisture-proof alanine granules.

[0079] Example 4.3 Moisture-proof SAMe includes the following components by weight percentage: alanine 80%, microcrystalline cellulose 8%, modified starch 10%, silicon dioxide 2%. Alanine is passed through a 60 mesh sieve, the prescribed amount of SAMe and microcrystalline cellulose are weighed into a fluidized bed coating machine, 20% concentration modified starch solution is added for granulation coating, 30°C hot air drying, 20 mesh sieve for granulation, and the prescribed amount of silicon dioxide is added to obtain moisture-proof alanine granules.

[0080] Example 4.4 Moisture-proof alanine includes the following components by weight percentage: alanine 87%, microcrystalline cellulose 3%, maltodextrin 8%, magnesium stearate 2%. Alanine is passed through a 60 mesh sieve, the prescribed amount of alanine and microcrystalline cellulose are weighed into a fluidized bed coating machine, 40% concentration maltodextrin solution is added for granulation coating, 30°C hot air drying, 20 mesh sieve for granulation, and the prescribed amount of magnesium stearate is added to obtain moisture-proof alanine granules.

[0081] Example 4.5 Moisture-proof alanine includes the following components by weight percentage: alanine 97%, microcrystalline cellulose 1%, hydroxypropyl methyl cellulose 1%, magnesium stearate 1%. Alanine is passed through a 60 mesh sieve, the prescribed amount of alanine and microcrystalline cellulose are weighed into a fluidized bed coating machine, 5% concentration hydroxypropyl methyl cellulose solution is added for granulation coating, 30°C hot air drying, 20 mesh sieve for granulation, and the prescribed amount of magnesium stearate is added to obtain moisture-proof alanine granules.

[0082] Example 4.6 Moisture-proof alanine includes the following components by weight percentage: alanine 96%, microcrystalline cellulose 1%, hydroxypropyl methyl cellulose 2%, magnesium stearate 1%. Alanine is passed through a 60 mesh sieve, the prescribed amount of alanine and microcrystalline cellulose are weighed into a fluidized bed coating machine, 5% concentration hydroxypropyl methyl cellulose solution is added for granulation coating, 30°C hot air drying, 20 mesh sieve for granulation, and the prescribed amount of magnesium stearate is added to obtain moisture-proof alanine granules.

[0083] Example 4.7 Moisture-proof alanine includes the following weight percentage of components: alanine 95%, microcrystalline cellulose 1%, hydroxypropyl methyl cellulose 3%, magnesium stearate 1%. Alanine is passed through a 60 mesh sieve, the prescribed amount of alanine, microcrystalline cellulose is placed in the fluidized bed coating machine, 5% concentration of hydroxypropyl methyl cellulose solution is added for granulation coating, 30°C hot air drying, passing through a 20 mesh sieve to granulate, and adding the prescribed amount of magnesium stearate to obtain moisture-proof alanine granules. The material of this example has good flowability, does not stick to the pot, and has good performance of fluidized bed granulation and coating.

[0084] Example 5 Moisture-proof performance of moisture-proof amino acid

[0085] Take a dry glass bottle (outer diameter 50 mm, height 100 mm), weigh the test product, and place it in an open container, and place it in a 75% RH stability using box. Every certain period of time (1 h, 2 h, 3 h, 5 h, 10 h, 15 h, 20 h), take out the glass bottle. According to the calculation formula: Calculate the 20 mesh sieve passing rate; and use a Karl Fischer moisture meter to measure the moisture.

[0086] The moisture-proof malic acid sample was placed in a 20 mesh sieve and the passing rate was detected, as shown in Table 1.1.

[0087] Table 1.1

[0088]

[0089] The moisture-proof melon amino acid malic acid sample was placed in a 20 mesh sieve and the passing rate was detected, as shown in Table 1.2.

[0090] Table 1.2

[0091]

[0092] The moisture-proof SAMe sample was placed in a 20 mesh sieve and the passing rate was detected, as shown in Table 1.3.

[0093] Table 1.3

[0094]

[0095] The moisture-proof alanine sample was placed in a 20 mesh sieve and the passing rate was detected, as shown in Table 1.4.

[0096] Table 1.4

[0097]

[0098] As can be seen from Table 1.1, the moisture-proof methacrylic acid sample particles of Example 1 have excellent moisture-proof performance while having high content under high humidity 75% RH conditions compared with the raw material. Among them, Example 1.8 has the best moisture-proof effect under high humidity, and reaches a high content of 95%. As can be seen from Table 1.2, the moisture-proof citrulline methacrylic acid sample particles of Example 2 have excellent moisture-proof performance while having high content under high humidity 75% RH conditions compared with the raw material. Among them, Example 2.7 has the best moisture-proof effect under high humidity, and reaches a high content of 95%. As can be seen from Table 1.3, the moisture-proof SAMe sample particles of Example 3 have excellent moisture-proof performance while having high content under high humidity 75% RH conditions compared with the raw material. Among them, Example 3.7 has the best moisture-proof effect under high humidity, and reaches a high content of 95%. As can be seen from Table 1.4, the moisture-proof alanine sample particles of Example 4 have excellent moisture-proof performance while having high content under high humidity 75% RH conditions compared with the raw material. Among them, Example 4.7 has the best moisture-proof effect under high humidity, and reaches a high content of 95%.

[0099] The moisture detection results of the moisture-proof methacrylic acid sample are shown in Table 2.1.

[0100] Table 2.1

[0101]

[0102] The moisture detection results of the moisture-proof citrulline methacrylic acid sample are shown in Table 2.2.

[0103] Table 2.2

[0104]

[0105] The moisture detection results of the moisture-proof SAMe sample are shown in Table 2.3.

[0106] Table 2.3

[0107]

[0108] The moisture detection results of the moisture-proof alanine sample are shown in Table 2.4.

[0109] Table 2.4

[0110]

[0111] As can be seen from Table 2.1, the moisture content of the moisture-proof malic acid sample particles of Example 1 is higher than that of the raw material, and the moisture-proof performance is excellent, and the moisture content is less increased. Among them, the moisture content of Example 1.8 is the least, the moisture-proof performance is the best, and reaches 95% high content. As can be seen from Table 2.2, the moisture content of the moisture-proof citrulline malate sample particles of Example 2 is higher than that of the raw material, and the moisture-proof performance is excellent, and the moisture content is less increased. Among them, the moisture content of Example 2.7 is the least, the moisture-proof performance is the best, and reaches 95% high content. As can be seen from Table 2.3, the moisture content of the moisture-proof SAMe sample particles of Example 3 is higher than that of the raw material, and the moisture-proof performance is excellent, and the moisture content is less increased. Among them, the moisture content of Example 3.7 is the least, the moisture-proof performance is the best, and reaches 95% high content. As can be seen from Table 2.4, the moisture content of the moisture-proof alanine sample particles of Example 4 is higher than that of the raw material, and the moisture-proof performance is excellent, and the moisture content is less increased. Among them, the moisture content of Example 4.7 is the least, the moisture-proof performance is the best, and reaches 95% high content.

[0112] The moisture-proof amino acid of the present application can achieve more obvious moisture-proof and anti-hydration and enhanced flowability than the raw material under high humidity conditions when containing not less than 51%, 52%, 53%, 54%, 55%, 56%, 57%, 58%, 59%, 60%, 61%, 62%, 63%, 64%, 65%, 70%, 75%, 80%, 85%, 90%, 95%, 97%, 99% of the amino acid by weight. The moisture-proof amino acid of the present application has a moisture content increase of less than 40%, preferably less than 30%, 20%, 10% than the raw material under high humidity 75% RH conditions for 20 hours.

[0113] Example 6 Preparation of anti-caking β-alanine

[0114] Example 6.1 Anti-caking β-alanine comprises the following components by weight percentage: β-alanine 50%, microcrystalline cellulose 47%, calcium silicate 3%. The prescribed amount of β-alanine, microcrystalline cellulose and calcium silicate are weighed and placed in purified water, sheared and dispersed to be uniform, and the suspension is sprayed and dried in a spray dryer, and then passed through a 20-mesh sieve to obtain anti-caking β-alanine.

[0115] Example 6.2 Anti-caking beta-alanine comprises the following weight percent of ingredients: beta-alanine 60%, microcrystalline cellulose 37%, calcium silicate 3%. The prescription amount of beta-alanine, microcrystalline cellulose and calcium silicate are weighed into purified water, sheared and dispersed to uniformity, the suspension is sprayed dry in a spray dryer, and passed through a 20 mesh screen to obtain anti-caking beta-alanine.

[0116] Example 6.3 Anti-caking beta-alanine comprises the following weight percent of ingredients: beta-alanine 70%, microcrystalline cellulose 27%, calcium silicate 3%. The prescription amount of beta-alanine, microcrystalline cellulose and calcium silicate are weighed into purified water, sheared and dispersed to uniformity, the suspension is sprayed dry in a spray dryer, and passed through a 20 mesh screen to obtain anti-caking beta-alanine.

[0117] Example 6.4 Anti-caking beta-alanine comprises the following weight percent of ingredients: beta-alanine 75%, microcrystalline cellulose 22%, calcium silicate 3%. The prescription amount of beta-alanine, microcrystalline cellulose and calcium silicate are weighed into purified water, sheared and dispersed to uniformity, the suspension is sprayed dry in a spray dryer, and passed through a 20 mesh screen to obtain anti-caking beta-alanine.

[0118] Example 6.5 Anti-caking beta-alanine comprises the following weight percent of ingredients: beta-alanine 80%, microcrystalline cellulose 17%, calcium silicate 3%. The prescription amount of beta-alanine, microcrystalline cellulose and calcium silicate are weighed into purified water, sheared and dispersed to uniformity, the suspension is sprayed dry in a spray dryer, and passed through a 20 mesh screen to obtain anti-caking beta-alanine.

[0119] Example 6.6 Anti-caking beta-alanine comprises the following weight percent of ingredients: beta-alanine 90%, microcrystalline cellulose 7%, calcium silicate 3%. The prescription amount of beta-alanine, microcrystalline cellulose and calcium silicate are weighed into purified water, sheared and dispersed to uniformity, the suspension is sprayed dry in a spray dryer, and passed through a 20 mesh screen to obtain anti-caking beta-alanine.

[0120] Example 6.7 Anti-caking beta-alanine comprises the following weight percent of ingredients: beta-alanine 98%, microcrystalline cellulose 1%, calcium silicate 1%. The prescription amount of beta-alanine, microcrystalline cellulose and calcium silicate are weighed into purified water, sheared and dispersed to uniformity, the suspension is sprayed dry in a spray dryer, and passed through a 20 mesh screen to obtain anti-caking beta-alanine.

[0121] Example 6.8 Anti-caking beta-alanine comprises the following weight percent of ingredients: beta-alanine 90%, microcrystalline cellulose 7%, calcium silicate 3%. The prescription amount of beta-alanine, microcrystalline cellulose and 2% calcium silicate are weighed into purified water, sheared and dispersed to uniformity, the suspension is sprayed dry in a spray dryer, and passed through a 20 mesh screen, and the remaining prescription amount of 1% calcium silicate is added to obtain anti-caking beta-alanine.

[0122] Example 6.9 Anti-caking beta-alanine comprises the following weight percent of ingredients: beta-alanine 90%, soluble starch 7%, calcium silicate 3%. Weigh out the prescription amount of beta-alanine, soluble starch and 2% calcium silicate into purified water, shear to disperse to uniform, spray dry the suspension into a spray dryer, pass through a 20 mesh screen, add the remaining prescription amount of 1% calcium silicate by weight to obtain anti-caking beta-alanine.

[0123] Example 6.10 Anti-caking beta-alanine comprises the following weight percent of ingredients: beta-alanine 90%, gum arabic 7%, calcium silicate 3%. Weigh out the prescription amount of beta-alanine, gum arabic and 2% calcium silicate into purified water, shear to disperse to uniform, spray dry the suspension into a spray dryer, pass through a 20 mesh screen, add the remaining prescription amount of 1% calcium silicate by weight to obtain anti-caking beta-alanine.

[0124] Example 6.11 Anti-caking beta-alanine comprises the following weight percent of ingredients: beta-alanine 90%, lactose 7%, calcium silicate 3%. Weigh out the prescription amount of beta-alanine, lactose and 2% calcium silicate into purified water, shear to disperse to uniform, spray dry the suspension into a spray dryer, pass through a 20 mesh screen, add the remaining prescription amount of 1% calcium silicate by weight to obtain anti-caking beta-alanine.

[0125] Example 6.12 Anti-caking beta-alanine comprises the following weight percent of ingredients: beta-alanine 90%, maltodextrin 7%, calcium silicate 3%. Weigh out the prescription amount of beta-alanine, maltodextrin and 2% calcium silicate into purified water, shear to disperse to uniform, spray dry the suspension into a spray dryer, pass through a 20 mesh screen, add the remaining prescription amount of 1% calcium silicate by weight to obtain anti-caking beta-alanine.

[0126] Example 6.13 Anti-caking beta-alanine comprises the following weight percent of ingredients: beta-alanine 90%, maltodextrin 4%, microcrystalline cellulose 3%, calcium silicate 3%. Weigh out the prescription amount of beta-alanine, maltodextrin, microcrystalline cellulose and 2% calcium silicate into purified water, shear to disperse to uniform, spray dry the suspension into a spray dryer, pass through a 20 mesh screen, add the remaining prescription amount of 1% calcium silicate by weight to obtain anti-caking beta-alanine.

[0127] Example 6.14 Anti-caking beta-alanine comprises the following weight percent of ingredients: beta-alanine 90%, maltodextrin 4%, microcrystalline cellulose 3%, calcium silicate 2%, talc 1%. Weigh out the prescription amount of beta-alanine, maltodextrin, microcrystalline cellulose, talc and 1% calcium silicate into purified water, shear to disperse to uniform, spray dry the suspension into a spray dryer, pass through a 20 mesh screen, add the remaining prescription amount of 1% calcium silicate by weight to obtain anti-caking beta-alanine.

[0128] Example 6.15 Anti-caking beta-alanine comprises the following weight percent of ingredients: beta-alanine 90%, maltodextrin 4%, microcrystalline cellulose 3%, calcium silicate 2%, sodium aluminosilicate 1%. Weigh the prescription amount of beta-alanine, maltodextrin, microcrystalline cellulose, sodium aluminosilicate and 1% of calcium silicate into purified water, shear to disperse uniformly, spray dry the suspension into a spray dryer, pass through a 20 mesh sieve, add the remaining prescription amount of 1% calcium silicate by conversion to obtain anti-caking beta-alanine.

[0129] Example 6.16 Anti-caking beta-alanine comprises the following weight percent of ingredients: beta-alanine 90%, maltodextrin 4%, microcrystalline cellulose 3%, calcium silicate 2%, silicon dioxide 1%. Weigh the prescription amount of beta-alanine, maltodextrin, microcrystalline cellulose, part of silicon dioxide and calcium silicate into purified water, shear to disperse uniformly, spray dry the suspension into a spray dryer, pass through a 20 mesh sieve, add the remaining prescription amount of silicon dioxide by conversion to obtain anti-caking beta-alanine.

[0130] Example 6.17 Anti-caking beta-alanine comprises the following weight percent of ingredients: beta-alanine 90%, maltodextrin 4%, microcrystalline cellulose 3%, calcium silicate 2%, magnesium stearate 1%. Weigh the prescription amount of beta-alanine, maltodextrin, microcrystalline cellulose, part of magnesium stearate and calcium silicate into purified water, shear to disperse uniformly, spray dry the suspension into a spray dryer, pass through a 20 mesh sieve, add the remaining prescription amount of magnesium stearate by conversion to obtain anti-caking beta-alanine.

[0131] Example 7 Preparation of anti-caking L-citrulline

[0132] Example 7.1 Anti-caking L-citrulline comprises the following weight percent of ingredients: L-citrulline 90%, maltodextrin 4%, microcrystalline cellulose 3%, calcium silicate 2%, talc 1%. Weigh the prescription amount of L-citrulline, maltodextrin, microcrystalline cellulose, talc and part of calcium silicate into purified water, shear to disperse uniformly, spray dry the suspension into a spray dryer, pass through a 20 mesh sieve, add the remaining prescription amount of calcium silicate by conversion to obtain anti-caking L-citrulline.

[0133] Example 7.2 Anti-caking L-citrulline comprises the following weight percent of ingredients: L-citrulline 90%, maltodextrin 4%, microcrystalline cellulose 3%, calcium silicate 2%, sodium aluminosilicate 1%. Weigh the prescription amount of L-citrulline, maltodextrin, microcrystalline cellulose, sodium aluminosilicate and part of calcium silicate into purified water, shear to disperse uniformly, spray dry the suspension into a spray dryer, pass through a 20 mesh sieve, add the remaining prescription amount of calcium silicate by conversion to obtain anti-caking L-citrulline.

[0134] Example 7.3 Anti-caking L-citrulline comprises the following weight percent of ingredients: L-citrulline 90%, maltodextrin 4%, microcrystalline cellulose 3%, calcium silicate 2%, silicon dioxide 1%. Weigh the prescription amount of L-citrulline, maltodextrin, microcrystalline cellulose, silicon dioxide and part of calcium silicate into purified water, shear dispersion to uniform, spray the suspension into the spray dryer to spray dry, pass through a 20 mesh sieve, add the rest of the prescription amount of calcium silicate to obtain anti-caking L-citrulline.

[0135] Example 7.4 Anti-caking L-citrulline comprises the following weight percent of ingredients: L-citrulline 90%, maltodextrin 4%, microcrystalline cellulose 3%, calcium silicate 2%, magnesium stearate 1%. Weigh the prescription amount of L-citrulline, maltodextrin, microcrystalline cellulose, magnesium stearate and part of calcium silicate into purified water, shear dispersion to uniform, spray the suspension into the spray dryer to spray dry, pass through a 20 mesh sieve, add the rest of the prescription amount of calcium silicate to obtain anti-caking L-citrulline.

[0136] Example 8 Preparation of anti-caking DL-malic acid

[0137] Example 8.1 Anti-caking DL-malic acid comprises the following weight percent of ingredients: DL-malic acid 90%, maltodextrin 4%, microcrystalline cellulose 3%, calcium silicate 2%, talc 1%. Weigh the prescription amount of DL-malic acid, maltodextrin, microcrystalline cellulose, talc and part of calcium silicate into purified water, shear dispersion to uniform, spray the suspension into the spray dryer to spray dry, pass through a 20 mesh sieve, add the rest of the prescription amount of calcium silicate to obtain anti-caking DL-malic acid.

[0138] Example 8.2 Anti-caking DL-malic acid comprises the following weight percent of ingredients: DL-malic acid 90%, maltodextrin 4%, microcrystalline cellulose 3%, calcium silicate 2%, sodium silicoaluminate 1%. Weigh the prescription amount of DL-malic acid, maltodextrin, microcrystalline cellulose, sodium silicoaluminate and part of calcium silicate into purified water, shear dispersion to uniform, spray the suspension into the spray dryer to spray dry, pass through a 20 mesh sieve, add the rest of the prescription amount of calcium silicate to obtain anti-caking DL-malic acid.

[0139] Example 8.3 Anti-caking DL-malic acid comprises the following weight percent of ingredients: DL-malic acid 90%, maltodextrin 4%, microcrystalline cellulose 3%, calcium silicate 2%, silicon dioxide 1%. Weigh the prescription amount of DL-malic acid, maltodextrin, microcrystalline cellulose, silicon dioxide and part of calcium silicate into purified water, shear dispersion to uniform, spray the suspension into the spray dryer to spray dry, pass through a 20 mesh sieve, add the rest of the prescription amount of calcium silicate to obtain anti-caking DL-malic acid.

[0140] Example 8.4 Anti-caking DL-malic acid comprises the following weight percent of ingredients: DL-malic acid 90%, maltodextrin 4%, microcrystalline cellulose 3%, calcium silicate 2%, magnesium stearate 1%. Weigh out the prescription amount of DL-malic acid, maltodextrin, microcrystalline cellulose, magnesium stearate and part of the calcium silicate into purified water, shear dispersion to uniform, the suspension to spray dryer spray dry, over 20 mesh sieve, add the rest of the prescription amount of calcium silicate, anti-caking DL-malic acid is obtained.

[0141] Example 9 Preparation of anti-caking cysteine

[0142] Example 9.1 Anti-caking cysteine comprises the following weight percent of ingredients: cysteine 90%, maltodextrin 4%, microcrystalline cellulose 3%, calcium silicate 2%, talc 1%. Weigh out the prescription amount of cysteine, maltodextrin, microcrystalline cellulose, talc and part of the calcium silicate into purified water, shear dispersion to uniform, the suspension to spray dryer spray dry, over 20 mesh sieve, add the rest of the prescription amount of calcium silicate, anti-caking cysteine is obtained.

[0143] Example 9.2 Anti-caking cysteine comprises the following weight percent of ingredients: cysteine 90%, maltodextrin 4%, microcrystalline cellulose 3%, calcium silicate 2%, sodium silicoaluminate 1%. Weigh out the prescription amount of cysteine, maltodextrin, microcrystalline cellulose, sodium silicoaluminate and part of the calcium silicate into purified water, shear dispersion to uniform, the suspension to spray dryer spray dry, over 20 mesh sieve, add the rest of the prescription amount of calcium silicate, anti-caking cysteine is obtained.

[0144] Example 9.3 Anti-caking cysteine comprises the following weight percent of ingredients: cysteine 90%, maltodextrin 4%, microcrystalline cellulose 3%, calcium silicate 2%, silicon dioxide 1%. Weigh out the prescription amount of cysteine, maltodextrin, microcrystalline cellulose, silicon dioxide and part of the calcium silicate into purified water, shear dispersion to uniform, the suspension to spray dryer spray dry, over 20 mesh sieve, add the rest of the prescription amount of calcium silicate, anti-caking cysteine is obtained.

[0145] Example 9.4 Anti-caking cysteine comprises the following weight percent of ingredients: cysteine 90%, maltodextrin 4%, microcrystalline cellulose 3%, calcium silicate 2%, magnesium stearate 1%. Weigh out the prescription amount of cysteine, maltodextrin, microcrystalline cellulose, magnesium stearate and part of the calcium silicate into purified water, shear dispersion to uniform, the suspension to spray dryer spray dry, over 20 mesh sieve, add the rest of the prescription amount of calcium silicate, anti-caking cysteine is obtained.

[0146] Example 10 Anti-caking performance of anti-caking amino acids

[0147] Take a dry weighing dish (outer diameter 50 mm, height 100 mm), take the appropriate amount of test sample and place it in it, place it in a 40°C / 75% RH stability box, and every time interval (1 h, 3 h, 7 h, 24 h), take out the glass bottle. According to the calculation formula: Calculate the 20-mesh sieve passing rate.

[0148] The anti-caking β-alanine sample was placed in a 20-mesh sieve and the passing rate was detected. The results are shown in Table 3.1.

[0149] Table 3.1

[0150]

[0151] The anti-caking L-citrulline sample was placed in a 20-mesh sieve and the passing rate was detected. The results are shown in Table 3.2.

[0152] Table 3.2

[0153]

[0154] The anti-caking cysteine sample was placed in a 20-mesh sieve and the passing rate was detected. The results are shown in Table 3.3.

[0155] Table 3.3

[0156]

[0157] As can be seen from Table 3.1, the anti-caking β-alanine sample of Example 1 has a 20-mesh sieve passing rate of 100% at a content of not less than 70% under accelerated / 75% RH conditions for 24 h. It has excellent anti-caking performance while having a high content of 90.0%. Examples 6.14 and 6.16 and other samples have the best anti-caking effect under high humidity, with a 20-mesh sieve passing rate of nearly 100% for 24 h, greatly improving the phenomenon of easy caking or easy caking due to moisture of the raw material itself. As can be seen from Tables 3.2 and 3.3, the anti-caking L-citrulline sample of Example 7 and the anti-caking cysteine sample of Example 9 have a 20-mesh sieve passing rate of 100% for 24 h. In addition, the process has considerable cost economy under mass production.

[0158] The anti-caking amino acid of the present application can achieve more obvious anti-caking and anti-hygroscopic and flowability enhancement effect than the raw material under high humidity conditions when containing not less than 51%, 52%, 53%, 54%, 55%, 56%, 57%, 58%, 59%, 60%, 61%, 62%, 63%, 64%, 65%, 70%, 75%, 80%, 85%, 90%, 95%, 97%, 99% of amino acid by weight. The anti-caking performance of the anti-caking amino acid of the present application is higher than that of the raw material itself, and the anti-caking performance is higher than 80%, preferably higher than 85%, 90%, and even 95%.

[0159] Although specific embodiments and examples of the present application have been described herein, those skilled in the art will understand that any modifications and variations can be made without departing from the principles of the present application. The above examples and illustrations are not limiting of the scope of the present application. Any combination of the embodiments of the present application, and any obvious extensions or analogs thereof, are within the scope of the present application. Furthermore, the present application encompasses any arrangement that exists to achieve the same purpose, and all such variations and modifications that fall within the scope of the appended claims.

Claims

1. A moisture resistant amino acid, characterized by, The moisture-proof amino acid comprises not less than 50% by weight of amino acids selected from one or more of malic acid, citrulline malate, SAMe, alanine, tryptophan, methionine, valine, proline, glycine, serine, threonine, cysteine, aspartic acid, lysine, arginine, histidine, glutamic acid.

2. The moisture resistant amino acid according to claim 1, characterized in that, The moisture-proof amino acid comprises not less than 51%, 52%, 53%, 54%, 55%, 56%, 57%, 58%, 59%, 60% by weight of amino acids.

3. The moisture-resistant amino acid according to claim 1 or 2, characterized in that, The moisture-proof amino acid has a water absorption rate of not more than 40%, 30%, 25%, 15%, 10%, 5%.

4. The moisture-resistant amino acid according to any one of claims 1 to 3, characterized in that, The moisture-proof amino acid further comprises excipients.

5. The moisture resistant amino acid according to claim 4, wherein The excipients are selected from one or more of p-hydroxypropyl cellulose, hydroxypropyl methyl cellulose, ethyl cellulose, methyl cellulose, microcrystalline cellulose, gum arabic, carrageenan, guar gum, modified starch, malt dextrin, talc, silicon dioxide, magnesium stearate, calcium silicate, calcium carbonate, calcium sulfate.

6. The moisture-resistant amino acid according to any one of claims 1 to 5, characterized in that, The moisture-proof amino acid comprises 51-99% by weight of amino acids; 1-49% by weight of one or more excipients selected from p-hydroxypropyl cellulose, hydroxypropyl methyl cellulose, ethyl cellulose, methyl cellulose, microcrystalline cellulose, gum arabic, carrageenan, guar gum, modified starch, malt dextrin, talc, silicon dioxide, magnesium stearate, calcium silicate, calcium carbonate, calcium sulfate.

7. The moisture-resistant amino acid according to any one of claims 1 to 6, characterized in that, The moisture-proof amino acid comprises 55-97% by weight of amino acids; 0.5-20% by weight of one or more excipients selected from microcrystalline cellulose, p-hydroxypropyl cellulose, methyl cellulose; 0.5-40% by weight of one or more excipients selected from hydroxypropyl methyl cellulose, ethyl cellulose, gum arabic, carrageenan, guar gum, modified starch, malt dextrin; 0.5-5% by weight of one or more excipients selected from magnesium stearate, calcium silicate, calcium carbonate, calcium sulfate, talc, silicon dioxide.

8. The moisture-resistant amino acid according to any one of claims 1 to 7, characterized in that, The moisture-proof amino acid comprises 75-95% by weight of amino acids; 1-8% by weight of one or more excipients selected from microcrystalline cellulose, p-hydroxypropyl cellulose, methyl cellulose; 1-15% by weight of one or more excipients selected from hydroxypropyl methyl cellulose, ethyl cellulose, gum arabic, carrageenan, guar gum, modified starch, malt dextrin; 1-2% by weight of one or more excipients selected from magnesium stearate, calcium silicate, calcium carbonate, calcium sulfate, talc, silicon dioxide.

9. The moisture-resistant amino acid according to any one of claims 1 to 8, characterized in that, The moisture-proof amino acid is in the form of granules or powder.

10. The moisture resistant amino acid according to claim 9, wherein The moisture-proof amino acid has a particle size of 5-100 mesh.

11. The moisture resistant amino acid according to any one of claims 1 to 10, characterized in that, The moisture-proof amino acid is formulated into a nutritional supplement, food, beverage or animal feed.

12. The moisture resistant amino acid according to any one of claims 1 to 11, characterized in that, The moisture-proof amino acid is prepared as a solid preparation or a liquid preparation.

13. A method of preparing moisture resistant amino acids, characterized by, The method comprises configuring one or more excipients selected from hydroxypropyl methyl cellulose, ethyl cellulose, gum arabic, carrageenan, guar gum, modified starch, malt dextrin into a solution; granulating and coating a formula amount of amino acids with one or more excipients selected from microcrystalline cellulose, p-hydroxypropyl cellulose, methyl cellulose; drying and sieving; adding a formula amount of one or more excipients selected from magnesium stearate, calcium silicate, calcium carbonate, calcium sulfate, talc, silicon dioxide to obtain the moisture-proof amino acid.

14. The method of claim 13, wherein, The moisture-proof amino acid comprises 75-95% amino acid by weight; 1-8% of one or more excipients selected from microcrystalline cellulose, hydroxypropyl cellulose, methyl cellulose; 1-15% of one or more excipients selected from hydroxypropyl methyl cellulose, ethyl cellulose, gum arabic, carrageenan, guar gum, modified starch, malt dextrin; 1-2% of one or more excipients selected from magnesium stearate, calcium silicate, calcium carbonate, calcium sulfate, talc, silicon dioxide.

15. The method according to claim 13 or 14, characterized in that, The granulating coating is one of fluidized bed coating, compression coating and rolling coating.

16. The method according to any one of claims 13-15, characterized by, The moisture-proof amino acid prepared by the method is used for preparing food, beverage, nutrient, skin care product or cosmetic.

17. A non-caking amino acid, characterized in that, The amino acid comprises not less than 50% by weight, and the amino acid is selected from one or more of beta-alanine, L-citrulline, DL-malic acid, cysteine.

18. The anti-caking amino acid of claim 17, wherein, The amino acid comprises not less than 51%, 52%, 53%, 54%, 55%, 56%, 57%, 58%, 59%, 60% by weight.

19. The anti-caking amino acid according to claim 17 or 18, characterized in that, The anti-caking amino acid has a screening passing rate of not less than 80%, 85%, 86%, 87%, 88%, 89%, 90%, 91%.

20. The anti-caking amino acid of any one of claims 17 to 19, wherein, The anti-caking amino acid further comprises an excipient.

21. The anti-caking amino acid of claim 20, wherein, The excipient is selected from one or more of the following: microcrystalline cellulose, soluble starch, gum arabic, lactose, malt dextrin, talc, sodium silicoaluminate, calcium silicate, silicon dioxide, magnesium stearate.

22. The anti-caking amino acid of any one of claims 17 to 21, wherein, The amino acid comprises 51-98% by weight; 1-49% of one or more excipients selected from the following: microcrystalline cellulose, soluble starch, gum arabic, lactose, malt dextrin, talc, sodium silicoaluminate, calcium silicate, silicon dioxide, magnesium stearate.

23. The anti-caking amino acid of any one of claims 17 to 22, wherein, The amino acid comprises 60-95% by weight; 0.5-47% of one or more excipients selected from the following: microcrystalline cellulose, soluble starch, gum arabic, lactose, malt dextrin; 0.5-15% of one or more excipients selected from the following: talc, sodium silicoaluminate, calcium silicate, silicon dioxide, magnesium stearate.

24. The anti-caking amino acid of any one of claims 17 to 23, wherein, The amino acid comprises 70-90% by weight; 1-25% of one or more excipients selected from the following: microcrystalline cellulose, soluble starch, gum arabic, lactose, malt dextrin; 1-10% of one or more excipients selected from the following: talc, sodium silicoaluminate, calcium silicate, silicon dioxide, magnesium stearate.

25. The anti-caking amino acid of any one of claims 17 to 24, wherein, The anti-caking amino acid is in the form of granules or powder.

26. The anti-caking amino acid of claim 25, wherein, The anti-caking amino acid has a particle size of 5-100 mesh.

27. The anti-caking amino acid of any one of claims 17 to 26, wherein, The anti-caking amino acid is formulated into a nutritional supplement, food, beverage or animal feed.

28. The anti-caking amino acid of any one of claims 17-27, wherein, The anti-caking amino acid is prepared as a solid preparation or a liquid preparation.

29. A method of making an anti-caking amino acid, characterized by, The method comprises dispersing a formula amount of amino acid and one or more excipients selected from the following: microcrystalline cellulose, soluble starch, gum arabic, lactose, malt dextrin, talc, sodium silicoaluminate, calcium silicate, silicon dioxide, magnesium stearate in water, drying the obtained mixture, screening, to obtain the anti-caking amino acid.

30. The method of claim 29, wherein, The anti-caking amino acid comprises 51-98% by weight of amino acid; 1-49% by weight of one or more excipients selected from the group consisting of microcrystalline cellulose, soluble starch, gum arabic, lactose, maltodextrin, talc, sodium aluminosilicate, calcium silicate, silicon dioxide, magnesium stearate.

31. The method of claim 29 or 30, wherein, After sieving, one or more excipients selected from the group consisting of talc, sodium aluminosilicate, calcium silicate, silicon dioxide, magnesium stearate are added.

32. The method of claim 31, wherein, The anti-caking amino acid comprises 60-95% by weight of amino acid; 0.5-47% by weight of one or more excipients selected from the group consisting of microcrystalline cellulose, soluble starch, gum arabic, lactose, maltodextrin; 0.5-15% by weight of one or more excipients selected from the group consisting of talc, sodium aluminosilicate, calcium silicate, silicon dioxide, magnesium stearate.

33. The method of any one of claims 29-32, wherein, The drying is one of spray drying, reduced pressure drying, normal pressure drying, microwave drying, freeze drying, infrared drying and boiling drying.

34. The method of any one of claims 29-33, wherein, The anti-caking amino acid prepared by the method is used for preparing food, beverage, nutritional product, skin care product or cosmetic.

Citation Information

Patent Citations

  • Methionine tablet preparation method

    CN104784142A

  • Moisture-proof premixing agent for medicine tableting and production method of moisture-proof premixing agent

    CN106265575A

  • Preparation method of moisture-proof amino acid material

    CN115397266A

  • Dampproof Chinese medicine sranular agent and its preparing method

    CN1781499A

  • Hydrophilic amino acid-containing preparation having improved taste

    US20110195115A1