Moisture-proof anti-caking beta-aminoisobutyric acid and preparation method thereof

Abstract

The invention provides moisture-proof and anti-caking beta-aminoisobutyric acid and a preparation method thereof. The moisture-proof and anti-caking beta-aminoisobutyric acid comprises the following components in percentage by weight: 80-98% of beta-aminoisobutyric acid; and 0.1-15% of one or more of ethyl cellulose, lactose, resistant dextrin, hydroxypropyl methylcellulose, povidone, sodium carboxymethyl cellulose, magnesium stearate, calcium hydrophosphate and aerosil.

Description

Technical Field

[0001] The present invention relates to the technical field of health care product preparations, and in particular to moisture-proof and anti-caking beta-aminoisobutyric acid and a preparation method thereof. Background Art

[0002] β-Aminoisobutyric acid (BAIBA), a non-proteinogenic amino acid, plays a key role in regulating life activities and functions. Studies have shown that BAIBA has unique efficacy in regulating glucose and lipid metabolism, activating related signaling pathways, promoting fat breakdown and glucose transport, and has potential value in improving insulin resistance and preventing metabolic syndrome. At the same time, it also has antioxidant stress resistance, which can protect cells from oxidative damage by scavenging free radicals and regulating antioxidant enzyme activity, playing an important role in delaying aging and preventing related degenerative diseases. In addition, BAIBA performs outstandingly in maintaining intestinal barrier function and regulating the balance of intestinal flora, helping to enhance intestinal immunity and reduce the risk of intestinal inflammation.

[0003] However, β-aminoisobutyric acid (β-AIB) is a water-soluble amino acid that is highly hygroscopic. Once exposed to moisture, water molecules form hydrogen bonds and capillary forces between its crystal particles, causing the particles to adhere to each other and subsequently clumping. This agglomeration not only seriously affects the uniform dispersion and processing suitability of β-aminoisobutyric acid in pharmaceuticals, food nutrient fortifiers, feed additives, and other fields, increasing the difficulty of formulation, processing, and storage management for manufacturers; the agglomeration process may also be accompanied by crystal transformations and changes in chemical properties, reducing product stability and biological activity, shortening shelf life, and ultimately affecting the quality of the end product and impairing the consumer experience.

[0004] Therefore, developing β-aminoisobutyric acid products with high moisture-proof and anti-caking properties and high loading capacity, solving its moisture absorption, deliquescence and agglomeration problems, and improving product quality and application convenience has become a technical bottleneck that needs to be overcome urgently. It has great market application value and industrial development significance. Summary of the Invention

[0005] In one aspect, the present invention provides a moisture-proof and anti-caking β-aminoisobutyric acid, which comprises 80%-98% by weight of β-aminoisobutyric acid; 0.1-15% of one or more of ethyl cellulose, lactose, resistant dextrin, hydroxypropyl methylcellulose, povidone, sodium carboxymethyl cellulose, magnesium stearate, calcium hydrogen phosphate, and micropowdered silica gel.

[0006] In some embodiments, the moisture-proof and anti-caking β-aminoisobutyric acid comprises 80%-98% β-aminoisobutyric acid by weight; 1-11% one or more of ethyl cellulose, lactose, and resistant dextrin; 0.1-5% one or more of hydroxypropyl methylcellulose, povidone, and sodium carboxymethyl cellulose; and 0.5-5% one or more of magnesium stearate, calcium hydrogen phosphate, and micronized silica gel.

[0007] In some embodiments, the moisture-proof and anti-caking β-aminoisobutyric acid comprises 80%-93% β-aminoisobutyric acid by weight; 3-11% one or more of ethyl cellulose, lactose, and resistant dextrin; 0.2-4% one or more of hydroxypropyl methylcellulose, povidone, and sodium carboxymethyl cellulose; and 1-4% one or more of magnesium stearate, calcium hydrogen phosphate, and micronized silica gel.

[0008] In some embodiments, the moisture-proof and anti-caking β-aminoisobutyric acid comprises, by weight, 80%-92.8% β-aminoisobutyric acid; 5-11% one or more of ethyl cellulose, lactose, and resistant dextrin; 2-3% one or more of hydroxypropyl methylcellulose and povidone, or 0.2% sodium carboxymethyl cellulose; and 1-3% one or more of magnesium stearate, calcium hydrogen phosphate, and micronized silica gel.

[0009] In some embodiments, the moisture-proof and anti-caking β-aminoisobutyric acid comprises, by weight, 80-90% β-aminoisobutyric acid; 5-11% ethylcellulose; 2-3% one or more of hypromellose and povidone; and 1-3% one or more of magnesium stearate, calcium hydrogen phosphate, and micronized silica gel. In some embodiments, the moisture-proof and anti-caking β-aminoisobutyric acid comprises, by weight, 82.5-90% β-aminoisobutyric acid; 5-10% ethylcellulose; 2% hypromellose; and 1-3% one or more of magnesium stearate, calcium hydrogen phosphate, and micronized silica gel.

[0010] In some embodiments, the moisture-resistant and anti-caking β-aminoisobutyric acid is in granular or powdered form.

[0011] In some embodiments, the moisture-proof and anti-caking β-aminoisobutyric acid is prepared as a solid preparation or a liquid preparation.

[0012] In some embodiments, the moisture-resistant and anti-caking β-aminoisobutyric acid is formulated into a nutritional supplement, food, beverage, or animal feed.

[0013] On the other hand, the present invention provides a method for preparing moisture-proof and anti-caking β-aminoisobutyric acid, which comprises the following steps: dispersing β-aminoisobutyric acid and one or more of ethyl cellulose, lactose, resistant dextrin, hydroxypropyl methylcellulose, povidone, sodium carboxymethyl cellulose, magnesium stearate, calcium hydrogen phosphate, and micropowdered silica gel in water; and drying the resulting mixture to obtain moisture-proof and anti-caking β-aminoisobutyric acid.

[0014] In some embodiments, the drying is spray drying.

[0015] In some embodiments, the method further comprises passing through a 20-60 mesh screen after spray drying.

[0016] In some embodiments, the method further comprises adding one or more of magnesium stearate, calcium hydrogen phosphate, and micronized silica gel after spray drying.

[0017] In some embodiments, the dispersion is a shear dispersion. In some embodiments, the water is pure water.

[0018] In some embodiments, the prepared moisture-proof and anti-caking β-aminoisobutyric acid comprises 80%-90% by weight of β-aminoisobutyric acid; 5-11% of one or more of ethyl cellulose, lactose, and resistant dextrin; 2-3% of one or more of hydroxypropyl methylcellulose and povidone; and 1-3% of one or more of magnesium stearate, calcium hydrogen phosphate, and micro-powdered silica gel.

[0019] In some embodiments, the moisture-proof and anti-caking β-aminoisobutyric acid prepared by the method is used to prepare food, beverages, nutritional products, skin care products or cosmetics.

[0020] This Summary is provided to introduce a selection of concepts in a simplified form that are further described below in the Detailed Description. This Summary is not intended to identify key features or essential features of the claimed subject matter, nor is it intended to be used to limit the scope of the claimed subject matter. DETAILED DESCRIPTION

[0021] The preferred embodiments of the present invention will now be described in detail with reference to the embodiments thereof. Although the present invention will be described in conjunction with the preferred embodiments, it should be understood that they are not intended to limit the present invention to these embodiments. On the contrary, the present invention is intended to cover substitutions, modifications and equivalents, which may be included within the spirit and scope of the present invention as defined in the claims.

[0022] As used herein, the term "or" is intended to include "and" and "or." In other words, the term "or" can also be replaced with "and / or."

[0023] As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.

[0024] As used herein, the terms "comprising" or "including", or variations thereof, are intended to mean that the terms are used in their non-limiting sense and can include more items than the specific recited item. It also includes the more restrictive verb 'consisting essentially of and 'consisting of.

[0025] The present application is aimed at the need for moisture-proof, combined with process feasibility, moisture-proof effect screening of excipient combination and granulation process; through comparison of moisture-proof performance of multiple batches of samples, accelerated hygroscopicity test verifies the process stability. Process screening: process mode screening, dry granulation, wet granulation, fluidized bed granulation and spray drying are screened, β-amino isobutyric acid has strong hygroscopicity, and a simple and convenient process should be selected, which can avoid the hygroscopicity caused by complicated process, so as to avoid the increase of moisture content of finished product, therefore, finally, according to the operability, economy, representation superiority of product preparation, and wide applicability of prescription process, spray drying is adopted for preparation, which can meet the requirements of: simple process, one-step granulation and drying; large batch production, low cost; relatively uniform particles; good moisture-proof effect and other advantages. Prescription screening: the composite excipient combination is determined by hygroscopicity test, and the excipients such as ethyl cellulose, lactose, dextrin, hydroxypropyl methyl cellulose, sodium carboxymethyl cellulose, povidone, magnesium stearate, calcium hydrogen phosphate, and micro powder silica gel are preferably selected, and the water-proof and anti-caking effect is better. Ethyl cellulose and the like construct the main waterproof layer, hydroxypropyl methyl cellulose and the like fill the micropores, magnesium stearate, calcium hydrogen phosphate, and micro powder silica gel and the like lubricant cover different surface defects, and the moisture-proof and anti-caking effect is realized by the synergistic effect of multiple components.

[0026] In the present application, unless otherwise specified, the scientific and technical terms used herein have the meanings commonly understood by a person skilled in the art. And, the laboratory operation steps used herein are conventional steps widely used in the corresponding field.

[0027] The raw materials or reagents used in the present application are commercially available, unless otherwise specified. All reagents are of commercial grade and are used according to the received standard.

[0028] The following examples are illustrative of selected embodiments of the present application, and are not meant to limit the scope of the application. Example 1

[0029] The moisture-proof and anti-caking β-amino isobutyric acid comprises the following components in weight percentage: β-amino isobutyric acid 90%, ethyl cellulose 5%, hydroxypropyl methyl cellulose 3%, and magnesium stearate 2%.

[0030] Weigh the prescribed amount of β-aminoisobutyric acid, ethyl cellulose, hypromellose, and 1% magnesium stearate into purified water and disperse uniformly by shearing. Dry the suspension in a spray dryer and collect 20-60 mesh granules. Add the remaining 1% magnesium stearate to obtain moisture-proof and anti-caking β-aminoisobutyric acid. Example 2

[0031] The moisture-proof and anti-caking beta-aminoisobutyric acid comprises the following components in percentage by weight: 90% beta-aminoisobutyric acid, 5% lactose, 3% hypromellose, and 2% magnesium stearate.

[0032] Weigh the prescribed amount of β-aminoisobutyric acid, lactose, hypromellose, and 1% magnesium stearate into purified water and disperse uniformly by shearing. Dry the suspension in a spray dryer and collect 20-60 mesh granules. Add the remaining 1% magnesium stearate to obtain moisture-proof and anti-caking β-aminoisobutyric acid. Example 3

[0033] The moisture-proof and anti-caking beta-aminoisobutyric acid comprises the following components in percentage by weight: 90% beta-aminoisobutyric acid, 5% resistant dextrin, 3% hypromellose, and 2% magnesium stearate.

[0034] Weigh the prescribed amount of β-aminoisobutyric acid, resistant dextrin, hypromellose, and 1% magnesium stearate into purified water and disperse by shear until uniform. Spray dry the suspension in a spray dryer and collect 20-60 mesh granules. Add the remaining 1% magnesium stearate to obtain moisture-proof and anti-caking β-aminoisobutyric acid. Example 4

[0035] The moisture-proof and anti-caking beta-aminoisobutyric acid comprises the following components in percentage by weight: 92.8% beta-aminoisobutyric acid, 5% ethyl cellulose, 0.2% sodium carboxymethyl cellulose, and 2% magnesium stearate.

[0036] Weigh the prescribed amount of β-aminoisobutyric acid, ethyl cellulose, sodium carboxymethyl cellulose, and 1% magnesium stearate into purified water and disperse uniformly by shearing. Dry the suspension in a spray dryer and collect 20-60 mesh granules. Add the remaining 1% magnesium stearate to obtain moisture-proof and anti-caking β-aminoisobutyric acid. Example 5

[0037] The moisture-proof and anti-caking beta-aminoisobutyric acid comprises the following components in percentage by weight: 90% beta-aminoisobutyric acid, 5% ethyl cellulose, 3% povidone, and 2% magnesium stearate.

[0038] Weigh the prescribed amount of β-amino isobutyric acid, ethyl cellulose, povidone and 1% magnesium stearate into purified water, shear dispersion to uniformity. The suspension into the spray dryer spray dry, collect 20-60 mesh particles. Add the remaining prescription amount of 1% magnesium stearate to get the moisture-proof anti-caking β-amino isobutyric acid. Example 6

[0039] Moisture-proof anti-caking β-amino isobutyric acid includes the following weight percentage of components: β-amino isobutyric acid 90%, ethyl cellulose 5%, hydroxypropyl methyl cellulose 3%, calcium hydrogen phosphate 2%.

[0040] Weigh the prescribed amount of β-amino isobutyric acid, ethyl cellulose, hydroxypropyl methyl cellulose and 1% calcium hydrogen phosphate into purified water, shear dispersion to uniformity. The suspension into the spray dryer spray dry, collect 20-60 mesh particles. Add the remaining prescription amount of 1% calcium hydrogen phosphate to get the moisture-proof anti-caking β-amino isobutyric acid. Example 7

[0041] Moisture-proof anti-caking β-amino isobutyric acid includes the following weight percentage of components: β-amino isobutyric acid 90%, ethyl cellulose 5%, hydroxypropyl methyl cellulose 3%, micro-silica gel 2%.

[0042] Weigh the prescribed amount of β-amino isobutyric acid, ethyl cellulose, hydroxypropyl methyl cellulose and 1% micro-silica gel into purified water, shear dispersion to uniformity. The suspension into the spray dryer spray dry, collect 20-60 mesh particles. Add the remaining prescription amount of 1% micro-silica gel to get the moisture-proof anti-caking β-amino isobutyric acid. Example 8

[0043] Moisture-proof anti-caking β-amino isobutyric acid includes the following weight percentage of components: β-amino isobutyric acid 90%, ethyl cellulose 5%, hydroxypropyl methyl cellulose 2%, magnesium stearate 1%, calcium hydrogen phosphate 1%, micro-silica gel 1%.

[0044] Weigh the prescribed amount of β-amino isobutyric acid, ethyl cellulose, hydroxypropyl methyl cellulose, calcium hydrogen phosphate and micro-silica gel into purified water, shear dispersion to uniformity. The suspension into the spray dryer spray dry, collect 20-60 mesh particles. Add the remaining prescription amount of 1% magnesium stearate to get the moisture-proof anti-caking β-amino isobutyric acid. Example 9

[0045] Moisture-proof anti-caking β-amino isobutyric acid includes the following weight percentage of components: β-amino isobutyric acid 87.5%, ethyl cellulose 7%, hydroxypropyl methyl cellulose 2%, magnesium stearate 1%, calcium hydrogen phosphate 1%, micro-silica gel 1.5%.

[0046] Weigh the prescribed amount of β-aminoisobutyric acid, ethyl cellulose, hypromellose, calcium hydrogen phosphate, and micronized silica gel in purified water and disperse by shear until uniform. Spray dry the suspension in a spray dryer to collect 20-60 mesh granules. Add the remaining 1% magnesium stearate to obtain moisture-proof and anti-caking β-aminoisobutyric acid. Example 10

[0047] The moisture-proof and anti-caking beta-aminoisobutyric acid comprises the following components in percentage by weight: 85% beta-aminoisobutyric acid, 8% ethyl cellulose, 2% hypromellose, 1% magnesium stearate, 2% calcium hydrogen phosphate, and 2% micro powder silica gel.

[0048] Weigh the prescribed amount of β-aminoisobutyric acid, ethyl cellulose, hypromellose, calcium hydrogen phosphate, and micronized silica gel in purified water and disperse by shear until uniform. Spray dry the suspension in a spray dryer to collect 20-60 mesh granules. Add the remaining 1% magnesium stearate to obtain moisture-proof and anti-caking β-aminoisobutyric acid. Example 11

[0049] The moisture-proof and anti-caking beta-aminoisobutyric acid comprises the following components in percentage by weight: 82.5% beta-aminoisobutyric acid, 10% ethyl cellulose, 2% hypromellose, 1.5% magnesium stearate, 2% calcium hydrogen phosphate, and 2% micro powder silica gel.

[0050] Weigh the prescribed amount of β-aminoisobutyric acid, ethyl cellulose, hypromellose, calcium hydrogen phosphate, and micronized silica gel in purified water and disperse uniformly by shearing. Dry the suspension in a spray dryer and collect 20-60 mesh granules. Add the remaining 1.5% magnesium stearate to obtain moisture-proof and anti-caking β-aminoisobutyric acid. Example 12

[0051] The moisture-proof and anti-caking beta-aminoisobutyric acid comprises the following components in percentage by weight: 80% beta-aminoisobutyric acid, 11% ethyl cellulose, 2% hypromellose, 2% magnesium stearate, 3% calcium hydrogen phosphate, and 2% micro powder silica gel.

[0052] Weigh the prescribed amount of β-aminoisobutyric acid, ethyl cellulose, hypromellose, calcium hydrogen phosphate, and micronized silica gel in purified water and disperse by shear until uniform. Dry the suspension in a spray dryer and collect 20-60 mesh granules. Add the remaining 2% magnesium stearate to obtain moisture-proof and anti-caking β-aminoisobutyric acid. Example 13 Investigation of moisture-proof and anti-caking properties

[0053] Take a dry weighing dish (outer diameter 50 mm, height 100 mm), take the test sample and place it in the above weighing dish, and place it in a 30℃ / 65% RH stability box. Every time interval (10 min, 30 min, 60 min, 120 min), take out the weighing dish. According to the calculation formula: The 20-mesh particle pass rate was calculated. The test results of the moisture-proof and anti-caking β-amino isobutyric acid sample are shown in Table 1. Table 1

[0054] As shown in Table 1, the moisture-proof and anti-caking β-amino isobutyric acid of the present application has a high load of not less than 90.0%, and its moisture-proof and anti-caking performance is excellent under accelerated 30℃ / 65% RH conditions compared with the raw material and the commercial competitor (79.0% load). The 20-mesh sieve pass rate of Example 8 after 120 min of sampling is even more than 70%. The moisture-proof and anti-caking performance is excellent under accelerated 30℃ / 65% RH conditions compared with the raw material and the commercial competitor while having a high load of not less than 80.0%. The 20-mesh sieve pass rate of Example 12 after 120 min of sampling is as high as more than 85%.

[0055] The embodiments of the present application have been verified to greatly improve the phenomenon of easy caking or easy caking due to moisture of the raw material itself, and the process has considerable cost economy under mass production. The high load can save 30%-50% of material cost, so the added value is high; the process is simplified, one-step molding by spray drying is omitted, multiple links of "granulation-granulation-drying" are omitted, and equipment energy consumption is reduced; and the batch is large, which can also reduce equipment energy consumption.

[0056] The moisture-proof and anti-caking β-amino isobutyric acid of the present application realizes a high content or load that cannot be achieved by the existing moisture-proof and anti-caking β-amino isobutyric acid on the market by adding a combination of specific hydrophobic substrates, adhesives, and anti-caking agents, and through a one-step granulation drying screening technical route. The moisture-proof and anti-caking high load β-amino isobutyric acid of the present application achieves excellent moisture-proof and anti-caking effects, improves the stability of β-amino isobutyric acid, and prolongs the shelf life after strict packaging, which also reflects the improvement of stability. In addition, it brings great convenience to transportation and storage conditions and application scenarios, and brings very high applicability to users. In the formula application, it can greatly improve the stability of the formula, and for the existing solid caking problem, the product of the present application will not caking for a long time in the solid beverage, which is convenient to take and brew, and reflects the convenience and applicability.

[0057] While specific embodiments and examples of the application have been described herein, those skilled in the art will understand that any modification and variations therefrom fall within the principles of the application. The above examples and illustrations are not intended to limit the scope of the application. Any combination of the embodiments of the application, as well as any obvious extension or analogue thereof, are within the scope of the application. Furthermore, the application encompasses any arrangement which is intended to achieve the same purpose, as well as all such variations and modifications falling within the scope of the appended claims.

Claims

1. A moisture-proof and anti-caking β-aminoisobutyric acid, characterized in that: The moisture-proof and anti-caking β-aminoisobutyric acid comprises 80%-98% of β-aminoisobutyric acid by weight; and 0.1-15% of one or more of ethyl cellulose, lactose, resistant dextrin, hydroxypropyl methylcellulose, povidone, sodium carboxymethyl cellulose, magnesium stearate, calcium hydrogen phosphate, and micro-powder silica gel.

2. The moisture-proof and anti-caking β-aminoisobutyric acid according to claim 1, characterized in that The moisture-proof and anti-caking β-aminoisobutyric acid comprises, by weight, 80%-98% of β-aminoisobutyric acid; 1-11% of one or more of ethyl cellulose, lactose, and resistant dextrin; 0.1-5% of one or more of hydroxypropyl methylcellulose, povidone, and sodium carboxymethyl cellulose; and 0.5-5% of one or more of magnesium stearate, calcium hydrogen phosphate, and micropowdered silica gel.

3. The moisture-proof and anti-caking β-aminoisobutyric acid according to claim 1, characterized in that The moisture-proof and anti-caking β-aminoisobutyric acid comprises, by weight, 80%-93% of β-aminoisobutyric acid; 3-11% of one or more of ethyl cellulose, lactose, and resistant dextrin; 0.2-4% of one or more of hydroxypropyl methylcellulose, povidone, and sodium carboxymethyl cellulose; and 1-4% of one or more of magnesium stearate, calcium hydrogen phosphate, and micropowder silica gel.

4. The moisture-proof and anti-caking β-aminoisobutyric acid according to claim 1, characterized in that The moisture-proof and anti-caking β-aminoisobutyric acid comprises, by weight, 80%-90% of β-aminoisobutyric acid; 5-11% of one or more of ethyl cellulose, lactose, and resistant dextrin; 2-3% of one or more of hydroxypropyl methylcellulose and povidone; and 1-3% of one or more of magnesium stearate, calcium hydrogen phosphate, and micropowder silica gel.

5. The moisture-proof and anti-caking β-aminoisobutyric acid according to any one of claims 1 to 4, characterized in that The moisture-proof and anti-caking β-aminoisobutyric acid is in the form of granules or powder.

6. A method for preparing moisture-proof and anti-caking β-aminoisobutyric acid, characterized in that: The method comprises the following steps: dispersing beta-aminoisobutyric acid and one or more of ethyl cellulose, lactose, resistant dextrin, hydroxypropyl methylcellulose, povidone, sodium carboxymethyl cellulose, magnesium stearate, calcium hydrogen phosphate, and micropowdered silica gel in water; and drying the obtained mixture to obtain the moisture-proof and anti-caking beta-aminoisobutyric acid.

7. The method according to claim 6, characterized in that The drying is spray drying.

8. The method according to claim 6 or 7, characterized in that The method further comprises passing the product through a 20-60 mesh sieve after spray drying.

9. The method according to any one of claims 6 to 8, characterized in that The method further comprises adding one or more of magnesium stearate, calcium hydrogen phosphate, and micro-powdered silica gel after spray drying.

10. The method according to any one of claims 6 to 9, characterized in that The moisture-proof and anti-caking β-aminoisobutyric acid comprises, by weight, 80%-90% of β-aminoisobutyric acid; 5-11% of one or more of ethyl cellulose, lactose, and resistant dextrin; 2-3% of one or more of hydroxypropyl methylcellulose and povidone; and 1-3% of one or more of magnesium stearate, calcium hydrogen phosphate, and micropowder silica gel.

Images