Preparation method and application of magnesium glycinate particles

Abstract

The invention discloses a preparation method and application of magnesium glycinate granules, and relates to the technical field of magnesium glycinate granule preparation.The preparation method comprises the steps that povidone and polyvinyl alcohol are adopted as adhesives for wet granulation, the polyvinyl alcohol is prepared into slurry with the concentration of 10%, magnesium glycinate and povidone are put into a wet granulator to be evenly mixed, and the magnesium glycinate granules are obtained; and adding polyvinyl alcohol slurry with the concentration of 10% to prepare slurry, performing wet granulation, putting the prepared granules into a drying machine, performing boiling drying, and finishing the dried granules through a screen, thereby obtaining the finished product magnesium glycinate granules. By optimizing the use of the adhesive, the Maillard reaction of magnesium glycinate in the storage and shelf life is effectively avoided, the stability and appearance of the product are kept, and the quality and market competitiveness of the product are improved; by adopting the magnesium glycinate particles provided by the invention, the compressibility is obviously improved, the pressed tablets are high in strength, and the magnesium glycinate particles can be produced on a large scale.

Description

Technical Field

[0001] The present invention relates to the technical field of the preparation of magnesium glycinate granules, and particularly relates to a preparation method and application of magnesium glycinate granules. Background Art

[0002] Magnesium glycinate, with the molecular formula Mg(C2H4NO2)2·H2O and a molecular weight of 190.44, is a white powder that is soluble in water and insoluble in ethanol. Magnesium glycinate is a common organic magnesium salt and is widely used in the food, beverage, and pharmaceutical industries as a buffer, stabilizer, and flavoring agent. It is also used in the production of some drugs, such as antibiotics and antiviral drugs.

[0003] Magnesium glycinate has various functions in the body, including participating in protein synthesis, regulating neurotransmitters, protecting the heart, and maintaining bone health. Magnesium glycinate forms soluble compounds with magnesium ions in the body, increasing the body's absorption and utilization of magnesium. Magnesium is an important cofactor for various enzymatic reactions, participating in processes such as protein synthesis and nerve conduction, and playing a key role in maintaining normal physiological functions. When the body lacks magnesium, symptoms such as muscle spasms and fatigue may occur; excessive intake may cause digestive discomfort such as diarrhea and nausea. These symptoms may vary among individuals.

[0004] The functions and effects of magnesium glycinate contribute to carbohydrate metabolism in the body, and at the same time, the magnesium element contained in it can increase the sensitivity of insulin, thereby reducing the risk of diabetes to a certain extent. Secondly, magnesium glycinate can also regulate the state of the brain and has the effect of calming the nerves and helping to sleep. Magnesium glycinate generally needs to be taken under the guidance of a professional doctor. As a dietary supplement, it cannot be used as a therapeutic drug, so it is recommended not to take it for a long time. If you feel unwell after taking it, it is recommended to seek medical attention in a timely manner.

[0005] In the prior art, magnesium glycinate is usually directly pressed into tablets or granulated by dry granulation.

[0006] The Chinese patent publication document with the publication number CN109608349A discloses a green preparation method of magnesium glycinate, belonging to the technical field of magnesium supplementation preparations, including the following steps: A. Add glycine and water to a reaction kettle and heat up to dissolve glycine; B. Add magnesium hydroxide when the temperature rises to 83 - 87°C, react for 2 - 3 hours, and then filter to remove insoluble substances to obtain a filtrate; C. Cool the filtrate to room temperature and then filter to obtain wet magnesium glycinate and a circulating mother liquor; D. Vacuum dry the wet magnesium glycinate to obtain the final product magnesium glycinate.

[0007] A Chinese published patent document with the publication number CN113121375A discloses a method for preparing food-grade and feed-grade magnesium glycinate and its implementation device. The method includes contacting a hydantoin glycine crystallization mother liquor with a zirconium raw material in the presence of one or more magnesium compounds such as magnesium oxide, magnesium hydroxide, and magnesium carbonate to carry out hydrolysis and chelation reactions, obtaining an aqueous solution of magnesium glycinate, and subsequently obtaining food-grade magnesium glycinate as a solid precipitate through concentration and cooling crystallization, and co-producing feed-grade magnesium glycinate. The purity of the obtained food-grade magnesium glycinate can reach more than 98.0%, and the recovery rate of glycine reaches more than 99%.

[0008] A Chinese published patent document with the publication number CN113321592A discloses a method for preparing magnesium glycinate. The preparation method includes: pre-treating raw materials glycine and magnesium hydroxide or magnesium oxide; adding the glycine into a solid-phase reactor; adding magnesium hydroxide or magnesium oxide into the solid-phase reactor in three portions according to a molar ratio of 2:(0.6 - 1):(0.08 - 0.4) under a certain environment, including: adding magnesium hydroxide or magnesium oxide with a molar ratio of 2, grinding and reacting for 20 - 40 minutes; adding magnesium hydroxide or magnesium oxide with a molar ratio of (0.6 - 1), grinding and reacting for 50 - 70 minutes; adding magnesium hydroxide or magnesium oxide with a molar ratio of (0.08 - 0.4), grinding and reacting for 30 - 50 minutes; washing the reaction product with ethanol and drying to obtain magnesium glycinate.

[0009] In the above method for preparing magnesium glycinate, there are the following disadvantages: 1) Insufficient compressibility: The compressibility of magnesium glycinate is poor, resulting in insufficient strength of the finished tablets, affecting mass production; 2) Maillard reaction problem: Magnesium glycinate is prone to Maillard reaction during storage and shelf life, resulting in color change, affecting the stability and appearance of the product. Summary of the Invention

[0010] The purpose of the present invention is to provide a method for preparing magnesium glycinate particles with sufficient compressibility, high tablet strength, and not easily discolored, and its application. By adding a suitable binder to carry out wet granulation on magnesium glycinate raw materials, the compressibility of magnesium glycinate is improved, so that the strength of the pressed magnesium glycinate tablets (with a magnesium content of 125 mg) can be coated in large batches (800 kg), improving production efficiency. At the same time, by screening a suitable binder, the problem that magnesium glycinate is prone to Maillard reaction and cause color change during storage, shelf life, and accelerated stability is solved, improving the stability and appearance of the product.

[0011] In order to achieve the above technical purpose and meet the above technical requirements, the technical solution adopted by the present invention is: a method for preparing magnesium glycinate particles, using povidone and polyvinyl alcohol as binders to carry out wet granulation. The preparation method specifically includes the following steps: Step 1: Prepare raw materials magnesium glycinate, povidone, and polyvinyl alcohol and carry out batching; Step 2: Make a 10% concentration slurry of polyvinyl alcohol; put magnesium glycinate and povidone into a wet granulator and mix evenly, add the 10% concentration polyvinyl alcohol slurry for slurry preparation and carry out wet granulation; Step 3: Put the made granules into a dryer for fluidized bed drying until the moisture content of the granules is below 2%; Step 4: Screen the dried granules through a 16-mesh or 20-mesh sieve to obtain the finished magnesium glycinate granules.

[0012] Preferably: The mass ratio of povidone to polyvinyl alcohol is 1:1 to 3:1, preferably 2:1.

[0013] A magnesium glycinate granule is prepared by a preparation method of a magnesium glycinate granule.

[0014] Apply the magnesium glycinate granules to the preparation of Magnesium Glycinate Tablet.

[0015] Carry out stability tests on the prepared magnesium glycinate granules and magnesium glycinate tablets under different storage conditions.

[0016] Storage conditions for the stability test of magnesium glycinate granules: ① Dry the prepared granules at 80°C to constant weight, and there is no color change under high temperature and high humidity conditions; ② Expose the dried granules at 40°C and 75% humidity for 1 month, and there is no color change reaction.

[0017] Storage conditions for the stability test of magnesium glycinate tablets: ① Expose the prepared tablets at 40°C and 75% humidity for 1 month, and there is no color change reaction; ② Put the prepared tablets into an HDPE high-density polyethylene bottle and observe for 6 months at 40°C and 75% humidity, and there is no color change reaction.

[0018] Compared with the traditional structure, the beneficial effects of the present invention: 1. By optimizing the use of binders, the present invention uses povidone and polyvinyl alcohol as binders, effectively avoiding the Maillard reaction of magnesium glycinate during storage and shelf life, not only maintaining the stability and appearance of the product, but also improving the quality and market competitiveness of the product; using the magnesium glycinate granules provided by the present invention, its compressibility is significantly improved, the tablets pressed out have high strength, and large-scale production can be carried out.

[0019] 2. The preparation process of the present invention is simple, the equipment investment is small, and the production cost is low. It not only improves the compressibility of magnesium glycinate, avoids the Maillard reaction, but also maintains the stability and appearance of the product, with obvious advantages. Detailed implementation mode

[0020] Taking magnesium glycinate granules with an active ingredient content of 90.28% as an example, the present invention will be further described below.

[0021] The indexes of 90.28% magnesium glycinate granules are shown in Table 1: Table 1 Indexes of magnesium glycinate granules Item Index Appearance White to off-white granules or granular powder Water content 1.5% - 2.0% (Detection temperature: 105°C) Particle size distribution Less than 10% above 20 mesh, less than 30% below 100 mesh Example 1: Prepare a 10% concentration slurry of polyvinyl alcohol. Put magnesium glycinate and hypromellose (HPMC) into a wet granulator, mix for 5 minutes, and add the slurry - prepared slurry (10% PVA polyvinyl alcohol) for wet granulation; put the prepared granules into a dryer for drying, and screen the dried granules through a 16 - or 20 - mesh sieve.

[0022] The finished product of 90.28% magnesium glycinate granules is off - white granular powder, with a moisture content of 1.81%. After screening, those above 20 - mesh reach 7%, and those below 100 - mesh reach 24%.

[0023] The prepared 90.28% magnesium glycinate granules were subjected to a stability test under different storage conditions. The results showed that the granules using hypromellose (HPMC) and polyvinyl alcohol as binders did not undergo the Maillard reaction during the test and could enter the next tablet - pressing test.

[0024] The 90.28% magnesium glycinate granules were used in the preparation of Magnesium Glycinate Tablets. The formula is shown in Table 2: Table 2 Formula for preparing magnesium glycinate tablets using magnesium glycinate granules Serial number Material name Dosage per 10,000 tablets (g) Dosage ratio (%) 1 Magnesium glycinate granules 90.28% 13095.47 91.385 2 Microcrystalline cellulose 1104.53 7.708 3 Magnesium stearate 80.000 0.558 4 Silicon dioxide 50.000 0.349 Total 14330.00 100.000 The prepared magnesium glycinate tablets were detected using instruments such as a hardness tester and a friability tester. The measured results are shown in Table 3: Table 3 Data of magnesium glycinate tablets prepared using magnesium glycinate granules in Example 1 Serial number Index name Data 1 Average hardness (N) 200N 2 Friability (%) 0.18 3 Disintegration time limit (min, with baffle) 23 4 Weight variation of tablets -0.82%~+0.71% 5 Number of broken tablets in free fall (20 tablets) 0 As can be seen from the above table, the average hardness of the magnesium glycinate tablets prepared from magnesium glycinate granules using hypromellose (HPMC) and polyvinyl alcohol as binders is 200 N, and this product can achieve large - batch coating of 700 kg / batch.

[0025] The prepared magnesium glycinate tablets were subjected to a stability test under different storage conditions. The results showed that the tablets using hypromellose (HPMC) and polyvinyl alcohol as binders did not undergo the Maillard reaction during storage and shelf life, and maintained good stability and appearance.

[0026] Example 2: Prepare a 10% concentration slurry of polyvinyl alcohol. Put magnesium glycinate and methylcellulose (MC) into a wet granulator, mix for 5 minutes, add the slurry - prepared slurry (10% PVA polyvinyl alcohol) for wet granulation. Put the prepared granules into a dryer for drying, and sieve the dried granules through a 16 - or 20 - mesh sieve.

[0027] The finished product of 90.28% magnesium glycinate granules is in white granular form, with a moisture content of 1.78%. After sieving, those above 20 - mesh reach 6%, and those below 100 - mesh reach 25%.

[0028] Perform stability tests on the prepared 90.28% magnesium glycinate granules under different storage conditions. The results show that the granules using methylcellulose (MC) and polyvinyl alcohol as binders did not undergo the Maillard reaction during the test and can enter the next tablet - pressing test.

[0029] Use the 90.28% magnesium glycinate granules to prepare Magnesium Glycinate Tablets. The formula is the same as in Example 1. The index data of the prepared tablets are shown in Table 4: Table 4 Data of Magnesium Glycinate Tablets Prepared from Magnesium Glycinate Granules in Example 2 Serial number Index name Data 1 Average hardness (N) 220N 2 Friability (%) 0.18 3 Disintegration time limit (min, with baffle) 13 4 Weight variation of tablets -0.55%~+0.91% 5 Number of broken tablets in free fall (20 tablets) 0 As can be seen from the above table, the average hardness of the magnesium glycinate tablets prepared from magnesium glycinate granules using methylcellulose (MC) and polyvinyl alcohol as binders is 220 N, and this product can achieve large - batch coating of 770 kg / batch.

[0030] Perform stability tests on the prepared magnesium glycinate tablets under different storage conditions. The results show that the tablets using methylcellulose (MC) and polyvinyl alcohol as binders did not undergo the Maillard reaction during storage and shelf life, and maintained good stability and appearance.

[0031] Example 3: Prepare a 10% concentration slurry of polyvinyl alcohol. Put magnesium glycinate and maltodextrin into a wet granulator, mix for 5 minutes, add the slurry - prepared slurry (10% PVA polyvinyl alcohol) for wet granulation. Put the prepared granules into a dryer for drying, and sieve the dried granules through a 16 - or 20 - mesh sieve.

[0032] The finished product of 90.28% magnesium glycinate granules is in white granular form, with a moisture content of 1.77%. After sieving, those above 20 - mesh reach 5%, and those below 100 - mesh reach 23%.

[0033] Perform stability tests on the prepared 90.28% magnesium glycinate granules under different storage conditions. The results show that the granules using maltodextrin and polyvinyl alcohol as binders changed color slightly during the test, underwent the Maillard reaction, and there is no need to conduct tablet - pressing tests.

[0034] Example 4: Prepare a slurry with a concentration of 10% of polyvinyl alcohol. Put magnesium glycinate and polyvinylpyrrolidone (K30) into a wet granulator, mix for 5 minutes, and add the slurry - prepared slurry (10% PVA polyvinyl alcohol) for wet granulation. Put the prepared granules into a dryer for drying, and sieve the dried granules through a 16 - or 20 - mesh sieve.

[0035] The finished product of 90.28% magnesium glycinate granules obtained is in the form of white granules, with a moisture content of 1.63%. After sieving, those above 20 - mesh reach 4%, and those below 100 - mesh reach 22%.

[0036] Perform stability tests on the prepared 90.28% magnesium glycinate granules under different storage conditions. The results show that the granules using polyvinylpyrrolidone (K30) and polyvinyl alcohol as binders did not undergo the Maillard reaction during the test and can enter the next step of tablet pressing test.

[0037] Use the 90.28% magnesium glycinate granules to prepare Magnesium Glycinate Tablets. The formula is the same as that in Example 1. The index data of the prepared tablets are shown in Table 5: Table 5 Data of Magnesium Glycinate Tablets Prepared from Magnesium Glycinate Granules in Example 4 Serial number Index name Data 1 Average hardness (N) 250N 2 Friability (%) 0.10 3 Disintegration time limit (min, with baffle) 14 4 Weight variation of tablets -0.42%~+0.59% 5 Number of broken tablets in free fall (20 tablets) 0 As can be seen from the above table, the average hardness of the magnesium glycinate tablets prepared from magnesium glycinate granules using polyvinylpyrrolidone and polyvinyl alcohol as binders is 250 N, and this product can achieve large - batch coating of 800 kg / batch.

[0038] Perform stability tests on the prepared magnesium glycinate tablets under different storage conditions. The results show that the tablets using polyvinylpyrrolidone and polyvinyl alcohol as binders did not undergo the Maillard reaction during storage and shelf life, and maintained good stability and appearance.

[0039] Example 5: Prepare a slurry with a concentration of 10% of polyvinyl alcohol. Put magnesium glycinate and copolyvinylpyrrolidone (PVA / A) into a wet granulator, mix for 5 minutes, and add the slurry - prepared slurry (10% PVA polyvinyl alcohol) for wet granulation. Put the prepared granules into a dryer for drying, and sieve the dried granules through a 16 - or 20 - mesh sieve.

[0040] The finished product of 90.28% magnesium glycinate granules obtained is in the form of white granules, with a moisture content of 1.66%. After sieving, those above 20 - mesh reach 6%, and those below 100 - mesh reach 25%.

[0041] The prepared 90.28% magnesium glycinate granules were subjected to stability tests under different storage conditions. The results showed that the granules using copovidone (PVA / A) and polyvinyl alcohol as binders slightly changed color during the test, and the Maillard reaction occurred, making it unnecessary to conduct tableting tests.

[0042] As can be seen from the above Examples 1 - 5, when maltodextrin and copovidone (PVA / A) are used as binders, the magnesium glycinate granules will undergo the Maillard reaction, and these two binders are not suitable for the preparation of magnesium glycinate granules.

[0043] When using polyvinylpyrrolidone (K30), hypromellose (HPMC), methylcellulose (MC), and polyvinyl alcohol (PVA) as binders, the Maillard reaction did not occur during storage and the shelf life, maintaining good stability and appearance, with the best effect.

[0044] As can be seen from Example 4, when using polyvinylpyrrolidone (K30) and polyvinyl alcohol (PVA) as binders, the magnesium glycinate tablets prepared from magnesium glycinate granules have the highest average hardness and the lowest friability. The tablet indexes prepared are better than those of other examples, and large - batch coating of 800 kg / batch can be achieved, greatly improving the production efficiency.

[0045] In summary, through the comparison of production efficiency, the most suitable binders were screened out: polyvinylpyrrolidone and polyvinyl alcohol. Using polyvinylpyrrolidone (K30) and polyvinyl alcohol (PVA) as binders for wet granulation not only improves the compressibility and production efficiency of magnesium glycinate, but also the product does not undergo the Maillard reaction during storage and the shelf life, while maintaining good stability and appearance.

[0046] The above embodiments of the present invention are merely examples clearly illustrating what the present invention does, but are not used to limit the protection scope of the present invention. All equivalent technical solutions also belong to the scope of the present invention. The patent protection scope of the present invention should be defined by each claim.

Claims

1. A method for preparing magnesium glycinate granules, characterized in that: The wet granulation is carried out by using povidone and polyvinyl alcohol as binders, and the preparation method specifically includes the following steps: Step 1: Prepare raw materials magnesium glycinate, povidone, and polyvinyl alcohol and carry out batching; Step 2: Prepare a 10% concentration slurry of polyvinyl alcohol; put magnesium glycinate and povidone into a wet granulator and mix evenly, and add the 10% concentration polyvinyl alcohol slurry for slurry preparation and carry out wet granulation; Step 3: Put the prepared granules into a dryer for drying; Step 4: Screen the dried granules through a 16-mesh or 20-mesh sieve to obtain the finished magnesium glycinate granules.

2. The preparation method of the magnesium glycinate particles according to claim 1, wherein: The drying is fluidized bed drying, and the drying is carried out until the moisture content of the granules is below 2%.

3. A magnesium glycinate granule, characterized in that: It is prepared by the preparation method of the magnesium glycinate granules according to any one of claims 1-2.

4. Use of magnesium glycinate granules, characterized in that: The magnesium glycinate granules according to claim 3 are used for the preparation of magnesium glycinate tablets.