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CN-122010753-A - Glycine chelated magnesium and preparation method thereof

CN122010753ACN 122010753 ACN122010753 ACN 122010753ACN-122010753-A

Abstract

The invention relates to the technical field of nutritional supplements, in particular to glycine chelated magnesium and a preparation method thereof, comprising the steps of raw material preparation, raw material dissolution, chelation reaction, separation, purification, crystallization and drying treatment, according to the method, the organic acid chelating accelerator similar to the glycine in molecular structure is added in the chelating reaction process, the pH value of a reaction system is regulated and controlled in the whole process, and the product is prepared through seed crystal induced crystallization, so that the chelating reaction efficiency and the product purity are effectively improved, the production flow is simplified, and the method is suitable for large-scale production. The invention can efficiently prepare high-purity stable glycine chelated magnesium, has simple and easily controlled process, low production cost and excellent water solubility and bioavailability of the product, and is suitable for application in multiple fields.

Inventors

  • SHI ZHIYONG
  • LIU ZHENGWU
  • WANG HONGHUI

Assignees

  • 宁乡新阳化工有限公司

Dates

Publication Date
20260512
Application Date
20260415

Claims (10)

  1. 1. The preparation method of the glycine chelated magnesium is characterized by comprising the following steps: S1, preparing a raw material, namely respectively weighing glycine and an inorganic magnesium source according to the molar ratio of glycine to magnesium ions in the magnesium source of 2.0:1-2.5:1, and simultaneously weighing a chelating accelerator, wherein the dosage of the chelating accelerator is 0.5-2.0% of the mass of glycine; S2, raw material dissolution, namely adding the weighed glycine into deionized water, stirring until the glycine is completely dissolved to obtain glycine aqueous solution, adding an inorganic magnesium source into the deionized water, stirring to prepare magnesium source slurry, or directly adding the inorganic magnesium source for standby; S3, chelating reaction, namely adding magnesium source slurry into glycine aqueous solution in batches under a stirring state, or directly adding inorganic magnesium source into glycine aqueous solution in batches, synchronously adding all chelating promoters, regulating and controlling the pH value of a reaction system to be 5.5-6.5 in the whole course, heating to 60-80 ℃, and carrying out heat preservation and stirring reaction for 2-4 hours to obtain a chelating reaction solution; s4, separating, purifying and crystallizing, namely filtering the chelation reaction solution while the chelation reaction solution is hot to remove unreacted substances, concentrating the obtained filtrate in vacuum to 1/3-1/5 of the original volume, adding glycine chelated magnesium seed crystals into the concentrated solution, standing for crystallization for 1-2 hours, filtering, and collecting crystal precipitate; s5, drying, namely placing the crystal precipitate into a vacuum drying oven, and drying to obtain a glycine chelated magnesium product; the chelating promoter is an organic acid compound with a molecular structure similar to glycine, and the ionization constant of an aqueous solution of the chelating promoter is 10 -5 ~10 -2 .
  2. 2. The method for preparing glycine chelated magnesium according to claim 1, wherein the inorganic magnesium source in step S1 is one or more of magnesium oxide, magnesium hydroxide, and magnesium carbonate.
  3. 3. The method for preparing glycine chelated magnesium according to claim 1, wherein the molar ratio of glycine to magnesium ions in the magnesium source in step S1 is 2.2:1.
  4. 4. The method for producing glycine chelated magnesium according to claim 1, wherein the chelating accelerator is one or more selected from acetic acid, monochloroacetic acid, and dichloroacetic acid.
  5. 5. The method for preparing glycine chelate magnesium according to claim 1, wherein the amount of the chelate accelerator in the step S1 is 0.5% -1.0% of the mass of glycine.
  6. 6. The method for preparing glycine chelate magnesium according to claim 1, wherein in the step S3, the temperature of the reaction system is raised to 60-70 ℃, and the reaction is carried out for 2-3 hours with stirring and heat preservation.
  7. 7. The method for preparing glycine chelated magnesium according to claim 1, wherein in the step S3, a chelating accelerator is used to synchronously adjust the pH value of the reaction system, and the pH value of the system is maintained within a range of 5.5-6.5 throughout the whole process.
  8. 8. The method for preparing glycine chelated magnesium according to claim 1, wherein the vacuum concentration in step S4 is performed by vacuum concentration and low-temperature evaporation concentration.
  9. 9. The method for preparing glycine chelated magnesium according to claim 1, wherein in the step S5, the temperature of vacuum drying is 50-70 ℃ and the drying time is 4-8 hours.
  10. 10. The glycine chelated magnesium prepared by the preparation method according to any one of claims 1-9, which is characterized in that the glycine chelated magnesium is white flowable crystalline powder, the molecular formula is Mg (C 2 H 4 NO 2 ) 2 ·nH 2 O, wherein n is 0-4, the purity of the product is more than or equal to 98% on a dry basis, the chelation rate is more than or equal to 90%, the mass fraction of magnesium element is 12.5% -13.5%, and the infrared spectrum has characteristic absorption peaks of carboxylate chelation structures at 1575-1641 cm -1 and 1380-1420 cm -1 .

Description

Glycine chelated magnesium and preparation method thereof Technical Field The invention relates to the technical field of nutritional supplements, in particular to glycine chelated magnesium and a preparation method thereof. Background Magnesium is a major mineral element essential for human body, and is widely involved in hundreds of physiological processes of enzymatic reaction, energy metabolism, neuromuscular excitability regulation and control, cell ion balance maintenance, bone mineralization, growth and the like, and is an essential nutrient substance for maintaining normal physiological functions of human body. The traditional factors such as insufficient dietary intake, abnormal physiological metabolism and the like are easy to cause magnesium deficiency of human bodies, and further cause abnormal functions of multiple systems such as nerves, cardiovascular diseases, bones and the like, so that safe and efficient magnesium supplement research and development are research hot spots in the fields of foods and medicines. Most of magnesium supplements sold in the market at present are inorganic magnesium salts such as magnesium oxide, magnesium hydroxide and magnesium carbonate, the products have the problems of poor water solubility, low human body absorption efficiency and insufficient bioavailability, and the products are easy to stimulate gastrointestinal tracts after being orally taken, cause uncomfortable symptoms such as abdominal distension, diarrhea and the like, and have obvious application limitation. The glycine chelated magnesium is used as a third-generation amino acid chelated mineral supplement, and a stable double five-membered ring chelated structure is formed by central magnesium ions and glycine through coordination bonds, so that the glycine chelated magnesium has the advantages of good water solubility, stable chemical property, no gastrointestinal tract irritation, easy absorption and utilization by human bodies and the like, is an ideal magnesium nutrition enhancer, and can be widely applied to multiple fields such as functional foods, health-care products, pharmaceutical preparations and the like. The existing preparation technology of glycine chelated magnesium still has the defects of low chelation reaction efficiency, high content of free glycine and free magnesium ions in the product, insufficient chelation rate, easiness in generating non-chelated double salt, serious influence on the purity and bioavailability of the product, great increase of production cost due to partial process of introducing an organic phase to construct a biphasic reaction system for improving chelation effect, difficulty in realizing large-scale production due to the fact that solvent residue risks and complicated separation and purification processes are brought, and the problems of poor reaction uniformity, high equipment requirement, insufficient product stability and the like in the processes of solid-phase synthesis, microwave assistance and the like are solved, so that the product quality and the production economy cannot be considered, and the large-scale production and market popularization and application of high-quality glycine chelated magnesium are severely restricted. Disclosure of Invention (One) solving the technical problems Aiming at the defects of the prior art, the invention provides glycine chelated magnesium and a preparation method thereof. (II) technical scheme A preparation method of glycine chelated magnesium comprises the following steps: S1, preparing a raw material, namely respectively weighing glycine and an inorganic magnesium source according to the molar ratio of glycine to magnesium ions in the magnesium source of 2.0:1-2.5:1, and simultaneously weighing a chelating accelerator, wherein the dosage of the chelating accelerator is 0.5-2.0% of the mass of glycine; S2, raw material dissolution, namely adding the weighed glycine into deionized water, stirring until the glycine is completely dissolved to obtain glycine aqueous solution, adding an inorganic magnesium source into the deionized water, stirring to prepare magnesium source slurry, or directly adding the inorganic magnesium source for standby; S3, chelating reaction, namely adding magnesium source slurry into glycine aqueous solution in batches under a stirring state, or directly adding inorganic magnesium source into glycine aqueous solution in batches, synchronously adding all chelating promoters, regulating and controlling the pH value of a reaction system to be 5.5-6.5 in the whole course, heating to 60-80 ℃, and carrying out heat preservation and stirring reaction for 2-4 hours to obtain a chelating reaction solution; s4, separating, purifying and crystallizing, namely filtering the chelation reaction solution while the chelation reaction solution is hot to remove unreacted substances, concentrating the obtained filtrate in vacuum to 1/3-1/5 of the original volume, adding glycine chelated magnesium seed cr