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Method for preparing high-bulk-density flavor nucleotides disodium mixed crystal

A technology of disodium nucleotide and density, which is applied in food science and other directions, can solve the problems of not being able to meet the preparation requirements of high-quality umami agents, not strictly controlling crystallization nucleation, and low product bulk density, and achieve a solvent system. Green and friendly, the effect of solving the difficulty of GMP crystallization and simple operation process

Active Publication Date: 2016-04-20
河南斯塔齐生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The initial precipitation of crystals in this method is achieved by continuously adding ethanol to dissolve and crystallize, and the crystallization nucleation is not strictly controlled. The solubility of 5'-flavored nucleotides in pure water system decreases rapidly with the increase of alcohol content, which is easy to cause explosive nucleation. , The product crystal is finely crushed
After cooling down to 20-40°C to precipitate a large number of crystals, raise the temperature of the feed liquid to 65°C to eliminate fine crystals. The disadvantage of this method is that the temperature rise is too large (~35°C), and a lot of energy is consumed.
Since the nucleation of crystallization is not strictly controlled, the subsequent temperature rise to eliminate fine grains cannot solve the fundamental problem of small particle size, and the product crystals are only about 60 μm, see the appendix of its manual Figure 1-5 , the crystal is flaky, the product has low bulk density, poor shape, and easy to agglomerate
Can not well meet the preparation requirements of high-quality flavoring agent

Method used

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  • Method for preparing high-bulk-density flavor nucleotides disodium mixed crystal
  • Method for preparing high-bulk-density flavor nucleotides disodium mixed crystal
  • Method for preparing high-bulk-density flavor nucleotides disodium mixed crystal

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] 1) Take 7.11 g of crude disodium inosinate and 7.89 g of amorphous disodium guanylate, add them to 250 ml of pure water, keep the solution at 25°C, start stirring at 100 rpm to dissolve it. Solid sodium hydroxide was added to adjust the pH of the aqueous I+G solution to 7.5.

[0049] 2) Adjust the stirring to 200rpm, add 75ml of absolute ethanol (V=30%V) within 30min 水 ), after mixing evenly, add 0.075 g of I+G seed crystal (w=0.5% I+G crude product), and grow the crystal for 20 minutes.

[0050] 3) Continue to add 425ml of ethanol dropwise, the time for adding the first 50ml is 2h, and the time for adding the last 375ml is 1h.

[0051] 4) Suction filtration, washing the filter cake with 95% ethanol, and drying at normal temperature and pressure for 1 hour. 12.2 g of the I+G mixed crystal product was obtained with a yield of 80.9%. After measurement, the bulk density of the product is 0.81g / ml. The detection result of the Malvern particle size analyzer is d(50)=360 ...

Embodiment 2

[0054] 1) Take 30.45g of crude disodium inosinate and 32.05g of crude disodium guanylate, add them to 250ml of pure water, keep the solution at 45°C, start stirring at 600rpm to dissolve it. Solid sodium hydroxide was added to adjust the pH of the aqueous I+G solution to 8.5.

[0055] 2) Adjust and stir at 400rpm, add 25ml of anhydrous methanol (V=10%V) within 30min 水 ), after mixing evenly, add 6.25 g of I+G seed crystals (w=0.5% I+G crude product), and grow the crystals for 30 minutes.

[0056] 3) Continue to add 225ml of methanol dropwise, the time for adding the first 150ml is 3h, and the time for adding the last 75ml is 1h.

[0057] 4) Suction filtration, the filter cake was washed with 95% ethanol, and dried at normal temperature and pressure for 3 hours to obtain 64.76 g of I+G mixed crystal product with a yield of 94.2%. After measurement, the bulk density of the product is 0.77g / ml. The detection result of the Malvern particle size analyzer was d(50)=244 μm.

[00...

Embodiment 3

[0060] 1) Take 18.75g of crude disodium inosinate and 18.75g of crude disodium guanylate, add them into 250ml of pure water, keep the solution at 35°C, start stirring at 300rpm to dissolve it. Solid sodium hydroxide was added to adjust the pH of the aqueous I+G solution to 8.0.

[0061] 2) Add 65ml of absolute ethanol (V=26%V) within 30min 水 ), after mixing evenly, add 2.0 g of I+G seed crystals (w=5.3% I+G crude product), and grow the crystals for 30 minutes.

[0062] 3) Continue to add 255ml of ethanol dropwise, the time for adding the first 65ml is 2h, and the time for adding the last 115ml is 2h.

[0063] 4) Suction filtration, the filter cake was washed with 95% ethanol, and dried at normal temperature and pressure for 1 h to obtain 37.95 g of I+G mixed crystal product with a yield of 96.1%. After measurement, the bulk density of the product is 0.86g / ml. The detection result of the Malvern particle size analyzer was d(50)=419 μm.

[0064] The product appearance obtain...

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Abstract

The invention relates to a method for preparing high-bulk-density flavor nucleotides disodium mixed crystal. The method comprises the following steps: adding a flavor nucleotides disodium crude product into water, keeping temperature constant at 25-45 DEG C, stirring and dissolving until clear; adding a certain amount of ethanol, adding I+G seed crystal into a metastable zone, growing crystal and continuously adding ethanol drop by drop at a certain rate; and filtering and washing, drying at normal temperature and at normal pressure for 1-3 h so as to obtain I+G mixed crystal. By adjusting key factors such as seed crystal and elution rate, etc., nucleation and growth of crystal are greatly controlled. The prepared I+G product is rodlike crystal, size distribution is d(50)=200-450 microns, and bulk density is 0.76-0.86 g / ml. The product has good fluidity. The product is applied in the field of food additives. By molecular mixing of IMP and GMP, flavor developing effect of the product is enhanced. The I+G mixed crystal's good form meets international market demand. The production technology is simple and is less time-consuming. By the technology, it is easy to realize industrial production.

Description

technical field [0001] The invention relates to the field of refining food additives, in particular to a method for preparing high-bulk-density taste-flavored nucleotide disodium mixed crystals through solution co-crystallization technology. Background technique [0002] Disodium 5'-ribonucleotide (I+G for short) is disodium 5'-inosinate (IMP for short) and disodium 5'-guanylate (Disodium5'-guanylate , referred to as GMP) crystals or mixtures, which need to be mixed according to the content ratio stipulated by the state (the content of IMP and GMP each accounts for 48.0% to 52.0%). The chemical formula of IMP is C 10 h 11 N 4 Na 2 o 8 P, with a molecular weight of 392.17, is a colorless to white crystal or white crystalline powder, containing about 7.5 molecules of crystal water. GMP chemical formula is C 10 h 12 N 5 Na 2 o 8 P, is a colorless to white crystal or crystalline powder, containing about 7 molecules of crystal water. Both IMP and GMP are nucleotide de...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A23L27/23
Inventor 龚俊波王艳刘增坤尹秋响侯宝红张美景陈巍鲍颖郝红勋王永莉王召谢闯
Owner 河南斯塔齐生物科技有限公司
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