5'-guanosine-disodium phosphate crystallizing method

A technology of disodium guanosine monophosphate and crystallization, which is applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc. The effect of stable crystal form, promoting crystal transformation and improving product quality

Inactive Publication Date: 2010-02-24
SOUTH CHINA UNIV OF TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The highest yield of the product through this process can reach more than 90%, but the reproducibility is not high, there is a certain amount of amorphous crystals in the crystal form, and some carbonate groups remain
[0007] Japan JP 46015668 proposes to use ethylene glycol, methanol and other solvents as anti-solvents (accounting for 60-90% of the total volume) to cool down at a rate of 2-3°C per hour, and the time to obtain the final crystal is greater than 10hr, which leads to too long time for the process and is not suitable for industrialization
[0008] South Korea KR 9500259 proposes to use 25-30% 5'-guanosine monophosphate aqueous solution with a pH value of 8.4-8.6, and use methanol or ethanol as anti-solvent (volume ratio is 37-40%), and add a small amount of seed crystals at the same time. The crystal form is stable, but the concentration of disodium 5'-guanosine monophosphate in the solution is slightly higher, the crystal is prone to explosive nucleation, and the operation is difficult to control

Method used

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  • 5'-guanosine-disodium phosphate crystallizing method
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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] The crude product of disodium 5'-guanosine monophosphate used in the examples of the present invention is produced by Guangdong Zhaoqing Xinghu Biotechnology Co., Ltd., wherein the content of disodium 5'-guanosine monophosphate is about 70%.

[0036] Weigh 150g of crude 5'-guanosine monophosphate disodium to configure a 15% aqueous solution by weight, add 7.5g of activated carbon and 1.5g of sodium hydrosulfite, react at 45°C for 30 minutes, and filter to obtain 950mL of filtrate.

[0037] Add sodium nitrate twice the mass of the crude 5'-guanosine monophosphate disodium, stir and add NaOH to adjust the pH to 10.50; control the stirring speed at 500 rpm, add 1.425L of anti-solvent methanol at one time, and heat to 50°C , and keep warm for 1.0h; adjust the stirring rate to 100 rpm, with the function T = 50 - 3 × sin ( t 7 ) ...

Embodiment 2

[0046] Weigh 50g crude disodium 5'-guanosine monophosphate to prepare a 5wt% aqueous solution, add 2.5g activated carbon and 0.5g sodium hydrosulfite, react at 45°C for 30 minutes, and filter to obtain 981mL filtrate.

[0047] Add sodium formate 0.2 times the mass of the crude product of 5'-guanosine monophosphate disodium, stir and add NaOH to adjust the pH to 9.49; control the stirring speed at 300 rpm, add 2.943 L of anti-solvent methanol at one time, and raise the temperature to 60 ℃, and keep warm for 0.5h; adjust the stirring rate to 300 rpm, with the function T = 60 - 3 × sin ( t 7 ) - 0.27 × t The determined temperature is the cooling temperature, and cooling crystallization is carried out. T is the temperature, and t is the cooling time. The total cooling time is 360 minutes...

Embodiment 3

[0049] Weigh 200g of crude 5'-guanosine monophosphate disodium to prepare a 20wt% aqueous solution, add 10g of activated carbon and 2g of hydrosulfite, react at 45°C for 30 minutes, and filter to obtain 933mL of filtrate.

[0050] Add sodium nitrate 1.0 times the mass of the crude 5'-guanosine monophosphate disodium, stir and add NaOH to adjust the pH to 8.50; control the stirring speed at 800 rpm, add 280 mL of anti-solvent ethanol at one time, and raise the temperature to 55 ℃, the stirring rate was controlled at 150 rpm, and kept warm for 0.6h; the stirring rate was adjusted to 50 rpm, and the function T = 55 - 3 × sin ( t 7 ) - 0.27 × t Carry out cooling crystallization, the cooling time is 120 minutes, and after cooling to about 10°C, the crystal slurry is separated by suction f...

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Abstract

The invention discloses a 5'-guanosine-disodium phosphate crystallizing method comprising the following steps: adding sodium salt which is 0.2-2 times of 5'-guanosine-disodium phosphate and desolvation with a volume being 0.3-3 times of that of a 5'-guanosine-disodium phosphate solution into a 5'-guanosine-disodium phosphate crude product water solution with concentration of 5-20 percent by weight; controlling the crystallizing temperature of 10-60 DEG C; controlling the mixing rotating speed of 50-300r / min; and after the crystallization is completed, filtering and drying the solution to obtain a 5'-guanosine-disodium phosphate crystal. Due to the adoption of the method, the product quality of the obtained 5'-guanosine-disodium phosphate crystal reaches the national standard, and the 5'-guanosine-disodium phosphate crystal with a stable crystal grain diameter range can be obtained by controlling a crystallizing technical condition and a flow field state. The 5'-guanosine-disodium phosphate crystallizing method has simple operation, good repeatability and shorter crystallizing time and is suitable for the industrial production of the 5'-guanosine-disodium phosphate product.

Description

technical field [0001] The invention belongs to the technical field of crystallization in chemical product engineering, in particular to a crystallization method of disodium 5'-guanosine monophosphate. Background technique [0002] Disodium 5'-guanosine monophosphate (hereinafter referred to as disodium 5'-guanosine monophosphate) has high biological activity, can enhance the immune function of the body, regulate the overall nutrition and metabolic balance of the human body, and promote the growth and development of the body. Antitumor bioregulatory effects. The umami taste intensity of 5'-guanosine disodium monophosphate is 2.3 times that of sodium sarcosinate, and it has a strong synergistic effect when combined with sodium glutamate, which can enhance the umami taste by 10-20 times; at the same time, 5'-guanosine Disodium monophosphate has a synergistic effect on sweetness and meaty taste, and has an inhibitory effect on salty, sour, bitter, fishy and burnt tastes. At p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H19/20C07H1/06
Inventor 江燕斌李鋆郑明英朱义福饶汗生
Owner SOUTH CHINA UNIV OF TECH
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