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Method for preparing 5'-disodium guanylate

A technology of disodium guanylate and guanylate, which is applied in the fields of food and medicine to achieve the effects of a simple preparation method, reduced pollution and a simple post-processing process

Active Publication Date: 2012-08-15
STAR LAKE BIOSCI CO INC ZHAOQING GUANGDONG
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In view of the above-mentioned shortcomings, the technical problem to be solved by the present invention is to simplify the complicated process in the past, reduce process pollution and improve product quality

Method used

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  • Method for preparing 5'-disodium guanylate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0016] Stir 54g of sodium guanylate and 480mL of triethyl phosphate to cool down to 0°C, then slowly add 35mL of phosphorus oxychloride dropwise, and then react at 0°C for 4 hours.

[0017] Freeze 350mL of water to 0°C, then add the above-mentioned guanosine 5'-phosphorylation reaction solution in a continuous flow, and the continuous addition is completed in about 1 hour, and the stirring is continued for 0.5 hours.

[0018] Then slowly feed ammonia gas into the hydrolyzate, control the temperature of the solution at 0-5° C., stop feeding ammonia gas when the pH value is 9.4, and continue stirring for 1 hour. Then let it stand for 10 minutes, and separate the lower aqueous phase layer.

[0019] Then the aqueous phase layer was adjusted to pH 3.0 with hydrochloric acid, stirred at 0°C for 1 hour, and filtered to obtain 5'-guanylic acid.

[0020] The wet product was stirred and dispersed with 360 mL of water, and the pH value was adjusted to 8.0 with caustic soda, and the temp...

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Abstract

The invention discloses a method for preparing 5'-disodium guanylate. The method comprises the following steps of: A, performing 5'-phosphorylation reaction by taking guanosine sodium salt and triethyl phosphate serving as raw materials; B, hydrolyzing phosphorylation reaction solution obtained in the step A in ice water to obtain hydrolyzate containing 5'-guanylate; C, adjusting the pH value of the hydrolyzate of the step B to be 9.0 to 10.0 with ammonium to obtain aqueous solution of the 5'-guanylate; D, standing aqueous solution of the step C and naturally demixing, and adjusting the pH value of a water phase layer of a lower layer to be 3.0+ / -0.5 with hydrochloric acid to obtain mixed solution containing a large amount of 5'-guanylate precipitate; E, separating the mixed solution of the step D to obtain a wet product of the 5'-guanylate; and F, dissolving the wet product of the 5'-guanylate of the step E in water, adjusting the pH value to be 8.0+ / -0.5 with sodium hydroxide, flowing 95 percent ethanol and crystallizing to obtain the 5'-disodium guanylate. The preparation method is simple and has light pollution.

Description

technical field [0001] The invention relates to the technical fields of food and medicine, in particular to a simple and easy preparation process of disodium 5'-guanylate. Background technique [0002] Disodium 5'-guanylate is a powerful freshness enhancer, which can be widely used in special fresh monosodium glutamate, chicken essence, special fresh soy sauce and other seasonings; in addition, disodium 5'-guanylate can also be used as an additive for infant milk powder . Over the years, its preparation process has been continuously developed, and the review is as follows: [0003] 1. Perform 5'-phosphorylation reaction of guanosine and POCL3 in DMF, DMSO, or acetonitrile in the presence of basic media such as pyridine and triethylamine. The reaction solution is hydrolyzed with water, then ① adjust the hydrolyzed solution to an appropriate pH value, then adsorb it with an activated carbon column, and elute it with lye; or extract triethyl phosphate with a water-insoluble o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H19/20C07H1/02
Inventor 龚美义郑明英陈武陈烘光黄永嫦崔锦栋杨艳庆
Owner STAR LAKE BIOSCI CO INC ZHAOQING GUANGDONG
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