A method for preparing adenylic acid crystals based on isoelectric dissolution coupling

An adenosine and crystal technology, which is applied in the field of medicine, can solve the problems of difficult drying, easy aggregation, and unclean removal, and achieves the effects of easy control of conditions, simple operation and complete shape.

Active Publication Date: 2016-03-16
天津普恒康泰科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The melting point of adenylic acid is 178-185°C, and it is usually white or off-white crystalline powder, but the particle size of adenosine produced in industry is relatively small, easy to aggregate, difficult to centrifuge (centrifuge separation), entrained salt impurities in the mother liquor It may not be removed cleanly, it is easy to preserve impurities, and it is difficult to dry, resulting in too fine particles of the finished product, showing a fine powder, which will fail the UV content test, which greatly reduces the use and economic value of adenosine acid products. [1,2]

Method used

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  • A method for preparing adenylic acid crystals based on isoelectric dissolution coupling
  • A method for preparing adenylic acid crystals based on isoelectric dissolution coupling

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Embodiment 1

[0025] A method for preparing adenylic acid crystals based on isoelectric dissolution coupling, comprising the following steps:

[0026] (1) Weigh 10 g of crude adenylic acid, measure 50 mL of water, stir and mix in a jacketed crystallizer, heat in a water bath to control the temperature at 40 ° C, and stir and mix for 20 minutes to obtain a suspension;

[0027] (2) Slowly add an aqueous NaOH solution with a mass concentration of 15% to the suspension to adjust the pH value to 8.50, then slowly add dropwise an aqueous HCl solution with a mass concentration of 10% to adjust the pH value to 4.0;

[0028] (3) Add the solution obtained in step (2) into the reactor at a stirring speed of 250 rpm, add adenylic acid seed crystals with a mass of 1% of the crude adenylic acid product and a particle size of 5 μm, and grow the crystals for 30 minutes;

[0029] (4) control stirring speed is 250rpm, while stirring, dripping volume concentration is the ethanol aqueous solution of 95%, the a...

Embodiment 2

[0030] A method for preparing adenylic acid crystals based on isoelectric dissolution coupling, comprising the following steps:

[0031] (1) Weigh 10 g of crude adenylic acid, measure 70 mL of water, stir and mix in a jacketed crystallizer, heat in a water bath to control the temperature at 45 ° C, stir and mix for 15 minutes to obtain a suspension;

[0032] (2) Slowly add an aqueous NaOH solution with a mass concentration of 20% to the suspension to adjust the pH value to 7.50, then slowly add dropwise an aqueous HCl solution with a mass concentration of 20% to adjust the pH value to 3.9;

[0033] (3) Add the solution obtained in step (2) into the reactor at a stirring speed of 200 rpm, add adenylic acid seed crystals with a mass of 0.5% of the crude adenylic acid product and a particle size of 10 μm, and grow the crystals for 30 minutes;

[0034] (4) control stirring speed is 200rpm, while stirring, dripping volume concentration is the ethanol aqueous solution of 90%, the ad...

Embodiment 3

[0035] A method for preparing adenylic acid crystals based on isoelectric dissolution coupling, comprising the following steps:

[0036] (1) Weigh 10g of crude adenylic acid, measure 60mL of water, stir and mix in a jacketed crystallizer, heat in a water bath to control the temperature at 40°C, stir and mix for 20min to obtain a suspension;

[0037] (2) Slowly add an aqueous NaOH solution with a mass concentration of 15% to the suspension to adjust the pH value to 8.0, then slowly add dropwise an aqueous HCl solution with a mass concentration of 20% to adjust the pH value to 4.0;

[0038] (3) Add the solution obtained in step (2) into the reactor at a stirring speed of 200 rpm, add adenylic acid seed crystals with a mass of 1% of the crude adenylic acid product and a particle size of 5 μm, and grow the crystals for 30 minutes;

[0039] (4) control stirring speed is 250rpm, while stirring, dripping volume concentration is the ethanol aqueous solution of 90%, the add-on of descr...

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Abstract

The invention discloses a method for preparing an adenylic acid crystal based on isoelectric eluting and coupling. The method comprises the following steps: (1) mixing an adenylic acid crude product and water, so as to obtain a suspension; (2) adding an aqueous liquid of NaOH into the suspension until the pH value is 7.50-9.50, and then, adding an aqueous liquid of HCl until the pH value is 3.9-4.5, so as to obtain a liquid; (3) adding the liquid obtained in the step (2) into a reactor while stirring, adding an adenylic acid seed crystal, and growing crystal; and (4) controlling the stirring speed, dropwise adding an ethanol water liquid with the volumetric concentration of 90-95% while stirring, controlling the dropwise adding time to 3-5 hours, carrying out suction filtration, and drying, thereby obtaining the adenylic acid crystal product. The adenylic acid crystal prepared by the method disclosed by the invention is large in grain size and complete in morphology, the operation is simple, the conditions are easily controlled, the cycle for obtaining the product is short, the purity is high, and the application requirements of the fields of medicine, biochemistry and food are met.

Description

technical field [0001] The invention relates to a method for preparing adenylic acid crystals based on isoelectric dissolution coupling, which belongs to the field of adenylic acid production in the fields of medicine, biochemistry and food. Background technique [0002] Adenosine is one of the four main mononucleotides that make up animal cell ribose, an energy transfer substance in the body, but it is more stable than adenosine triphosphate (ATP). It is clinically used for disseminated sclerosis, porphyria, itching, liver disease, and varicose ulcer complications. It has significant peripheral vasodilation and antihypertensive effects. Adenosine is an ingestible substance that can be used as a nucleic acid production Drug intermediates, health food and biochemical reagents, and used in the manufacture of adenosine triphosphate, cyclic adenosine acid, etc. [1] . The melting point of adenylic acid is 178-185°C, and it is usually white or off-white crystalline powder, but t...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): C07H19/20C07H1/06
Inventor王占忠卫宏远
Owner天津普恒康泰科技有限公司