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Preparation method of proline as medicine

A technology of proline and strong acidic cations, which is applied in the field of preparation of medicinal proline, can solve the problems of low boiling point of solvents, easy moisture absorption, unsuitable application and production, etc., and achieve the effect of high purity and good crystal form

Inactive Publication Date: 2018-10-12
WUXI JINGHAI AMINO ACID
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Existing purification methods mainly include ion exchange resin method, anhydrous ethanol recrystallization method, ethanol-ether method, water-ethanol-acetone method, wherein, ion exchange resin method has low yield and low efficiency, and is not suitable for application and production; The water-ethanol recrystallization method cannot remove inorganic salts, and the operation process is easy to absorb moisture, and absolute ethanol is expensive and difficult to recycle; both the ethanol-ether method and the water-ethanol-acetone method have the disadvantages of low solvent boiling point, flammability and difficulty in recycling

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Specific steps are as follows:

[0044] (1) Take 10L of proline fermentation broth, pass through 2L of regenerated 732 resin, and perform adsorption. Determine whether the adsorption is over by measuring whether the adsorption discharge liquid leaks out amino acids. The adsorption rate is 20mL / min, and finally a volume of 5L is obtained. For the adsorption resin, wash away unadsorbed amino acids and some impurities with 6L of water, and elute the adsorption resin with 4% sodium hydroxide to obtain liquid A;

[0045] (2) Put the liquid A in (1) into a decolorization tank for decolorization, the decolorization temperature is 60°C, the decolorization time is 30min, the amount of activated carbon added is 5‰ of the quality of liquid A, the stirring speed is 200r / min, and the activated carbon is removed by filtration. Decolorization was repeated twice to obtain a decolorization solution;

[0046] (3) passing the decolorizing solution in (2) successively through 301 anion re...

Embodiment 2

[0056]Specific steps are as follows:

[0057] (1) Take 10L of proline fermentation broth, pass through 2L of regenerated 732 resin, and perform adsorption. Determine whether the adsorption is over by measuring whether the adsorption discharge liquid has amino acids leaking out. The adsorption rate is 15mL / min, and finally a volume of 5L is obtained. For the adsorption resin, wash away unadsorbed amino acids and some impurities with 6L of water, and elute the adsorption resin with 4% sodium hydroxide to obtain liquid A;

[0058] (2) Put the liquid A in (1) into a decolorization tank for decolorization, the decolorization temperature is 55°C, the decolorization time is 1h, the amount of activated carbon added is 5‰ of the quality of liquid A, the stirring speed is 180r / min, and the activated carbon is removed by filtration. Decolorization was repeated twice to obtain a decolorization solution;

[0059] (3) passing the decolorizing solution in (2) successively through 301 anion ...

Embodiment 3

[0069] Specific steps are as follows:

[0070] (1) Take 10L of proline fermentation broth, pass through 2L of regenerated 732 resin, and perform adsorption. Determine whether the adsorption is over by measuring whether the adsorption discharge liquid leaks out amino acids. The adsorption rate is 20mL / min, and finally a volume of 5L is obtained. For the adsorption resin, wash away unadsorbed amino acids and some impurities with 6L of water, and elute the adsorption resin with 4% sodium hydroxide to obtain liquid A;

[0071] (2) Put the liquid A in (1) into a decolorization tank for decolorization, the decolorization temperature is 60°C, the decolorization time is 30min, the amount of activated carbon added is 5‰ of the quality of liquid A, the stirring speed is 200r / min, and the activated carbon is removed by filtration. Decolorization was repeated twice to obtain a decolorization solution;

[0072] (3) passing the decolorizing solution in (2) successively through 301 anion re...

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PUM

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Abstract

The invention discloses a preparation method of proline as medicine, which belongs to the technical field of separation extraction. The method comprises the following steps: absorbing a proline fermented solution by virtue of strong-acidity cationic resin, then filtering successively by virtue of a weak-alkalinity anion resin and weak-acidity cationic resin, obtaining proline monohydrate, dehydrating the proline monohydrate by virtue of ethanol, and obtaining the anhydrous proline finished product as medicine. The proline as medicine prepared by using the method of the invention is the anhydrous proline and is good in crystal form, high in purity (the purity is greater than 99 percent, and the light transmittance is greater than 99 percent), and capable of controlling the specific rotationin a range of -84.5 degrees to -86 degrees.

Description

technical field [0001] The invention relates to a preparation method of medicinal proline, which belongs to the technical field of separation and extraction. Background technique [0002] L-proline (referred to as proline) is one of the eighteen kinds of amino acids that the human body synthesizes protein. It has certain physiological activities and is widely used in medicine, agriculture, chemical industry and food, especially in medicine. Intermediates for the synthesis of new drugs. [0003] At present, there are three main methods for the production of L-proline: protein hydrolysis, synthesis and microbial fermentation. However, these three methods will produce pigments, sugars, other amino acids, organic acids and inorganic salts, etc. Impurities. Therefore, in order to obtain high-purity proline, proline must be extracted, separated and purified. [0004] Existing purification methods mainly include ion exchange resin method, anhydrous ethanol recrystallization meth...

Claims

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Application Information

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IPC IPC(8): C07D207/16
CPCC07D207/16
Inventor 宁健飞蔡立明陈晓双
Owner WUXI JINGHAI AMINO ACID