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Refining method of alanyl-glutamine crude drug

A technology of alanyl glutamine and refining method, which is applied in the fields of peptide preparation method, chemical instrument and method, organic chemistry, etc. It can solve the problem of fine-quality products without adjusting the pH value, not being able to be directly prepared by injection, and the content of fine-quality products To achieve the effect of reducing the possibility of new impurities, reducing the content of impurities and bacterial endotoxin, and moderate crystallization speed

Active Publication Date: 2013-10-23
SHANDONG QIDU PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] At the same time, the refining method described in the above literature for the alanyl glutamine raw material drug is only a simple supplement to the synthetic method, and there is no special research on the refining process. In the mentioned method, the refined product is not refined. The detection of the content of relevant substances, the detection of bacterial endotoxins, and the pH value of the prepared fine products have not been adjusted, so they cannot be directly used in the preparation of injections

Method used

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  • Refining method of alanyl-glutamine crude drug
  • Refining method of alanyl-glutamine crude drug
  • Refining method of alanyl-glutamine crude drug

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 50kg of alanylglutamine into 150kg of water, stir until completely dissolved, add 5% potassium hydroxide solution to adjust the pH to 5.0, then add 0.25kg of activated carbon, keep the stirring speed at 200 rpm, stir and absorb at room temperature for 30min, filter and decolorize to obtain Colorless clear liquid. Add the clarified feed liquid into the crystallization tank and raise the temperature to 40°C. Maintain the stirring speed at 200 rpm, add methanol 600kg at 45°C, and white crystals precipitate out. After the precipitation is completed, they are centrifuged and washed, the filter cake is vacuum-dried, and 47.5kg of high-purity alanyl glutamine is obtained by weighing, with a yield of 95%. 99.97% (HPLC detection).

[0034] HPLC impurity reference substance method detection, cyclo-(L-alanyl-L-glutamine), cyclo-(L-alanyl-L-glutamyl), L-pyroglutamyl-L-alanine Acid, L-pyroglutamic acid, D-alanyl-L-glutamine (or L-alanyl-D-glutamine), L-alanyl-L-glutamic acid a...

Embodiment 2

[0044] Add 100kg of alanylglutamine into 500kg of water, stir until completely dissolved, add 10% potassium hydroxide solution to adjust the pH to 5.5, then add 0.3kg of activated carbon, maintain the stirring speed at 400 rpm, stir and absorb at 50°C for 30 minutes, filter and decolorize A colorless clear liquid was obtained. Add the clarified feed liquid into the crystallization tank and raise the temperature to 45°C. Maintain the stirring speed at 500 rpm, add 1280kg of methanol at 62°C, and white crystals precipitate out. After the precipitation is completed, they are centrifuged and washed, the filter cake is vacuum-dried, and the high-purity alanyl glutamine is weighed to obtain 95kg. The yield is 95%, and the purity is 99.98. % (HPLC detection).

[0045] HPLC impurity reference substance method detection, cyclo-(L-alanyl-L-glutamine), cyclo-(L-alanyl-L-glutamyl), L-pyroglutamyl-L-alanine Acid, L-pyroglutamic acid, D-alanyl-L-glutamine (or L-alanyl-D-glutamine), L-alan...

Embodiment 3

[0053] Add 100kg of alanylglutamine into 250kg of water, stir until completely dissolved, add methanol solution with a potassium methoxide content of about 28%-32%, adjust the pH to 6.0, then add 0.5kg of activated carbon, maintain the stirring speed at 500rpm, 60℃ Stir and adsorb for 30 minutes, filter and decolorize to obtain a colorless and clear feed liquid. Add the clarified feed liquid into the crystallization tank and raise the temperature to 50°C. Maintain the stirring speed at 400 rpm, add 1000 kg of methanol at 40 °C, white crystals precipitate out, centrifuge and wash the filter cake after the precipitation, vacuum dry the filter cake, weigh 95 kg of high-purity alanyl glutamine, yield 95%, purity 99.97 % (HPLC detection).

[0054] HPLC impurity reference substance method detection, cyclo-(L-alanyl-L-glutamine), cyclo-(L-alanyl-L-glutamyl), L-pyroglutamyl-L-alanine Acid, L-pyroglutamic acid, D-alanyl-L-glutamine (or L-alanyl-D-glutamine), L-alanyl-L-glutamic acid ...

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Abstract

The invention relates to a refining method of an alanyl-glutamine crude drug. The method comprises the following processes: adding an alanyl-glutamine crude product to water, stirring until the alanyl-glutamine crude product is completely dissolved; adding alkali to adjust the pH value, adding active carbon, stirring for realizing absorption; filtering and decolorizing to obtain clear material liquid, then adding a polar solvent, crystallizing and filtering; and drying to obtain an alanyl-glutamine refined product. By adopting the refining method, alanyl-glutamine impurities and the content of bacterial endotoxin are effectively controlled; the target of intravenous administration is achieved; and the safety of alanyl-glutamine intravenous preparations is also improved.

Description

technical field [0001] The invention relates to the field of drug synthesis, in particular to a method for refining alanyl glutamine crude drug. Background technique [0002] Alanyl Glutamine (Alanyl Glutamine), chemical name: N(2)-L-alanyl-L-glutamine, chemical structure as follows: [0003] [0004] Alanylglutamine can be broken down into glutamic acid and alanine in the body, which makes it possible to supplement glutamine through parenteral nutrition infusion. The amino acids released by the decomposition of dipeptide can be stored in the corresponding parts of the body as nutrients and metabolized according to the needs of the body. When applying parenteral nutrition support to many diseases, patients may experience depletion of glutamine in the body, and dipeptide infusion can prevent the appearance of this symptom, and dipeptide can be quickly and effectively decomposed into alanine and alanine by the body. Glutamine is used by the body without any side effects. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K5/062C07K1/36C07K1/30C07K1/22
Inventor 刘绪贵路云黄国英刘明明宋彩香
Owner SHANDONG QIDU PHARMA
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