L-alanyl-L-glutamine special ultrafine powder freeze dried preparation, and preparation method thereof

A technology of alanyl glutamine and ultrafine powder, which is applied in the field of medicine, can solve the problems of low purity, small specific surface area, and poor solubility of alanyl glutamine, and achieve reduced drug consumption, large specific surface area, The effect of less impurities

Active Publication Date: 2015-08-26
HAINAN LINGKANG PHARMA CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the alanyl glutamine produced by these methods has the disadvantages of low purity, many impurities, large particles, small specific surface area, poor solubility, and low activity.

Method used

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  • L-alanyl-L-glutamine special ultrafine powder freeze dried preparation, and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Take 0.2 mol of commercially available N-(α-chloro)-propionyl-glutamine, dissolve it in 1000ml of water, then add 0.22 mol of methylhydrazine, and react at 55°C under normal pressure, The reaction time was 18 hours, then concentrated, and cooled at a low temperature of 10°C to precipitate the crude product of alanyl glutamine, and the content of alanyl glutamine was measured to be 85.52%.

[0031] At a temperature of 10°C, add anhydrous methanol to the crude product of alanyl glutamine, the amount of anhydrous methanol is 80% of the volume of alanyl glutamine, then vigorously stir to form a slurry, and then pump Consider removing the methanol solution to obtain a filter cake containing alanylglutamine, and wash it 3 times with methanol, and the volume of methanol used for each washing accounts for 1 / 3 of the slurry or suspension volume. In this step, the methanol solution obtained by filtration and the methanol solution obtained by washing are recycled. Therefore, a sm...

Embodiment 2

[0036] Take 0.2 mol of commercially available N-(α-chloro)-propionyl-glutamine, dissolve it in 1200ml of water, then add 0.22 mol of methylhydrazine, and react at 60°C under normal pressure, The reaction time was 16 hours, then concentrated, and cooled at a low temperature of 15°C to precipitate the crude product of alanyl glutamine, and the content of alanyl glutamine was measured to be 85.63%.

[0037]At a temperature of 10°C, add anhydrous methanol to the crude product of alanyl glutamine, the amount of anhydrous methanol is 80% of the volume of alanyl glutamine, then vigorously stir to form a slurry, and then pump Consider removing the methanol solution to obtain a filter cake containing alanylglutamine, and wash it 3 times with methanol, and the volume of methanol used for each washing accounts for 1 / 2 of the slurry or suspension volume. In this step, the methanol solution obtained by filtration and the methanol solution obtained by washing are recycled. Therefore, a sma...

Embodiment 3

[0042] Take 0.2 mol of commercially available N-(α-chloro)-propionyl-glutamine, dissolve it in 1300ml of water, then add 0.22 mol of methylhydrazine, and react at 65°C under normal pressure, The reaction time was 15 hours, then concentrated, and cooled at a low temperature of 13°C to precipitate a crude product of alanyl glutamine, and the content of alanyl glutamine was measured to be 85.58%.

[0043] At a temperature of 10°C, add anhydrous methanol to the crude product of alanyl glutamine, the amount of anhydrous methanol is 80% of the volume of alanyl glutamine, then vigorously stir to form a slurry, and then pump Consider removing the methanol solution to obtain a filter cake containing alanylglutamine, and wash it 3 times with methanol, and the volume of methanol used for each washing accounts for 1 / 2 of the slurry or suspension volume. In this step, the methanol solution obtained by filtration and the methanol solution obtained by washing are recycled. Therefore, a smal...

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Abstract

The invention discloses an L-alanyl-L-glutamine special ultrafine powder freeze dried preparation, and a preparation method thereof. The preparation method comprises following steps: step 1, N-(alpha-chloro)-propionyl-glutamine is taken as a raw material, methylhydrazine is taken as an ammonification agent, reaction is carried out under normal pressure, concentration and low temperature cooling are carried out, and an L-alanyl-L-glutamine crude product is obtained via precipitation; step 2, at 10 DEG C, absolute methanol is added into the L-alanyl-L-glutamine crude product, stirring is carried out, and methanol solution is removed via air pump filtration so as to obtain a filter cake containing L-alanyl-L-glutamine; step 3, the filter cake containing L-alanyl-L-glutamine is dissolved in water, an obtained mixed solution is heated to 75 DEG C, and the temperature is maintained for a certain time for condensation, ethanol is added, gradient cooling and recrystallization are carried out so as to obtain purified L-alanyl-L-glutamine; step 4, crystallized L-alanyl-L-glutamine is subjected to centrifugal washing and drying; and step 5, the dried L-alanyl-L-glutamine is smashed into ultrafine powder with gas stream, and freeze drying is carried out.

Description

technical field [0001] The invention relates to a special ultrafine powder freeze-dried preparation of alanyl glutamine and a preparation method thereof, belonging to the technical field of medicine. Background technique [0002] Alanyl glutamine is also known as N-(2)-L-alanyl-glutamine, the English name is L-alanyl-L-glutamine, and the chemical name is N(2)-L-alanyl-glutamine , formula C 8 h 15 N 3 o 4 , molecular weight 217.22, structural formula: [0003] [0004] Alanyl glutamine was first developed by Fresenius, AG in Germany and imported to China in 1999. In December 1999, "Special Ultrafine Powder Preparation Technology" won the first prize of the National Science and Technology Progress Award. The award-winning unit: Nanjing University of Science and Technology (Li Fengsheng), certificate number: 30-1-003-01. January 2, 2014, Nanjing University of Science and Technology's "Application of Special Ultrafine Powder Preparation Technology in Pharmaceutical Prep...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K9/19A61K38/05
Inventor 姜晓东李凤生
Owner HAINAN LINGKANG PHARMA CO LTD
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