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Preparation method of hydroxypropyl-[beta]-cyclodextrin

A technology of cyclodextrin and hydroxypropyl, which is applied in the field of preparation of pharmaceutical excipients in medicine, can solve the problems of low yield of hydroxypropyl-β-cyclodextrin and high degree of product substitution, and achieve high yield and substitution low degree of effect

Active Publication Date: 2014-11-19
ZIBO QIANHUI BIOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to overcome the problems of low yield and high product substitution degree in the production of hydroxypropyl-β-cyclodextrin in the prior art, the invention provides a production method of hydroxypropyl-β-cyclodextrin, and the obtained hydroxypropyl -β-cyclodextrin has the advantages of high yield, low degree of substitution, high hemolysis, etc.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Use distilled water to prepare starch milk with a potato starch mass concentration of 12%, stir at 75°C for 30 minutes; then adjust the temperature to 40°C, and add cyclodextrin glucose at a concentration of 9 enzyme activity units per gram of starch Base transferase, and then add cyclohexane: add 0.8mL cyclohexane per gram of starch, convert for 6 hours, adjust the pH value to 8 during the conversion process, and obtain the β-cyclodextrin by crystallization after filtration Refined products;

[0023] (2) heating the aqueous sodium hydroxide solution with a mass concentration of 20% to 50°C, slowly adding the β-cyclodextrin obtained in step (1) while stirring, continuing to stir until the β-cyclodextrin is completely dissolved, and cooling to room temperature, Add 30ml of 1,2-propylene oxide dropwise evenly within 3 hours while stirring in a water bath, control the temperature at 22°C during the dropwise addition, and continue stirring for 3 hours after the dropwise...

Embodiment 2

[0028] (1) Use distilled water to prepare starch milk with a potato starch mass concentration of 14%, stir at 85°C for 50 minutes; then adjust the temperature to 45°C, and add cyclodextrin glucose at a concentration of 13 enzyme activity units per gram of starch Base transferase, and then add cyclohexane: add 1.1mL cyclohexane per gram of starch, convert for 7 hours, adjust the pH value to 9 during the conversion process, and obtain the β-cyclodextrose by crystallization from the filtrate after filtration Refined products;

[0029] (2) Heat the aqueous sodium hydroxide solution with a mass concentration of 25% to 55° C., slowly add the β-cyclodextrin obtained in step (1) while stirring, continue stirring until the β-cyclodextrin is completely dissolved, and cool to room temperature. Add 35ml of 1,2-propylene oxide dropwise evenly within 3.5 hours while stirring in a water bath, and control the temperature at 24°C during the dropwise addition, and continue to stir for 5 hours a...

Embodiment 3

[0034](1) Use distilled water to prepare starch milk with a potato starch mass concentration of 13%, stir at 80°C for 40 minutes; then adjust the temperature to 42°C, and add cyclodextrin glucose at a concentration of 10 enzyme activity units per gram of starch Base transferase, and then add cyclohexane: add 1.0mL cyclohexane per gram of starch, convert for 6 hours, adjust the pH value to 8 during the conversion process, and obtain the β-cyclodextrose by crystallization from the filtrate after filtration Refined products;

[0035] (2) Heat the aqueous sodium hydroxide solution with a mass concentration of 23% to 53° C., slowly add the β-cyclodextrin obtained in step (1) while stirring, continue stirring until the β-cyclodextrin is completely dissolved, and cool to room temperature. Add 33ml of 1,2-propylene oxide dropwise evenly within 3.2 hours while stirring under the water bath, and control the temperature at 23°C during the dropwise addition, and continue to stir for 4 hou...

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Abstract

The invention discloses a preparation method of hydroxypropyl-[beta]-cyclodextrin. The method includes following steps: (1) preparing a product of [beta]-cyclodextrin; (2) heating a sodium hydroxide aqueous solution with a mass concentration being 20%-25% to 50-55 DEG C, slowly adding the [beta]-cyclodextrin obtained in the step (1) with stirring, continuously performing stirring until the [beta]-cyclodextrin is dissolved completely, cooling the solution to room temperature, dropwisely adding 30-35 ml of 1,2-epoxypropane uniformly in 3-3.5h with stirring in water bath with a temperature being controlled within 22-24 DEG C, and continuously performing stirring for 3-5 hours after the dropwisely adding process is finished, wherein a molar ratio of the sodium hydroxide, the [beta]-cyclodextrin and the 1,2-epoxypropane is 4:2-3:1-2; (3) neutralizing the reactant obtained in the step (2) for adjusting the pH of the reactant to be 7; (4) performing reduced pressure distillation to the reactant obtained in the step (3), dissolving a obtained slurry subject through ethanol, performing a stirring and filtering process and performing the reduced pressure distillation again to obtain a thick slurry; and step (5) feeding the thick slurry to a spray drier with the temperature being controlling within 5-10 DEG C to obtain a white amorphous powder of the hydroxypropyl-[beta]-cyclodextrin. The prepared hydroxypropyl-[beta]-cyclodextrin is low in substitution degree and is high in yield.

Description

technical field [0001] The invention relates to a preparation method of medical auxiliary materials, in particular to a preparation method of hydroxypropyl-β-cyclodextrin. Background technique [0002] Cyclodextrin (cyclodextrin, CD), also known as cyclopolyglucose, is a general term for a group of oligosaccharides composed of several D-glucopyranose units arranged in a ring. Cyclodextrins were discovered by Villiers in 1891 by enzymatically degrading starch. In 1904, Schardinger first described the preparation of cyclodextrin in detail. Because of this description, early literature also referred to cyclodextrins as Schardinger dextrins. [0003] Cyclodextrin chemistry has advanced by leaps and bounds in the past two to three decades. So far, there have been many monographs and several long reviews, more than 1400 patents and thousands of articles describing the structure, properties and applications of cyclodextrin and its inclusion complexes. As a simple organic macrom...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B37/16C12P19/18
Inventor 王丽萍毕方玉许维成王哲
Owner ZIBO QIANHUI BIOTECH
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