Technology for purifying medicines for treating deep fungal infection

A deep fungus and drug technology, applied in the direction of sugar derivatives, sugar derivatives, organic chemistry, etc., can solve the problems of high cost, complicated process, low yield, etc., and achieve high yield, simple pretreatment, and good adsorption effect Effect

Active Publication Date: 2012-10-24
SHANGHAI NEW ASIA PHARMA
View PDF3 Cites 3 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The technical problem to be solved by the present invention is to provide a purification process for the treatment of deep fungal infection medicaments for the origi

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Technology for purifying medicines for treating deep fungal infection

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Step 1: Put 8.47g (10 billion total) of Amphotericin B in 150ml DMF and 200ml 80% methanol water solvent, adjust the pH to 2.0-4.0 with citric acid to dissolve, and filter the dissolved solution to obtain a clear filtrate;

[0023] Step 2: Pretreat A resin and B resin with DMF and methanol. A resin uses AM-7 resin and B resin uses AM-18 resin. Take 170ml AM-7 resin and 230ml AM-18 resin respectively by wet method Load it into a chromatography column with a column diameter ratio of 12.5:1, pass the filtrate through a mixed resin column, and control the outflow rate to 2-10ml / min; then add the filtrate from the column to a mixture of 100ml dichloromethane and 100ml water for injection In the solvent, adjust the pH to 4.0-6.0 with triethylamine to crystallize; after crystallization, the solution is placed in a water bath and slowly heated to 35-45°C, and kept for 18-24 hours to grow crystals.

[0024] Step 3: The obtained crystal growth solution is suction filtered and sent to ...

Embodiment 2

[0027] Step 1: Put 462.96g (50 billion total) of Amphotericin B into 10LDMF and 10L of 80% methanol water solvent, adjust the pH to 2.0-4.0 with citric acid to dissolve, and filter the dissolved solution to obtain a clear filtrate;

[0028] Step 2: Pretreat macroporous resins of HPD-100 and HPD-500 with DMF and methanol, respectively, weigh 11.4L of HPD-100 and 13.6L of HPD-500 resin into the column diameter ratio of 12.5 by wet method :1 chromatographic column, pass the filtrate obtained in step 1 through a mixed resin column, and control the outflow rate to 2-10ml / min; then add the filtrate obtained through the column to a mixed solvent of 10L dichloromethane and 12.5L water for injection , Adjust the pH to 4.0-6.0 with citric acid, and crystallize; after crystallization, keep the crystal growing tank at 35-45°C and let it stand for 18-24h.

[0029] Step 3: The crystal growth solution obtained in step 2 is suction filtered and sent to an oven for drying at a temperature of 40° C....

Embodiment 3

[0032] Step 1: Put 847.46g (100 billion total) of Amphotericin B in 18LDMF and 20L methanol (80%) solvent, adjust the pH to 2.0-4.0 with citric acid to dissolve, and filter the dissolved solution to obtain a clear filtrate ;

[0033] Step 2: Pretreat macroporous resins of HPD-100 and HPD-500 with DMF and methanol, respectively, weigh 17.8L of HPD-100 and 22.2L of HPD-500 resin into the column diameter ratio of 12.5. :1 chromatographic column, pass the filtrate obtained in step 1 through a mixed resin column, and control the outflow rate to 2-10ml / min; then add the filtrate obtained through the column to a mixed solvent of 15L dichloromethane and 20L water for injection, Adjust the pH to 4.0-6.0 with citric acid to crystallize; after crystallization, keep the crystal growing tank at 35-45°C and leave it to stand for 18-24 hours.

[0034] Step 3: Filter the obtained crystal growth solution, send the crystal to an oven for drying, at a temperature of 50° C., a pressure of 0.8-1.0 Mpa...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

PUM

No PUM Login to view more

Abstract

The invention discloses a technology for purifying medicines for treating deep fungal infection. The technology is characterized in that the technology comprises the following steps: 1, adding one-hundred-million amphotericin B to a mixed solvent of dimethyl formamide and a 180% methanol solution, and adjusting the pH value of the resulting solution; 2, preprocessing a macroporous absorbent resin A and a macroporous absorbent resin B which have different polarities with the dimethyl formamide and ethanol, mixing the resin A with the resin B according to a resin A/resin B ratio of 3:4-5:6, packing the resulting mixed resin to a chromatographic column having a column length-diameter ratio of 12.5:1 through using a wet packing method to obtain a mixed resin column, allowing a filtrate obtained in step 1 to pass through the mixed resin column, mixing the filtrate passing through the mixed resin column with dichloromethane and injection water according to a ratio of the amphotericin B to the dichloromethane to the injection water of one hundred million:10-20ml:10-25ml, adjusting the pH of the resulting solution with an acid or an alkali to 4.0-6.0, crystallizing, maintaining the temperature at 35-45DEG C after crystal generation, and carrying out crystal growing through allowing crystals to stand for 18-24h; and 3, carrying out suction filtration on the solution obtained after the crystal growing, and drying at 40-60DEG C for 24-30h to obtain products. The technology solves problems of low yield, complex technology and high cost of traditional recrystallization methods, and solves disadvantages of use of a single resin to purify, long column passing time, large resin consumption amount, and unsatisfactory effect.

Description

Technical field [0001] The invention relates to a process for refining and purifying raw materials, in particular to a process for purification of raw materials for treating deep fungal infections. Background technique [0002] Amphotericin B (Amphotericin B) is the first macromolecular polyene antibiotic produced by Streptomyces nodosus to be effective against fungal infections. It has a broad antibacterial spectrum and is clinically useful for the treatment of deep fungal infections. The drug of choice. Its chemical name [0003] [1R-(1R*, 3S*, 5R*, 6R*, 9R*, 11R*, 15S*, 16R*, 17R*, 18S*, 19E, 21E, 23E, 25E, 27E, 29E, 31E, 33R* , 35S*, 36R*, 37S*)]-33-[(3-amino-3,6-dideoxy-β-D-mannopyranosyl)oxy]-1,3,5,6,9, 11,17,37-octahydroxy-15,16,18-trimethyl-13-oxo-14,39-dioxobicyclo-[33.3.1]nonaccharane-19,21,23,25, 27,29,31-Heptaene-36-carboxylic acid, the chemical structure is as follows [0004] [0005] Although the current production of amphotericin B in my country has reached the i...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to view more

Application Information

Patent Timeline
no application Login to view more
IPC IPC(8): C07H17/08C07H1/06
Inventor 池王胄宋庭李仁勤孙常悖石永胜张玉莲
Owner SHANGHAI NEW ASIA PHARMA
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Try Eureka
PatSnap group products

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic.

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap