Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Method for preparing high-purity samples of impurities of vancomycin hydrochloride

A vancomycin hydrochloride, high-purity technology is applied in the field of high-purity sample preparation, which can solve the problems of low content, high preparation cost, and consumption of a large amount of vancomycin hydrochloride, and achieve the effect of simple process and cost saving.

Inactive Publication Date: 2017-04-19
PEKING UNIV FOUNDER GRP CO LTD +2
View PDF5 Cites 2 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] Wherein impurity 4, impurity 6, impurity 9 (see figure 1 ) is relatively low in vancomycin hydrochloride finished product, and the separation and preparation of this impurity by C18 packing preparation column requires the consumption of a large amount of vancomycin hydrochloride finished product and a large amount of mobile phase, and the preparation cost is very high

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
  • Method for preparing high-purity samples of impurities of vancomycin hydrochloride
  • Method for preparing high-purity samples of impurities of vancomycin hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] 1. Take 6g of vancomycin hydrochloride crystalline powder, add purified water to prepare a 10g / L aqueous solution, and the volume of the solution is about 600mL;

[0038] 2. Heat the solution prepared in step 1 in a water bath at a temperature of 30°C; add 42mL of ethylene glycol, stir evenly and keep warm for 122 hours;

[0039] 3. Cool down to 20°C, slowly add 3852mL of absolute ethanol dropwise to crystallize, and centrifuge to separate the crystals;

[0040] 4. High-pressure liquid chromatography detects crystals, the content of impurity 4 is 17.68% (mass percentage, the same below), the content of impurity 6 is 21.4%, and the content of impurity 9 is 6.97%;

[0041] 5. Use high-pressure preparative liquid chromatography for preparative separation, separate impurities for freeze-drying detection, and the results are shown in Table 3.

[0042] table 3

[0043] Impurity name Chromatographic purity freeze-dried weight Impurity 4 98.5％ 246μg ...

Embodiment 2

[0045] 1. Take 8g of vancomycin hydrochloride crystalline powder, add purified water to make a 1.5g / L aqueous solution, and the volume of the solution is about 533mL;

[0046] 2. Heat the solution prepared in step 1 in a water bath at a temperature of 33°C; add 42.6mL of ethylene glycol, stir evenly and keep warm for 120 hours;

[0047] 3. Cool down to 21°C, slowly add 2302mL of absolute ethanol dropwise to crystallize, and centrifuge to separate the crystals;

[0048] 4. The crystals were detected by high-pressure liquid chromatography, and the content of impurity 4 was 15.32%, the content of impurity 6 was 19.36%, and the content of impurity 9 was 10.67%;

[0049] 5. Use high-pressure preparative liquid chromatography for preparative separation, and separate impurities for freeze-drying detection. The results are shown in Table 4.

[0050] Table 4

[0051] Impurity name Chromatographic purity freeze-dried weight Impurity 4 98.6％ 186μg Impurity 6 ...

Embodiment 3

[0053] 1. Take 5g of vancomycin hydrochloride crystalline powder, add purified water to make a 1g / L aqueous solution, and the volume of the solution is about 500mL;

[0054] 2. Heat the solution prepared in step 1 in a water bath at a temperature of 33°C; add 35mL of ethylene glycol, stir evenly and keep warm for 120 hours;

[0055] 3. Cool down to 21°C, slowly add 2675mL of absolute ethanol dropwise to crystallize, and centrifuge to separate the crystals;

[0056] 4. The crystals were detected by high-pressure liquid chromatography. The content of impurity 4 was 16.73%, the content of impurity 6 was 22.34%, and the content of impurity 9 was 11.65%;

[0057] 5. Use high-pressure preparative liquid chromatography for preparative separation, separate impurities for freeze-drying detection, and the results are shown in Table 5.

[0058] table 5

[0059] Impurity name Chromatographic purity freeze-dried weight Impurity 4 97.8％ 173μg Impurity 6 98.3％ ...

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

PropertyMeasurementUnit
wavelengthaaaaaaaaaa
Login to View More

Abstract

The invention discloses a method for preparing high-purity samples of related impurities (4, 6 and 9) of vancomycin hydrochloride. The method comprises the steps: preparing an aqueous solution with the concentration of 10g / L to 15g / L from crystalline powder of vancomycin hydrochloride; carrying out water-bath heating to the temperature of 30 DEG C to 33 DEG C, adding ethylene glycol, and carrying out stirring and heat preservationfor 120 to 122 hours; then, cooling the solution to 20 DEG C to 21 DEG C, and dropwise adding anhydrous ethanol into the cooled solution slowly for crystallization; and carrying out crystal separation by using high performance liquid chromatography preparative columns, thereby obtaining the high-purity samples of the impurities (4, 6 and 9) in vancomycin hydrochloride. According to the method, the process is simple, and the preparation cost is reduced greatly.

Description

technical field [0001] The invention belongs to the field of biofermentation pharmaceuticals, and relates to a method for preparing related impurities in antibiotic products, in particular to a method for preparing high-purity samples of vancomycin hydrochloride related impurities 4, 6 and 9. Background technique [0002] Vancomycin hydrochloride is a branched product of tricyclic glycosylated nonribosomal peptides produced by fermentation of the Actinomycetes genus Amycolatopsis orientalis (formerly named Nocardia orientalis). Vancomycin hydrochloride is a narrow-spectrum antibiotic, which is only effective against Gram-positive bacteria, such as hemolytic streptococcus, pneumococcus and enterococcus, which are all sensitive, and are especially sensitive to drug-resistant Staphylococcus aureus. Its mechanism of action is to inhibit the synthesis of bacterial cell walls, and it mainly combines with bacterial cell walls, so that certain amino acids cannot enter the glycopepti...

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
Patent Type & Authority Applications(China)
IPC IPC(8): C07K1/30C07K1/16
Inventor 何勇崴赵燕詹付凤张洪兰谢云
Owner PEKING UNIV FOUNDER GRP CO LTD
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products

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

© 2024 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com