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Method for preparation of high purity samples of 3 impurities in vancomycin hydrochloride

A vancomycin hydrochloride and 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 effects of cost saving and simple process.

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

AI Technical Summary

Problems solved by technology

[0016] Among them, impurity 1, impurity 2, and impurity 10 (see figure 1 ) in vancomycin hydrochloride finished product is relatively low, C18 packing preparation column separation preparation of this impurity needs to consume a large amount of vancomycin hydrochloride finished product and a large amount of mobile phase, the preparation cost is very high

Method used

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  • Method for preparation of high purity samples of 3 impurities in vancomycin hydrochloride
  • Method for preparation of high purity samples of 3 impurities in vancomycin hydrochloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] 1. Take 5g of vancomycin hydrochloride crystalline powder, add purified water to prepare a 50g / L aqueous solution, and the volume of the solution is about 100mL;

[0040] 2. Keep the solution prepared in step 1 warm in a water bath at a temperature of 30°C; add 5mL of hydrogen peroxide, stir evenly and keep warm for 42 hours;

[0041] 3. Use a dropper to slowly add 1% oxalic acid aqueous solution dropwise to the solution, and stir evenly. Stop adding when there are no obvious bubbles in the solution;

[0042] 4. The solution was ultrafiltered with an ultrafiltration membrane with a pore size of 7000Da, and the ultrafiltrate was nanofiltered with a cup-type nanofiltration machine with a pore size of 400Da, and the volume of the solution after nanofiltration was 33.3mL;

[0043] 5. Slowly add 166.6mL of absolute ethanol solution for crystallization, and separate the crystallization mother liquor;

[0044] 6. High-pressure liquid chromatography detects the crystallization...

Embodiment 2

[0049] 1. Take 6g of vancomycin hydrochloride crystalline powder, add purified water to prepare a 40g / L aqueous solution, and the volume of the solution is about 150mL;

[0050] 2. Heat the solution prepared in step 1 in a water bath at a temperature of 25°C; add 9mL of hydrogen peroxide, stir evenly and keep warm for 40 hours;

[0051] 3. Use a dropper to slowly add 2% oxalic acid aqueous solution dropwise to the solution, and stir evenly. Stop adding when there are no obvious bubbles in the solution;

[0052] 4. The solution is ultrafiltered using an ultrafiltration membrane with a pore size of 5000 Da, and the ultrafiltrate is subjected to nanofiltration with a cup-type nanofiltration machine with a pore size of 500 Da, and the volume of the solution after nanofiltration is 60 mL;

[0053] 5. Slowly add 180mL of absolute ethanol solution for crystallization, and separate the crystallization mother liquor;

[0054] 6. The crystallization mother liquor was detected by high p...

Embodiment 3

[0059] 1. Take 5.4g of vancomycin hydrochloride crystalline powder, add purified water to prepare a 40g / L aqueous solution, and the volume of the solution is about 135mL;

[0060] 2. Keep the solution prepared in step 1 warm in a water bath at 28°C; add 8mL of hydrogen peroxide, stir evenly and keep warm for 41 hours;

[0061] 3. Use a dropper to slowly add 1.5% oxalic acid aqueous solution dropwise to the solution, and stir evenly. Stop adding when there are no obvious bubbles in the solution;

[0062] 4. The solution is ultrafiltered using an ultrafiltration membrane with a pore size of 7000Da, and the ultrafiltrate is nanofiltered with a cup-type nanofiltration machine with a pore size of 400Da, and the volume of the solution after nanofiltration is 41.5mL;

[0063] 5. Slowly add 166.2mL of absolute ethanol solution for crystallization, and separate the crystallization mother liquor;

[0064] 6. The crystallization mother liquor was detected by high pressure liquid chromat...

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Abstract

The invention discloses a method for preparation of high purity samples of an impurity 1, an impurity 2 and an impurity 10 in vancomycin hydrochloride. The method includes: taking vancomycin hydrochloride crystalline powder and preparing it into an aqueous solution with a concentration of 40-50g / L; conducting water bath heat preservation at 25-30DEG C, adding hydrogen peroxide, and performing stirring for 40-42h; then adding an oxalic acid aqueous solution slowly, stirring the substances evenly till no generation of bubbles, then stopping adding, and carrying out ultrafiltration and nanofiltration in order; slowly adding ethanol into nanofiltrate to conduct crystallization, and performing pumping filtration to obtain a crystallization mother solution; and employing a high pressure liquid chromatography preparation column to isolate the crystallization mother solution, thus obtaining high purity samples of the impurity 1, impurity 2 and impurity 10 in vancomycin hydrochloride. The method has simple process, and greatly lowers the preparation cost.

Description

technical field [0001] The invention belongs to the field of biological fermentation pharmacy, 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 1, 2 and 10. 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 glycopep...

Claims

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Application Information

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IPC IPC(8): C07K1/34C07K1/30C07K1/16
Inventor 何勇崴赵燕詹付凤张洪兰谢云
Owner PEKING UNIV FOUNDER GRP CO LTD
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