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Method for preparing high-purity sample of vancomycin hydrochloride impurities 3 and 8

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
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] Wherein impurity 3, 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

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  • Method for preparing high-purity sample of vancomycin hydrochloride impurities 3 and 8
  • Method for preparing high-purity sample of vancomycin hydrochloride impurities 3 and 8
  • Method for preparing high-purity sample of vancomycin hydrochloride impurities 3 and 8

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] 1. Take 5g of vancomycin hydrochloride crystalline powder (purity detected by high pressure liquid chromatography is 95%), add 5% sodium chloride aqueous solution to configure a 42g / L aqueous solution, and the solution volume is about 119mL;

[0056] 2. Insulate the solution prepared in step 1 in a water bath at a temperature of 72°C for 72 hours, then cool down to 4°C and perform nanofiltration with a cup-type nanofiltration machine with a pore size of 500 Da. After nanofiltration, the solution volume is 70 mL and stored at 4°C;

[0057] 3. Put the solution after nanofiltration on 1000mL HP20SS resin column;

[0058] 4. Wash the resin with 3000 mL of 1% concentration (g / mL) of ammonium acetate aqueous solution after loading the column;

[0059] 5. Use 3000mL of 0.3% concentration (g / ml) of NH 4 HCO 3 Aqueous solution (pH7.9~8.0) pre-washing;

[0060] 6. Use 5000mL of 0.5% concentration (g / ml) of NH 4 HCO 3 Water-soluble (pH7.9-8.0) liquid elution, collect one bott...

Embodiment 2

[0075] 1. Take 5g of vancomycin hydrochloride crystalline powder (purity detected by high pressure liquid chromatography is 96%), add 6% sodium chloride aqueous solution to configure a 45g / L aqueous solution, and the solution volume is about 111mL;

[0076] 2. Insulate the solution prepared in step 1 in a water bath at a temperature of 73°C for 73 hours, then cool down to 4°C and perform nanofiltration with a cup-type nanofiltration machine with a pore size of 500 Da. After nanofiltration, the solution volume is 64.6mL and stored at 4°C;

[0077] 3. Put the solution after nanofiltration on 1000mL Chromatography-3 resin column;

[0078] 4. After loading the column, wash the resin with 3000mL of 1% ammonium acetate aqueous solution;

[0079] 5. Use 3000mL of 0.3% NH 4 HCO 3 Aqueous solution (pH7.9~8.0) pre-washing;

[0080] 6. Use 5000mL of 0.5% NH 4 HCO 3 Aqueous solution (pH7.9~8.0) elution, every 100mL collects a bottle, and sampling high-pressure liquid chromatography d...

Embodiment 3

[0087] 1. Take 5g of vancomycin hydrochloride crystalline powder (purity detected by high pressure liquid chromatography is 95.6%), add 6% aqueous sodium chloride solution to form a 50g / L aqueous solution, and the volume of the solution is about 100mL;

[0088] 2. Insulate the solution prepared in step 1 in a water bath at a temperature of 72.5°C and hold for 72.5 hours, then cool down to 4°C and perform nanofiltration with a cup-type nanofiltration machine with a pore size of 500Da. After nanofiltration, the solution volume is 60.8mL and stored at 4°C ;

[0089] 3. Put the solution after nanofiltration on 1000mL Chromatography-3 resin column;

[0090] 4. After loading the column, wash the resin with 3000mL of 1% ammonium acetate aqueous solution;

[0091] 5. Use 3000mL of 0.3% NH 4 HCO 3 Aqueous solution (pH7.9~8.0) pre-washing;

[0092] 6. Use 5000mL of 0.5% NH 4 HCO 3 Aqueous solution (pH7.9~8.0) elution, every 100mL collects a bottle, and sampling high-pressure liqui...

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Abstract

The invention discloses a method for preparing a high-purity sample of vancomycin hydrochloride impurities 3 and 8. The method comprises the following steps: taking vancomycin hydrochloride crystalline powder, preparing the vancomycin hydrochloride crystalline powder into a solution with concentration being 40-50g / L by use of a sodium chloride aqueous solution; preserving heat for 72-73 hours at a water bath ranging from 70 DEG C to 75 DEG C; cooling the solution to 4-6 DEG C, and carrying out nanofiltration desalination; carrying out resin chromatography enrichment on nanofiltration liquor, and separately collecting desorbed solutions of an impurity 3 and an impurity 8, purity of which is greater than 80%; sequentially carrying out ultrafiltration and nanofiltration on the desorbed solutions; and desalinizing the nanofiltration liquor with a high-pressure liquid-phase chromatography preparation column to obtain high-purity samples of the impurity 3 and the impurity 8, and the purity of the samples is greater than 97%. The method disclosed by the invention is simple in process, so that preparation cost is greatly reduced.

Description

technical field [0001] The invention belongs to the field of bio-fermentation 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 3 and 8. 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 glycopeptide...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K1/34C07K1/16
Inventor 詹付凤何勇崴赵燕张洪兰谢云
Owner PEKING UNIV FOUNDER GRP CO LTD
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