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Preparation method of high purity samples of vancomycin hydrochloride impurities 11, 13, and 15

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.

Active Publication Date: 2017-04-19
新方正控股发展有限责任公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0016] Wherein impurities 11, 13 and 15 (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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  • Preparation method of high purity samples of vancomycin hydrochloride impurities 11, 13, and 15
  • Preparation method of high purity samples of vancomycin hydrochloride impurities 11, 13, and 15

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] 1. Take 10 g of vancomycin hydrochloride crystalline powder (purity detected by high pressure liquid chromatography is 95.1%), add 5% purified water to prepare a 52 g / L aqueous solution, and the solution volume is 192.4 mL;

[0048] 2. Adjust the pH of the solution to 4.15 with 2% oxalic acid solution, and keep it in a water bath at 40-42°C for 8 hours;

[0049] 3. Add 2% sodium bicarbonate solution to the solution after heat preservation to adjust the pH to 6.37;

[0050] 4. Perform FPDA13 resin chromatography on the solution after adjusting the pH. The column loading capacity of FPDA13 resin is 1500mL, and the flow rate is 2250mL / h.

[0051] 5. Use 4500mL of 0.03mol / L NH 4 Pre-wash the resin with Cl aqueous solution, the flow rate is 1200mL / h;

[0052] 6. Use 5500mL of 0.3mol / L NH 4 Cl aqueous solution is carried out eluting, and flow rate is 900mL / h, and 150mL collects a bottle, and sampling high-pressure liquid chromatography detects (detection method is the same...

Embodiment 2

[0058] 1. Take 10g of vancomycin hydrochloride crystalline powder (purity detected by high pressure liquid chromatography is 96.3%), add 5% purified water to prepare a 56g / L aqueous solution, and the solution volume is 178.6mL;

[0059] 2. Adjust the pH of the solution to 4.69 with 1% oxalic acid solution, and keep it in a water bath at 40-42°C for 9 hours;

[0060] 3. Add 1.5% sodium bicarbonate solution to the solution after heat preservation to adjust the pH to 6.93;

[0061] 4. Perform FPDA13 resin chromatography on the solution after adjusting the pH. The column loading capacity of FPDA13 resin is 1500mL, and the flow rate is 2250mL / h.

[0062] 5. Use 4500mL of 0.03mol / L NH 4 Pre-wash the resin with Cl aqueous solution, the flow rate is 1100mL / h

[0063] 6. Use 5500mL of 0.3mol / L NH 4 Cl aqueous solution was used for elution, the flow rate was 1000mL / h, 150mL was collected in one bottle, and samples were detected by high-pressure liquid chromatography, and the analysis s...

Embodiment 3

[0069] 1. Take 10g of vancomycin hydrochloride crystalline powder (purity detected by high pressure liquid chromatography is 95.3%), add 5% purified water to prepare a 60g / L aqueous solution, and the solution volume is 166.7mL;

[0070] 2. Adjust the pH of the solution to 5.86 with 1.5% oxalic acid solution, and keep it in a water bath at 40-42°C for 8.5 hours;

[0071] 3. Add 1.5% sodium bicarbonate solution to the solution after heat preservation to adjust the pH to 6.21;

[0072] 4. Perform FPDA13 resin chromatography on the solution after adjusting the pH. The column loading capacity of FPDA13 resin is 1500mL, and the flow rate is 1500mL / h.

[0073] 5. Use 4500mL of 0.03mol / L NH 4 Pre-wash the resin with Cl aqueous solution, the flow rate is 1100mL / h

[0074] 6. Use 5500mL of 0.3mol / L NH 4 Cl aqueous solution was used for elution, the flow rate was 900mL / h, 150mL was collected in one bottle, and samples were detected by high-pressure liquid chromatography, and the analy...

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Abstract

The invention discloses a preparation method of high purity samples of vancomycin hydrochloride impurities 11, 13, and 15. The preparation method comprises the following steps: preparing a vancomycin hydrochloride water solution with a concentration of 60 to 70 g / L from vancomycin hydrochloride crystallized powder, adjusting the pH to 4-6, maintaining a constant temperature of 40 to 42 DEG C for 8 to 9 hours in water bath, adjusting the pH to 6-7, carrying out macroporous resin chromatographic enrichment, collecting the coarse product liquids (with impurities from 40 to 60%) of impurities 11, 13, and 15, subjecting the coarse product liquids to ultrafiltration and nano filtration in sequence, and desalinating the nano filtrate by a high performance liquid chromatography (HPLC) column to obtain the high purity samples of vancomycin hydrochloride impurities 11, 13, and 15. The technology is simple, and the preparation cost is largely 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 11, 13 and 15. 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 glycop...

Claims

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Application Information

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IPC IPC(8): G01N1/28
Inventor 詹付凤何勇崴赵燕张洪兰谢云
Owner 新方正控股发展有限责任公司
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