Preparation method of bacitracin zinc

A technology of bacitracin zinc and bacitracin, which is applied in the field of peptide drug preparation, can solve the problems of a large number of crystallization, low yield, unfavorable reaction rate and impurities, etc., and achieves the improvement of crystallization level, product quality, and reduction of product impurity content. Effect

Pending Publication Date: 2021-12-17
JIANGSU JIUYANG BIOLOGICAL PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method has been applied to a certain extent, there are some shortcomings: adding inorganic zinc directly under alkaline conditions will cause a large amount of crystallization, which is not conducive to the control of reaction rate and impurities, and the yield is low

Method used

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  • Preparation method of bacitracin zinc
  • Preparation method of bacitracin zinc
  • Preparation method of bacitracin zinc

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Take 50 L of secondary bacitracin filtrate (the content of bacitracin is 6400 U / mL), and prepare 10% hydrochloric acid solution to adjust the pH to 6.0. Weigh 500.0 g of zinc chloride, prepare a 30% zinc chloride solution, and add the bacitracin filtrate. After stirring and clarification, 5% sodium hydroxide solution was added to adjust the pH to 6.5. After stirring for 10 minutes, retest the pH to 6.5, and continue stirring for 1 hour. Stop stirring, let it stand for 6 hours, filter with suction, take the filter cake, and dry it for 2 hours at a temperature of 80°C. After receiving the materials, 4.55 kg of white powdery dry product was obtained, and the molar yield was 80.2%. Detected by HPLC (spectrum see figure 1 ), the content of bacitracin A is 58.17%, the total amount of bacitracin A, B1, B2, and B3 is 82.31%, the content of bacitracin F is 1.38%, and the sum of impurities precipitated before bacitracin B1 is 10.33%. Conforms to USP standards. According to U...

Embodiment 2

[0031] Take 50L of secondary bacitracin filtrate (bacitracin content is 6400U / mL), prepare 20% hydrochloric acid solution to adjust the pH to 4.0. Weigh 500.0 g of zinc chloride, prepare a 50% zinc chloride solution, and add the bacitracin filtrate. After stirring and clarification, 10% sodium hydroxide solution was added to adjust the pH to 7.5. After stirring for 30 minutes, retest the pH to 7.5, and continue stirring for 1 hour. Stop stirring, let it stand for 6 hours, filter with suction, take the filter cake, and dry it for 4 hours at a temperature of 170°C. After collecting the materials, 4.78 kg of white powdery dry product was obtained, and the molar yield was 84.3%. Detected by HPLC (spectrum see figure 2 ), the content of bacitracin A is 63.86%, the total amount of bacitracin A, B1, B2, and B3 is 81.88%, the content of bacitracin F is 2.49%, and the sum of impurities precipitated before bacitracin B1 is 4.07%. Conforms to USP standards. According to USP standar...

Embodiment 3

[0033] Take 50L of secondary bacitracin filtrate (the content of bacitracin is 6400U / mL), and prepare 30% hydrochloric acid solution to adjust the pH to 2.5. Weigh 500.0 g of zinc chloride, prepare a 60% zinc chloride solution, and add it to the bacitracin filtrate. After stirring and clarification, 20% sodium hydroxide solution was added to adjust the pH to 8.5. After stirring for 40 minutes, retest the pH to 8.5, and continue stirring for 1 hour. Stop stirring, let it stand for 8 hours, filter with suction, take the filter cake, and dry it for 8 hours at a temperature of 250°C. After receiving the materials, 4.51 kg of white powdery dry product was obtained, and the molar yield was 79.5%. Detected by HPLC (spectrum see image 3 ), the content of bacitracin A is 64.15%, the total amount of bacitracin A, B1, B2, and B3 is 82.54%, the content of bacitracin F is 2.15%, and the sum of impurities precipitated before bacitracin B1 is 5.18%. Conforms to USP standards. According...

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Abstract

The invention provides a preparation method of bacitracin zinc. The preparation method comprises the following steps of: (1) adding a hydrochloric acid solution into bacitracin filtrate to adjust the pH to 2.5-6.0, then adding a zinc salt solution, and stirring until the solution is transparent; (2) adding a sodium hydroxide solution, adjusting the pH to 6.5-8.5, continuously stirring for 10-40 minutes, then re-measuring the pH to 6.5-8.5, and standing for more than 6 hours; and (3) carrying out suction filtration to obtain a filter cake, and drying to obtain white bacitracin zinc powder. The preparation method provided by the invention can be used for solving the defect of unstable salifying yield of bacitracin zinc in the prior art; and the zinc salt solution is added under an acidic condition, and then the pH is slowly adjusted to crystallize, so that the reaction phenomenon can be observed more easily, the reaction process can be controlled more easily, and the preparation method has relatively great industrial production and application prospects.

Description

technical field [0001] The invention belongs to the field of preparation of peptide drugs, and in particular relates to a preparation method of bacitracin zinc. Background technique [0002] Bacitracin zinc (Bacitracin zinc, abbreviated as BcZn, CAS1405-89-6) is formed by Zn2+ and the δ-N of the imidazole group of histidine of bacitracin, the sulfur atom of the thiazoline ring and the carboxylate of glutamic acid complexes. White or off-white powder with special odor and bitter taste. The substance is almost insoluble in water, methanol, acetone, and chloroform, easily soluble in pyridine, and slightly soluble in ether. Bacitracin zinc is an effective narrow-spectrum polypeptide antibiotic. Its antibacterial spectrum is similar to that of penicillin. It mainly targets Gram-positive cocci and bacilli. It has the advantages of high efficiency, low toxicity, and less residue. Therefore, bacitracin zinc is not only an important antibiotic drug, but also a safe antibiotic fee...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07K7/58C07K1/107C07K1/30
CPCC07K7/58
Inventor 徐强如
Owner JIANGSU JIUYANG BIOLOGICAL PHARMA
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