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Etimicin sulfate preparation method

A technology of etimicin sulfate and etimicin sulfate, applied in the field of separation of macroporous adsorption resin, preparation of etimicin sulfate, purification and preparation of high-purity etimicin sulfate, can solve the problem of ammonia volatilization production, difficult Control, cumbersome resin regeneration and other problems, to achieve the effect of less organic solvent, easy operation and low production cost

Active Publication Date: 2013-07-10
SHANGHAI INST OF PHARMA IND CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has problems such as cumbersome resin regeneration, volatilization of ammonia water and difficulty in production control.

Method used

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  • Etimicin sulfate preparation method
  • Etimicin sulfate preparation method

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Experimental program
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Effect test

Embodiment 1

[0028] Dissolve 10.0 g of the crude product of etimicin in 200 ml of pure water (purity detected by HPLC is about 64%, and the concentration of the crude product is 50 mg / ml; it is carried out according to the method of the 2005 edition of the Pharmacopoeia, the same below), and the pH is adjusted to 9.0.

[0029] Install a HZ-806 adsorption resin column with a height of about 20 cm and a diameter of about 4 cm, and pass the above solution through the column at a flow rate of 10 ml / min, and a small amount of etimicin flows out. And use 2CV of pure water to wash away the salt and water-soluble impurities, and the etimicin will not leak out at this time. Then use 20CV of dilute sulfuric acid solution of pH 3.0 to elute impurities such as gentamicin C1a, and a small amount of etimicin sulfate will be washed out at this time. Finally, the column was eluted with a dilute sulfuric acid solution with pH 1.5, and the part with higher purity in the eluate was distributed and collected....

Embodiment 2

[0043] Dissolve 10.0 g of the crude product of etimicin in 200 ml of pure water (the detection purity is about 64%, the concentration of the crude product is 50 mg / ml), and the pH is adjusted to 10.8.

[0044] Install a HZ-806 adsorption resin column with a height of about 20 cm and a diameter of about 4 cm, pass the above solution through the column at a flow rate of 10 ml / min, and the etimicin is completely adsorbed on the column. And use 2CV of pure water to wash away the salt and water-soluble impurities, and the etimicin will not leak out at this time. Then use 20CV of dilute sulfuric acid solution of pH 3.0 to elute impurities such as gentamicin C1a, and a small amount of etimicin sulfate will be washed out at this time. Finally, the column was eluted with a dilute sulfuric acid solution of pH 1.5, and the part with higher purity in the eluate was distributed and collected. HPLC detection showed that the purity was 93.4%, and a large amount of pigment was removed. The c...

Embodiment 3

[0047] Dissolve 10.0 g of the crude product of etimicin in 200 ml of pure water (the detection purity is about 64%, the concentration of the crude product is 50 mg / ml), and the pH is adjusted to 12.0.

[0048] Install a HZ-806 adsorption resin column with a height of about 20 cm and a diameter of about 4 cm, pass the above solution through the column at a flow rate of 10 ml / min, and the etimicin is completely adsorbed on the column. And use 2CV of pure water to wash away the salt and water-soluble impurities, and the etimicin will not leak out at this time. Then use 20CV of dilute sulfuric acid solution of pH 3.0 to elute impurities such as gentamicin C1a, and a small amount of etimicin sulfate will be washed out at this time. Finally, the column was eluted with a dilute sulfuric acid solution with pH 1.5, and the part with higher purity in the eluate was distributed and collected. HPLC detection found that the purity was 93.1%, and a large amount of pigment was removed. The ...

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Abstract

The invention provides an etimicin sulfate preparation method. The method comprises the following steps: 1, adjusting the pH value of an etimicin-containing crude solution having a concentration of 50-100mg / ml to 9.0-12.0 to obtain a mother solution; 2, adding the mother solution to a macro-porous adsorption resin column, eluting with water, a dilute sulfuric acid solution having a pH value of 2.5-3.0 and a dilute sulfuric acid solution having a pH value of 1.5-2.0 step by step, collecting, and concentrating to obtain a primary separation solution which is an etimicin sulfate solution having a concentration of 50-100mg / ml; and 3, adjusting the pH value of the primary separation solution to 10.0-11.5, adding the obtained solution to a reversed-phase adsorption resin column, eluting with water and the dilute sulfuric acid solution having a pH value of 1.5-2.0 step by step, collecting, concentrating to an etimicin sulfate solution having a concentration of 100-200mg / ml, and lyophilizing to obtain a refined product.

Description

technical field [0001] The invention belongs to the field of pharmaceutical engineering and relates to a method for preparing etimicin sulfate, in particular to a method for separating, purifying and preparing high-purity etimicin sulfate by using a macroporous adsorption resin. Background technique [0002] Etimicin Sulfate (Etimicin Sulfate, also known as antibiotic 89-07, adamicin) is a new generation of semi-synthetic aminoglycoside antibiotics with high efficiency, low toxicity and resistance to drug-resistant bacteria. Its chemical name is 1-N - Ethyl gentamicin C1a sulfate. For details on its specific structure and properties, please refer to China Pharmacopoeia. [0003] In the patent application CN 1100467A, etimicin sulfate inventor Zhao Min et al. reported the chemical structure, preparation method, pharmaceutical dosage form and pharmacological research results of the new drug. However, its preparation method is relatively rough. Although macroporous adsorpti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/236C07H1/00C07H1/06
Inventor 李继安封成军陈舟舟陈代杰李兴刚蓝鸿
Owner SHANGHAI INST OF PHARMA IND CO LTD
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