Purification method of gentamicin C1a

A technology of gentamicin and purification method, which is applied in the field of refining pharmaceutical raw materials, can solve the problems of unpredictable purification effect and unpredictable separation effect, and achieve the effects of simplified steps, high purification yield and good purification effect

Active Publication Date: 2019-12-13
CHANGZHOU FANGYUAN PHARMA +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore the above method for a single gentamicin C 1a The purification effect of C 1 、C 1a 、C 2 、C 2a separation effect

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1）

[0021] Gentamicin C of the present embodiment 1a The purification method comprises the following steps:

[0022] ① Separation by macroporous adsorption resin column chromatography.

[0023] The HZ chromatographic filler NM100 chromatographic macroporous adsorption resin is pretreated, and the pretreatment is to soak the resin in 80% ethanol for 24 hours and then rinse it with purified water.

[0024] The pretreated resin was loaded into an atmospheric chromatography column with a column capacity of 300 mL and a height-to-diameter ratio of 4:1.

[0025] 9g gentamicin C 1a The crude product was dispersed in 100mL aqueous solution, and sodium hydroxide was added to adjust the pH to 10-12 to obtain a sample solution, and the gentamicin C in the sample solution 1a The purity is 92.5%.

[0026] Pass the gentamicin C1a sample solution through the column at a flow rate of 1 BV h -1 , the loading amount is 3g gentamicin C1a crude product / 100mL wet resin.

[0027] First rinse with...

Embodiment 2）

[0035] Gentamicin C of the present embodiment 1a The purification method all the other are identical with embodiment 1, difference is:

[0036] Step ① In the macroporous adsorption resin column chromatography separation process, when using dilute sulfuric acid water with a pH value of 1.6 for analysis, the analysis flow rate is 1.5 BV h -1 , Gentamicin C after column chromatography 1a The purity is 96%, and the yield of this step is 62.4%.

[0037] Step ② During the salting out and crystallization process:

[0038] Mix methanol and ethanol at a volume ratio of 1:2 to obtain mixed alcohols.

[0039] At 10°C, mix 70mL of mixed alcohol with 10mL of the solution obtained in step ① to mix evenly (volume ratio 7:1).

[0040] Add 0.52 mL of 98% concentrated sulfuric acid to the above mixture to adjust the pH to 6.5-6.7, stir magnetically at room temperature (20°C-25°C) for 3 hours, and solids are precipitated, which is the purified gentamicin C 1a .

[0041] Determination of Ge...

Embodiment 3）

[0043] Gentamicin C of the present embodiment 1a The purification method all the other are identical with embodiment 1, difference is:

[0044] Step ① During the separation process of the macroporous adsorption resin column chromatography, the HZ chromatographic filler NM200 chromatographic macroporous adsorption resin is pretreated. The pretreatment is to soak the resin in 80% ethanol for 24 hours and then rinse it with purified water.

[0045] When using dilute sulfuric acid water with a pH value of 2.0 for analysis, the analysis flow rate is 0.5 BV h -1 , Gentamicin C after column chromatography 1a The purity is 95.2%, and the yield of this step is 76%.

[0046] Step ② During the salting out and crystallization process:

[0047] Mix methanol and ethanol at a volume ratio of 1:2 to obtain mixed alcohols.

[0048] At 20°C-25°C, mix 70mL of mixed alcohol with 10mL of the solution obtained in step ① to mix evenly (volume ratio 7:1).

[0049] Add 0.52 mL of 98% concentrated...

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Abstract

The invention discloses a purification method of gentamicin C1a. The method comprises the following steps: (1) separation by macroporous adsorption resin column chromatography; and (2) salting out crystallization: mixing methanol and ethanol to obtain a mixed alcohol, mixing the mixed alcohol with the analytical solution of step (1) according to a volume ratio of 5:1-7:1, conducting magnetic stirring at 20-25 DEG C, a solid being precipitated, and the precipitated solid being purified gentamicin C1a. According to the present invention, a method of combining macroporous adsorption resin columnchromatography and salting out crystallization is adopted to achieve the purification of gentamicin C1a, the purity of gentamicin C1a is raised to 98% or above, and gentamicin C1a with high purity isobtained. The purification method of the invention has the advantages of simple steps, good purification effect, and high purification yield of gentamicin C1a.

Description

technical field [0001] The invention relates to the technical field of refining pharmaceutical raw materials, in particular to gentamicin C 1a purification method. Background technique [0002] In 1963, Weinstein of Schering Company in the United States isolated Gentamicin (Gentamicin) for the first time from Micromonas aculeatus. Gentamicin is one of the few heat-stable aminoglycoside alkaline antibiotics, stable in nature, soluble in water, insoluble in organic solvents such as ethanol and acetone. [0003] At present, there are mainly products related to gentamicin sulfate on the market, because of its broad antibacterial spectrum: against E. It has antibacterial effect on Gram-negative bacteria such as bacteria, certain achromogenous Rhine bacilli and Shigella, and it also has a strong antibacterial effect on Staphylococcus aureus among Gram-positive bacteria. Its antibacterial mechanism is to directly combine with the decoding region A of the 30S ribosomal subunit 16...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/236C07H1/06
CPCC07H15/236C07H1/06Y02A50/30
Inventor 陈代杰陈舟舟杨涛殷瑜刘鹏宇王海东刘昕钱军蒋艳君
Owner CHANGZHOU FANGYUAN PHARMA
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