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A kind of aminoglycoside compound and its extraction and separation method

A compound, the technology of etimicin sulfate, is applied in chemical instruments and methods, sugar derivatives, sugar derivatives, etc., and can solve problems such as difficult purification, side effects, and undiscovered problems

Active Publication Date: 2016-12-21
WUXI JIYU SHANHE PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Etimicin sulfate is a multi-structural product, which is difficult to purify during production, so that it is difficult to control the quality and has side effects. The present invention unexpectedly finds a new pure single-structure compound in the purification process. So far, no patents or literature reports have been found

Method used

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  • A kind of aminoglycoside compound and its extraction and separation method
  • A kind of aminoglycoside compound and its extraction and separation method
  • A kind of aminoglycoside compound and its extraction and separation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] Preparation of crude etimicin sulfate: O-2-amino-2,3,4,6-tetradeoxy-6-(amino)-a-D-erythro-hexapyranosyl-(1→4)-O -[3-Deoxy-4-C-methyl-3-(methylamino)-b-L-arabinopyranosyl-(1→6)-2-deoxy-N-ethyl-L-streptamine-5 / 2 sulfuric acid preparation

[0064] Gentamicin C1a base adds cobalt acetate and acetic anhydride to the solvent to generate 3,2,,6,-tri-N-acetyl gentamicin C1a (P1), which is extracted and concentrated, and hydrogen sulfide is added to the concentrated solution Gas to remove cobalt ions to obtain P1 with a purity of 90%-95%, then add acetaldehyde and hydrogenate with a reducing agent in an ice-water bath at 0-5°C to obtain 3,2,6,-tri-N-acetyl-1 -N ethyl gentamycin C1a (P2), after separation by adsorption macroporous resin, P2 with higher purity was obtained, and P2 with higher purity was added with 1N sodium hydroxide solution, hydrolyzed and refluxed for 48 hours, and the hydrolyzed solution was adsorbed The 1-N-ethylgentamycin C1a solution with a purity of mor...

Embodiment 2

[0067] Embodiment 2, the preparation of hydrochloride:

[0068] Get the etimicin sulfate crude product produced by the prior art, add water to dissolve, load the sample on HD-2 weakly acidic cation exchange resin column, use water respectively, ammoniacal liquor gradient elution, TLC detection (developing agent: chloroform-methanol-ammonia liquor , 1:1:1, lowerlayer, I2) and combined fractions to obtain impurity-enriched fractions. The impurity-enriched fractions were separated by column chromatography with silica gel H (chloroform:methanol:ammonia water (2:1:1, lower layer) and CM-SephadexC-25 repeatedly, and the fourth fraction was collected and concentrated to 200-500mg / ml, adjust the pH to 4.0-5.0 with 10mol / L hydrochloric acid, then add 2%-5% activated carbon, stir and decolorize at 60-80°C for 30 minutes, filter, and freeze-dry the filtrate to obtain the salt of the substance salt solid.

Embodiment 3

[0069] Embodiment 3, the preparation of sulfate:

[0070] Get the etimicin sulfate crude product produced by the prior art, add water to dissolve, load the sample on HD-2 weakly acidic cation exchange resin column, use water respectively, ammoniacal liquor gradient elution, TLC detection (developing agent: chloroform-methanol-ammonia liquor , 1:1:1, lowerlayer, I2) and combined fractions to obtain impurity-enriched fractions. The impurity-rich fractions were separated by column chromatography with silica gel H (chloroform:methanol:ammonia water (2:1:1, lower layer) and CM-SephadexC-25 repeatedly, and the fourth fraction was collected and concentrated to 200-500mg / ml, use 5mol / L sulfuric acid to adjust the pH to 4.0-5.0, then add 2%-5% activated carbon, stir and decolorize at 60-80°C for 30 minutes, filter, and freeze-dry the filtrate to obtain the sulfuric acid of the substance salt solids.

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Abstract

The invention relates to aminoglycoside compounds and an extraction and separation method therefor. The compounds are separated from etimicin sulfate and have a structural formula as described in the specification. The invention also relates to a separation method for the aminoglycoside compounds.

Description

technical field [0001] The invention relates to the field of medicinal chemistry, and relates to a chemical structure of an aminoglycoside compound and an extraction and separation method thereof. Background technique [0002] Aminoglycosides are glycosides formed by linking aminosugar and aminocycloalcohol through an oxygen bridge. There are natural aminoglycosides such as streptomycin from Streptomyces, gentamicin and other natural aminoglycosides from Micromonospora, and semi-synthetic aminoglycosides such as etimicin, all of which are broad-spectrum antibiotics. [0003] The effect of aminoglycoside antibiotics on bacteria is mainly to inhibit the synthesis of bacterial proteins, and the action point is at the A site of the 16SrRNA decoding region of the 30S ribosomal subunit of the cell. Studies have shown that such drugs can affect the entire process of bacterial protein synthesis, hinder the synthesis of the initial complex, induce bacteria to synthesize wrong protei...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H15/236C07H1/06C07H1/00A61K31/7036A61P31/04
Inventor 姜迎庆黄毅杨春艳陈环钱小燕
Owner WUXI JIYU SHANHE PHARM CO LTD
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