A kind of aminoglycoside compound and its extraction and separation method

A compound, ammonia water technology, applied in chemical instruments and methods, sugar derivatives, sugar derivatives, etc., can solve problems such as no patents or literature reports, difficult to purify, etc.

Active Publication Date: 2016-01-20
WUXI JIYU SHANHE PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Etimicin sulfate is a multi-structural product, which is difficult to purify during production. The present invention discovers a new compound unexpectedly during the research and purification process of etimicin sulfate intermediates. So far, no patent has been found for this compound. or literature report

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
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Effect test

Embodiment 1

[0049] Take gentamicin C1a base powder and add DMSO to dissolve it, add cobalt acetate and acetic anhydride to obtain a synthetic solution, and add water to dilute the synthetic solution. Adsorbed on 732 cation exchange resin column and eluted with ammonia water. The eluate was concentrated, passed through hydrogen sulfide to precipitate cobalt ions, and filtered; the filtrate was spray-dried to obtain P1. Take P1, add water to dissolve, use H 2 SO 4 Adjust the pH, load the sample on the HD-2 weakly acidic cation exchange resin column, elute with water and ammonia water gradient respectively, and detect by TLC (developing solvent: chloroform-methanol-ammonia water, 1:1:1, lowerlayer, I 2 ) and combined fractions to obtain impurity-enriched fractions. The impurity-rich fractions were separated by column chromatography repeatedly using silica gel H (chloroform:methanol:ammonia water (2:1:1, lowerlayer) and CM-SephadexC-25), and the fourth fraction was collected as the compoun...

Embodiment 2

[0050] Embodiment 2, the preparation of hydrochloride:

[0051] Take gentamicin C1a base powder and add DMSO to dissolve it, add cobalt acetate and acetic anhydride to obtain a synthetic solution, and add water to dilute the synthetic solution. Adsorbed on 732 cation exchange resin column and eluted with ammonia water. The eluate was concentrated, passed through hydrogen sulfide to precipitate cobalt ions, and filtered; the filtrate was spray-dried to obtain P1. Take P1, add water to dissolve, use H 2 SO 4 Adjust the pH, load the sample on the HD-2 weakly acidic cation exchange resin column, elute with water and ammonia water gradient respectively, and detect by TLC (developing solvent: chloroform-methanol-ammonia water, 1:1:1, lowerlayer, I 2 ) and combined fractions to obtain impurity-enriched fractions. The impurity-rich fractions were separated by column chromatography repeatedly using silica gel H (chloroform:methanol:ammonia water (2:1:1, lowerlayer) and CM-SephadexC...

Embodiment 3

[0052] Embodiment 3, the preparation of sulfate:

[0053] Take gentamicin C1a base powder and add DMSO to dissolve it, add cobalt acetate and acetic anhydride to obtain a synthetic solution, and add water to dilute the synthetic solution. Adsorbed on 732 cation exchange resin column and eluted with ammonia water. The eluate was concentrated, passed through hydrogen sulfide to precipitate cobalt ions, and filtered; the filtrate was spray-dried to obtain P1. Take P1, add water to dissolve, use H 2 SO 4 Adjust the pH, load the sample on the HD-2 weakly acidic cation exchange resin column, elute with water and ammonia water gradient respectively, and detect by TLC (developing solvent: chloroform-methanol-ammonia water, 1:1:1, lowerlayer, I 2 ) and combined fractions to obtain impurity-enriched fractions. The impurity-rich fractions were separated by column chromatography repeatedly using silica gel H (chloroform:methanol:ammonia water (2:1:1, lowerlayer) and CM-SephadexC-25), ...

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PUM

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Abstract

The invention relates to an aminoglycoside substance and an extracting and separating method thereof. The compound is separated from etimicin sulfate, and has a structural formula shown in the specification. The invention further relates to a separating method of the aminoglycoside substance.

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): C07H15/236C07H1/06A61K31/7036A61P31/04
Inventor 吴凌云夏冰许盛
Owner WUXI JIYU SHANHE PHARM CO LTD
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