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.
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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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