A kind of purification method of etimicin sulfate

A technology of etimicin sulfate and etimicin, applied in the field of medicine, can solve the problems of high impurity content, low purity of etimicin sulfate, etc., so as to improve the purity of finished products, increase the safety of clinical medication, and reduce adverse reactions. Effect

Active Publication Date: 2016-03-23
WUXI JIYU SHANHE PHARM CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The synthesis process reported in this patent has no purification operation in the final step, and the purity of the salt-forming precursor is only about 90%, resulting in low purity and high impurity content of the finished product etimicin sulfate
At present, there are no literature reports or patents on the purification of etimicin sulfate

Method used

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  • A kind of purification method of etimicin sulfate
  • A kind of purification method of etimicin sulfate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] Embodiment 1, preparation method of the present invention

[0052] Get the etimicin solution with a purity of more than 90% obtained through adsorption-type macroporous resin separation, concentrate to a concentration of 75%, and obtain the etimicin concentrate, add 30% concentration of 6mol / L dilute sulfuric acid to adjust to pH 5.8 to obtain the concentrated solution of etimicin sulfate, add 30% activated carbon, heat to 70°C, stir and keep for 1 hour, filter to obtain refined solution of etimicin sulfate, cool to 2°C, and use 0.1L / min Slowly add in 15L of solvent, the solvent contains 21% acetone, 15% methanol, 15% ethanol, 17% ether, 20% ethyl acetate, 12% methyl butanone, while stirring continuously, maintain the stirring speed at 280rpm, and The temperature was lowered to 4°C and maintained for 60 minutes to obtain a mother liquor rich in seed crystals. Cool the etimicin sulfate refined solution to 2°C, add it into the seed-rich mother liquor at a rate of 1L / min,...

Embodiment 2

[0053] Embodiment 2, preparation method of the present invention

[0054] Get the etimicin solution with a purity of more than 90% obtained through adsorption-type macroporous resin separation, concentrate to a concentration of 72%, obtain the etimicin concentrate, add 33% of the concentration to be 7mol / L dilute sulfuric acid to adjust to pH 5.9, to obtain the concentrated solution of etimicin sulfate, add 33% activated carbon, heat to 75 ° C, stir and keep for 1.5 hours, filter to obtain refined solution of etimicin sulfate, cool to 4 ° C, at 0.5 L / min Slowly add into 18L solvent, the solvent contains 5% water, 15% acetone, 10% methanol, 20% ethanol, 17% isopropanol, 21% hexane, 12% ether, while stirring continuously, maintain the stirring speed at 200rpm , and the temperature was lowered to 4° C., and maintained for 90 minutes to obtain a mother liquor rich in seed crystals. Cool the etimicin sulfate refined solution to 4°C, add it into the mother liquor rich in seed cryst...

Embodiment 3

[0055] Embodiment 3, preparation method of the present invention

[0056] Get the etimicin solution with a purity of more than 90% obtained through adsorption-type macroporous resin separation, concentrate to a concentration of 70%, obtain the etimicin concentrate, add 30% of the concentration to be 5mol / L dilute sulfuric acid to adjust to pH 4.5, to obtain etimicin sulfate concentrated solution, add 40% activated carbon, heat to 90 ° C, stir and keep for 2 hours, filter to obtain etimicin sulfate refined solution, cool to 6 ° C, with 0.3L / min Slowly add to 20L solvent, the solvent contains 8% water, 15% acetone, 15% methanol, 10% ethanol, 12% isopropanol, 15% ether, 10% methyl butanone, ethylene glycol monomethyl ether 15%, while stirring continuously, maintaining a stirring speed of 250 rpm, and cooling down to 6° C., maintaining for 120 min to obtain a mother liquor rich in seed crystals. Cool the etimicin sulfate refined solution to 6°C, add it into the mother liquor rich...

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Abstract

The invention belongs to the field of medicines and relates to a purifying method for etimicin sulfate. The purifying method for etimicin sulfate provided by the invention comprises the following steps: 1) taking an etimicin sulfate solution and concentrating into an etimicin sulfate concentrated solution; 2) adding dilute sulphuric acid into the etimicin sulfate concentrated solution, thereby obtaining an etimicin sulfate concentrated solution; 3) adding active carbon in the etimicin sulfate concentrated solution, heating, stirring and filtering, thereby obtaining an etimicin sulfate refined solution; 4) adding the etimicin sulfate refined solution in a solvent, and stirring, thereby obtaining a mother solution rich in seed crystals; 5) adding another batch of etimicin sulfate refined solution prepared according to the steps 1-3 in the mother solution rich in seed crystals obtained in the step 4, controlling the temperature and standing by, thereby obtaining a crystal mixture of the etimicin sulfate; 6) mashing and filtering the crystal mixture of the etimicin sulfate, thereby obtaining a wet crystal of the etimicin sulfate; and 7) drying the wet crystal of the etimicin sulfate, thereby obtaining a high-purity etimicin sulfate crystal.

Description

technical field [0001] The invention belongs to the field of medicine and relates to a method for purifying pharmaceutical compounds, in particular to a new method for purifying etimicin sulfate. Background technique [0002] Etimicinsulfate (Etimicinsulfate) is a new generation of semi-synthetic aminoglycoside antibiotics with high efficiency, low toxicity and resistance to drug-resistant bacteria with independent intellectual property rights. It is the only antibiotic that has obtained the national first-class new drug certificate. Infectious medicines. [0003] Etimicin sulfate injection is suitable for Escherichia coli, Klebsiella pneumoniae, Serratia spp., Citrobacter spp., Enterobacter spp., Acinetobacter spp., Proteus spp. Bacteria, Pseudomonas aeruginosa and Staphylococcus caused by various infections. Clinical studies have shown that this product has a good effect on the following infections: Respiratory tract infections: such as acute bronchitis, acute exacerbati...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H15/236C07H1/06
Inventor 吴凌云
Owner WUXI JIYU SHANHE PHARM CO LTD
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