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A kind of purification method of tedirosine crude product

A new technology of Tidelotide and purification method, which is applied in chemical instruments and methods, organic chemistry, sugar derivatives, etc., to achieve low production costs, reduce environmental pressure, and enhance competitiveness

Active Publication Date: 2017-02-22
宁夏泰瑞制药股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, there is no domestic literature report on the purification and removal of impurities

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Add 10 kg of Tedirosin crude product, add a hydrochloric acid solution with a volume concentration of 10%, dissolve to obtain a Tedirosin solution, adjust its pH 3, and the volume of the Tedirosin solution is 600 L.

[0035] Add 40kg of adsorbent (filler) Y-type activated alumina to the packed column, and the aspect ratio of the packed column is 4:1. Add 160L of methanol to wash the adsorbent, repeat 2 times. Wash the adsorbent with deionized water at a flow rate of 50 L / h until the effluent is free of methanol. The Tedirosin solution was passed through the packed column for adsorption treatment in a two-effect series mode. The flow rate of the Tedirosin solution was controlled at 180L / h, the solution temperature was controlled at 20°C, and the filtered solution was collected. The Tedirosin content was 0.28%. Add 1800L of methanol into the packed column, control the flow rate at 300L / h, and collect 1750L of desorption liquid.

[0036] Add 2625L of purified water to th...

Embodiment 2

[0038] Add 10 kg of tadirosin crude product, add a sulfuric acid solution with a volume concentration of 12%, dissolve to obtain tadirosin solution, adjust its pH4, and the volume of tadirosin solution is 700L.

[0039] Add 50 kg of adsorbent (filler) silica gel into the packed column, and the height-to-diameter ratio of the packed column is 5:1. Add 250L of ethanol to wash the adsorbent, repeat 2 times. The adsorbent was washed with deionized water at a flow rate of 60 L / h until the effluent was free of ethanol. The Tedirosin solution was passed through the packed column for adsorption treatment in a two-effect series mode. The flow rate of the Tedirosin solution was controlled at 190L / h, and the solution temperature was controlled at 23°C. The filtered solution was collected and the Tedirosin content was 0.24%. Add 2450L of ethanol to the packed column, control the flow rate at 350L / h, and collect 2400L of desorption liquid.

[0040] Add 4350L of purified water to the anal...

Embodiment 3

[0042] Add 15% hydrochloric acid solution to 10 kg of Tedirosin crude product, dissolve to obtain Tedirosin solution, adjust its pH to 4.5, and the volume of Tedirosin solution is 800 L.

[0043] Add 60kg of adsorbent Y-type activated alumina into the packed column, add 360L of methanol to wash the adsorbent, and repeat 3 times. Wash the adsorbent with deionized water at a flow rate of 75 L / h until the effluent is free of methanol. The Tedirosin solution was passed through the packed column for adsorption treatment in a two-effect series mode. The flow rate of the Tedirosin solution was controlled at 200L / h, and the solution temperature was controlled at 25°C. The filtered solution was collected and the Tedirosin content was 0.19%. Add 3200L of acetone to the packed column, control the flow rate at 400L / h, and collect 3100L of desorption liquid.

[0044]Add 6200L of purified water to the analysis solution, control the pH at 6.8, control the temperature at 75°C, and control th...

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Abstract

The invention relates to a method for purifying a crude Tildipirosin product. The method comprises the processing steps of acidifying, dissolving, adsorbing, desorbing, crystallizing, washing and drying the crude Tildipirosin product to obtain a pure Tildipirosin product. The method provided by the invention is used for effectively separating Tildipirosin impurities, improving the quality of a finished product of Tildipirosin and helping to enhance the market competitiveness of the product at home and abroad.

Description

technical field [0001] The invention belongs to the technical field of antibiotic extraction, in particular to a method for purifying crude tedirosin. Background technique [0002] Tylosin is the latest animal-specific macrolide semi-synthetic antibiotic developed by the foreign company Intervet-Schering-Plough, and it is a derivative of tylosin. On March 8, 2011, the European Commission for Veterinary Medicines (CVMP) approved the market authorization application of Intervet's sterile injection solution (trade name Zuprevo) with Tedirosin as the main component, and will subsequently The EU countries have successively approved the listing. The new CAS number of Tedrol is 328898-40-4 and the molecular formula is C 41 h 71 N 3 o 8 , molecular weight 734.02, melting point 192°C, soluble in polar organic solvents (such as methanol, acetone, etc.), slightly soluble in water. [0003] Tedirosin is a broad-spectrum antibacterial drug, which has antibacterial activity against ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/08C07H1/06
CPCC07H1/06C07H17/08
Inventor 任勇
Owner 宁夏泰瑞制药股份有限公司
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