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Purification method for Tylosin

A technology of tylosin and purification method, which is applied in chemical instruments and methods, organic chemistry, preparation of sugar derivatives, etc., and can solve problems such as high cost, large amount of petroleum ether, and incomplete removal of impurities

Active Publication Date: 2009-10-28
河北威远药业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that the amount of petroleum ether is large, the cost is high, and the removal of impurities is not complete, and further purification is required
Therefore, this method has not been used to produce

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0037] Example one, extract tylosin (TL) from fermentation filtrate with chloroform

[0038] 1. Fine filtration of fermentation filtrate: fine filtration with a 0.2-1 μm filter.

[0039] 2. Adjust pH: adjust the pH of the filtrate to 8.5 (at 20-25° C.) with 40% NaOH.

[0040] 3. Extraction: TL was extracted twice with chloroform (TT).

[0041] 3.1 First pass extraction

[0042] 3.1.1 The amount of chloroform: fine filtrate: chloroform = 100: 4 ~ 6

[0043] 3.1.2 Extraction conditions: 20-25°C, pH 7.8-8.5, fully stirred and extracted for 20-30 minutes.

[0044] 3.1.3 Phase separation:

[0045] After the first extraction is completed, the liquid is completely pressed into the phase separation tank, and the phases are left to separate. After the phase separation is completed, the lower chloroform phase and the upper aqueous phase are further centrifuged with a centrifuge to obtain the first extraction. and the aqueous phase after the first extraction.

[0046]3.2 Second ext...

example 2

[0073] Example two, extract tylosin (TL) from fermentation filtrate with dichloromethane

[0074] 1. Fine filtration of fermentation filtrate: filter with 1-0.2 μm filter to obtain fine filtrate.

[0075] 2. Extract TL:

[0076] 2.1 Fine filtrate pH: fine filtrate with saturated Na 2 CO 3 solution or use 20% NaOH solution to adjust the pH to 8.0-8.5 (adjust the pH while stirring at 20-25°C).

[0077] 2.2 Dichloromethane dosage: fine filtrate: dichloromethane = 100:4

[0078] 2.3 First extraction:

[0079] Extract TL with dichloromethane for about 20 to 30 minutes at 20 to 25°C under the condition of thorough mixing.

[0080] Note: It is best to carry out the extraction in a special extraction tank with reasonable structure.

[0081] 2.4 Separation of the first extract:

[0082] After 20-30 minutes of extraction, press the liquid into a special phase-separation tank, let it stand for 30-60 minutes, and centrifuge to separate the phases to obtain the aqueous phase liquid ...

example 3

[0109] Example 3. Small laboratory experiment

[0110] 1. Take 3000ml of fermented filtrate with a titer of 8700 μg / ml (component A, determined by HPLC method), and use saturated Na 2 CO 3 Adjust the pH to 8.2.

[0111] 2. Add 120ml of chloroform, stir (254rpm) and extract for 30 minutes.

[0112] 3. Centrifuge (3000rpm) to separate the phases, and separate the lower chloroform phase; add 120ml chloroform to the upper aqueous phase, perform the second extraction, centrifuge, and separate the phases to obtain the second extract.

[0113] Note: The second extraction of large production is applied mechanically

[0114] 4. Combine the first and second extracts, dehydrate with anhydrous sodium sulfate, then distill at 55~58°C and -0.08~-0.1mPa to remove chloroform, and obtain a concentrate of about 10~11g .

[0115] 5. Dissolve the concentrate with 60 ml of phosphoric acid aqueous solution (pH 3.3) to obtain an aqueous solution containing tylosin phosphate.

[0116] 6. Add 30...

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PUM

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Abstract

The invention relates to a purification method for tylosin. The invention describes the post treatment of the extraction liquid of tylosin when chloroform is used for extracting the tylosin from fermentation filter liquid, i.e. a purification method. The essential of the method is as follows: the extraction liquid is concentrated into a condition that chloroform is basically removed; a condensateis dissolved by acid water; butyl acetate or toluene or 4-methyl-2-pentanone is added; the pH value is adjusted to 7.5-9.5 by alkali liquid, and extraction and phase splitting are sequentially performed; and a tartaric acid aqueous solution or a phosphoric acid aqueous solution is added to an ester phase for performing back extraction, back extraction liquid is obtained and is sprayed and dried, or the pH value of the back extraction liquid is adjusted to 7.5-10.5, and the back extraction liquid is pressed and filtered or centrifugated to obtain the tylosin.

Description

technical field [0001] The invention relates to antibiotic refining technology. It specifically relates to the refining technology of tylosin, and is a method for purifying tylosin. Background technique [0002] Tylosin is a special antibiotic for livestock and poultry, which is a fermentation product of Streptomyces freundii. At present, liquid submerged fermentation is used at home and abroad. After the fermentation liquid is treated with a flocculant (such as aluminum sulfate or aluminum chloride), the fermentation filtrate is obtained through solid-liquid separation. The fermentation filtrate is subjected to liquid-liquid extraction with butyl acetate to obtain an ester phase liquid. , the tartaric acid or tylosin phosphate can be obtained by back-extracting, concentrating and spray-drying the ester phase liquid. [0003] Using butyl acetate to extract tylosin from the fermentation filtrate has the following two disadvantages: [0004] 1. The amount of butyl acetate (...

Claims

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Application Information

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IPC IPC(8): C07H17/08C07H1/06
Inventor 王玉万潘贞德戴晓曦
Owner 河北威远药业有限公司
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