Improved extraction method for tylosin
A technology of tylosin and extraction method, applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., can solve the problems of high loss of tylosin, low product yield, high impurity content, etc.
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example 1
[0021] Example 1. Using butyl acetate (BA) to extract tylosin (TL) from fermentation filtrate
[0022] This extraction method is the tylosin extraction process used in the current factory. The extraction process is as follows:
[0023] The fermentation filtrate, pH 6.21, with a titer of 6500-6800 μg / ml, was adjusted to pH 8.41 with 40% NaOH, and BA was added to stir to extract TL. Dosage per extraction: fermentation filtrate / BA=100 / 30 (volume / volume, v / v)
[0024] Results: The residual titer of the aqueous phase after the first extraction: 1150μg / ml, the extraction rate of tylosin: 83.05%;
[0025] The residual titer of the aqueous phase after the second extraction: 521μg / ml, the total extraction rate of the two times: 92.32%.
example 2
[0026] Example 2: Extraction of Tylosin (TL) with 3.85% Trichloromethane (TT) / Butyl Acetate (BA)
[0027] (1) Fermentation filtrate for experiment, with a titer of 6500-6800μg / ml and a pH of 6.21. Take 200ml fermentation filtrate and use saturated Na 2 CO 3 Adjust the pH of the aqueous solution from 6.90 to 6.98 and place it in a 35°C water bath to increase the temperature of the fermentation filtrate to 30 to 33°C.
[0028] (2) Take it out at room temperature and under stirring conditions, adjust the pH to 8.2-8.5.
[0029] (3) Pour into a 250ml separatory funnel, add 8ml TT / BA (3:1), mix well and let stand for about 2 hours, completely layer, release the lower layer, and then use 8ml TT / BA (3:1) for the upper layer Perform a second extraction.
[0030] (4) Combine the extracts of the lower layer twice, centrifuge, wash the precipitate with a small amount of TT, centrifuge, pour the supernatant and combine the extract after centrifugation, and dehydrate with anhydrous sodium sulfate...
example 3
[0037] Example 3. Extract TL with 5.7% TT / BA (3:1)
[0038] (1) Fermentation filtrate, pH 6.37, adjust the pH to 6.98, and raise the temperature of the fermentation broth to 30°C in a 35°C water bath.
[0039] (2) Take 200ml, 30℃, pH 6.98 fermentation filtrate, and use saturated Na 2 CO 3 The pH of the aqueous solution was adjusted to 8.44.
[0040] (3) In a 250ml separatory funnel, add 12ml TT / BA (3:1), mix well for extraction, stand for 2.5 hours, completely separate, take 0.5ml upper layer, add 4.5ml of water, and analyze by HPLC.
[0041] (4) The pH of the upper aqueous phase is 7.97, and 12ml TT / BA (3:1) is added for the second extraction.
[0042] (5) Take 200ml of new fermentation filtrate, adjust the pH to 6.9, heat it to 30°C (pH 6.70) of the fermentation broth at 35°C, and use saturated Na 2 CO 3 (About 5ml) adjust the pH to 8.67, add the second extraction ester phase liquid in item (4) to carry out the first extraction of this batch (using the second extraction solvent).
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