A kind of purification method of teicoplanin
A technology of teicoplanin and purification method, applied in the field of chemistry, can solve problems such as no research or report
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Embodiment 1
[0029] Purification by state-of-the-art methods
[0030] Take 1L of the teicoplanin eluate obtained from the fermentation broth through the macroporous resin column HZ801 (the potency is 81.085mg / ml, and the effective peak area is 73.7% and the peak area of other impurities is 10.2% by HPLC analysis) . Adjust the pH to 4.0, add 10 g of activated carbon, stir at a medium speed at 45°C for 30 minutes, filter off the activated carbon to obtain 887 ml of a clear filtrate, the titer of the clear liquid is 69.602 mg / ml, and contains 61.737 g of teicoplanin. Add 60 g of NaCl to the clarified filtrate while stirring. After all the NaCl is dissolved, adjust the pH to 4.5 with 1M HCl solution, continue to stir for 60 min, let stand at 4°C for 24 h, filter and wash the crystals with water to obtain the wet crude product of teicoplanin, 40 ℃ vacuum drying to obtain coarse powder 51.489g. The sample yield was 63.5%, among which the crystallization process yield was 83.40%. The specifi...
Embodiment 2
[0032] Take 1L of the teicoplanin eluent obtained from the fermentation broth through the macroporous resin column HZ801 (the potency is 81.085 mg / ml, and the effective peak area is 73.7% and the peak area of other impurities is 10.2% by HPLC analysis) . Adjust the pH to 4.0, add 10 g of activated carbon, stir at a medium speed at 45°C for 30 minutes, filter off the activated carbon to obtain 859 ml of a clear filtrate, the titer of the clear liquid is 68.598 mg / ml, and contains 58.926 g of teicoplanin. Put the clarified filtrate into a freeze-drying tray and put it into a vacuum freeze dryer. The sample is pre-frozen at a freezing rate of 40°C / h to -42°C and then kept for 4 hours. The heating rate of ℃ / h is slowly heated to -12 ℃ for sublimation drying, the temperature curves of the samples overlap, and the interface between the dry layer and the frozen layer reaches the bottom of the plate and disappears, and then keep warm for 2 hours. Afterwards, heat-desorption drying wa...
Embodiment 3
[0034] For further purification, 50 g of the teicoplanin coarse powder obtained in the above-mentioned Example 2 was dissolved to 20,000 units with 2.5 L of pure water, and the polyamide resin was eluted with 30% ethanol aqueous solution of pH 4.0, and the collected eluted Liquid 2.15L, titer is 21.749mg / ml. Add 20 g of activated carbon for needles, stir at a medium speed at 45°C for 30 minutes, filter off the activated carbon to obtain 2 L of clarified filtrate, the titer of the clear liquid is 19.618 mg / ml, and contains 39.236 g of teicoplanin. After decolorization, put it into a freeze-drying tray, put it into a vacuum freeze-drying machine, and follow the method in Example 2 to obtain 38.255 g of teicoplanin fine powder, with a sample yield of 76.51%, of which the freeze-drying process yield was 97.49%. The specific titer of the sample was 1073U / mg. After HPLC analysis, the effective peak area was 94.5%, and the peak area of other impurities was 2.9%. Freeze-dried powd...
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