A kind of extraction method of rapamycin
A technology of rapamycin and extraction method, which is applied in the field of separation and purification, can solve the problems of low yield, poor effect, low content and purity of sirolimus, etc., to overcome resin adsorption, small footprint, The effect of low cost
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Embodiment 1
[0037] 10L of fermented liquid containing rapamycin was cultured by microbial fermentation, adjusted to pH 5.1 with oxalic acid, and filtered to obtain 461.30g of filter cake; 1.5L of ethanol was added, extracted, filtered to obtain filtrate; ethanol was concentrated and recovered, and 0.6 Extract with L ethyl acetate, cool down to 3°C, add 0.4L of 3% sodium bicarbonate solution at 3°C, stir and wash, let stand, and separate layers; add pH 5.2, 0.5L of 3% ammonium acetate buffer solution, stir and wash After 1h, let stand, separate layers, concentrate and recover ethyl acetate, and obtain 38.91g of crude rapamycin. HPLC purity 45.72%.
[0038] Add 80ml of L-methyl lactate to the crude product, stir to dissolve, and filter; cool down to 0°C, add 300ml of ethyl propyl ether to crystallize dropwise while stirring, filter, wash with 30ml of ethyl propyl ether, and dry under reduced pressure to obtain 6.83g of rapamycin . The yield is 81.16%, the HPLC purity is 98.13%, and the ra...
Embodiment 2
[0040]10L of fermented liquid containing rapamycin was cultivated by microbial fermentation, adjusted to pH 4.8 with hydrochloric acid, and filtered to obtain 450.84g of filter cake; 0.9L of methanol was added, extracted, filtered to obtain filtrate; methanol was concentrated and recovered, and the mixture was added to Extract with 2.3L butyl acetate, cool down to 2°C, add 1.4L of 3% sodium bicarbonate solution at 2°C, stir and wash, let stand, and separate layers; add 1.4L of 3% ammonium acetate buffer solution with a pH value of 5.5, and stir Wash for 1 h, let stand, separate layers, concentrate and recover butyl acetate to obtain 39.53 g of crude rapamycin. HPLC purity 41.84%. Add 65ml of L-methyl lactate to the crude product, stir to dissolve, and filter; cool down to 5°C, add 130ml of diethyl ether to crystallize dropwise with stirring, filter, wash with 30ml of diethyl ether, and dry under reduced pressure to obtain 6.52g of rapamycin. The yield is 77.50%, the HPLC puri...
Embodiment 3
[0042] 10L of fermented liquid containing rapamycin was cultivated by microbial fermentation, adjusted to pH 5.5 with phosphoric acid, and filtered to obtain 466.25g of filter cake; 2.6L of isopropanol was added, extracted, filtered to obtain filtrate; concentrated recovery of isopropanol, Add 0.46L of dichloromethane to the mixture for extraction, cool down to 4°C, add 0.23L of 3% sodium bicarbonate solution at 4°C, stir and wash, let stand, and separate layers; add pH 4.8, 3% ammonium acetate buffer solution 0.23 L, stirring and washing for 1 h, standing still, separating layers, concentrating and recovering dichloromethane, and obtaining 37.21 g of crude rapamycin. HPLC purity 46.73%. Add 470ml of L-methyl lactate to the crude product, stir to dissolve, and filter; cool down to -8°C, add 1880ml of diethyl ether to crystallize dropwise with stirring, filter, wash with 30ml of diethyl ether, and dry under reduced pressure to obtain 2.55g of rapamycin. The yield is 30.30%, th...
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