Separation and purification method of docetaxel
A docetaxel, separation and purification technology, applied in the field of high-efficiency separation and purification of docetaxel, can solve the problems such as the purification method's purity and yield need to be further improved, and achieve stable yield, high yield and mobile phase quantity. saving effect
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Embodiment 1
[0039] 1) Take the crude product of docetaxel with a purity of 97%, add dichloromethane to dissolve it, and obtain a docetaxel solution with a concentration of 50 mg / mL; use;
[0040] 2) Use a 50×250mm chromatographic column, UniSil normal phase silica gel (produced by Suzhou Nawei Technology Co., Ltd.) as the chromatographic column filler, and the column volume is 490mL; pre-column pretreatment of the chromatographic column, first use ethyl acetate Ester carries out impurity removal, after using volume ratio is dichloromethane: the mobile phase of ethyl acetate=9:1 balances; Then sample injection, sample liquid is 1) described filtrate; Then adopting volume ratio is dichloromethane: The mixed solution of ethyl acetate=9:1 was used as the mobile phase to elute for 240min, and the flow rate was controlled at 60mL / min;
[0041] 3) The solution of the target peak was collected in sections, and the components meeting the requirements were summarized. After analysis by high perfor...
Embodiment 2
[0044] 1) Take the crude product of docetaxel with a purity of 97%, add dichloromethane to dissolve it, and obtain a docetaxel solution with a concentration of 50 mg / mL; use;
[0045] 2) Use a 50×250mm chromatographic column, UniSil normal phase silica gel (produced by Suzhou Nawei Technology Co., Ltd.) as the chromatographic column filler, and the column volume is 490mL; pre-column pretreatment of the chromatographic column, first use ethyl acetate Esters were used to remove impurities, and then equilibrated with a mobile phase with a volume ratio of dichloromethane:ethyl acetate=8.5:1.5. Then adopting volume ratio is dichloromethane: the mobile phase of ethyl acetate=8.5:1.5 carries out elution 240min, and flow velocity is controlled at 60ml / min;
[0046] 3) Collect the solution of the target peak in sections, summarize the component solutions that meet the requirements, and analyze by high performance liquid chromatography, the purity of docetaxel in the eluent is 99.56%, ...
Embodiment 3
[0048] The difference between this example and Example 1 is that the organic solution for dissolving the docetaxel sample is ethyl acetate, and the others are the same as those in Example 1.
[0049] The solution of the target peak was collected in sections, and the components meeting the requirements were summarized. After analysis by high performance liquid chromatography, the purity of docetaxel in the eluent was 99.51%, and the yield was 95.2%.
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