Method for high efficiency separating and purifying 1-deacetyl Baccatins III (10-DABIII)
A technology of separation, purification and deacetylation, which is applied in the direction of organic chemistry, can solve problems such as yield loss, large solvent consumption, and reduced solvency, so as to improve the separation degree and separation peak shape, increase yield and purity, and demand Reduced effect
Patent Information
- Authority / Receiving Office
- CN · China
- Current Assignee / Owner
- Publication Date
- 2007-10-03
- Estimated Expiration
- Not applicable · inactive patent
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Abstract
Description
technical field
[0001] The present invention belongs to the technology of extracting medicinal substances from Taxus chinensis, especially the separation and purification of the semi-finished product 10-deacetylbaccatin III (interpreted as: 10-DAB III) extracted from Taxus chinensis into a high-purity fine product Methods. Background technique
[0002] 10-Deacetylbaccatin III (10-DAB III), as a structural monomer mainly present in Taxus species, can be used as the precursor of semi-synthetic antineoplastic drugs paclitaxel and docetaxel. Paclitaxel and docetaxel have been clinically used in the treatment of breast cancer, ovarian cancer, lung cancer, etc., with good curative effect and low side effects, and have gradually become the first-line anti-tumor drugs. As the number of cancer patients increases year by year, the demand for paclitaxel and docetaxel is increasing day by day, and the demand for their raw materials is even greater. In the...
Examples
Embodiment 1
[0031] Embodiment 1, the raw material of semi-finished product 10-deacetylbaccatin III is low content, and the method for sample dissolution and separation and purification has tetrahydrofuran
[0032] Take by weighing 100 grams of 10-DAB III raw material powder with a content of 23%, prepare a chromatographic column with a dynamic axial compression liquid phase of 100mm, the packing is spherical silica gel of 20-45um, and the aperture is 70A, and a total of 1650 grams of packing ( 10-DABIII: the weight ratio of packing is about 1.40%), the separation chromatographic column is 40cm long, and the mobile phase is 22:77:1=tetrahydrofuran:n-hexane:methanol (volume ratio).
[0033] Weigh 100 grams of 10-DAB III raw material powder with a content of 23%, use tetrahydrofuran at 50° C. to promote dissolution by ultrasonic waves, filter, and inject 50 grams of samples into the compressed liquid phase preparative chromatographic column each time. A mixed solution of tetrahydrofuran, n-h...
Embodiment 2
[0035] Example 2, the raw material of semi-finished product 10-deacetylbaccatin III has a high content, and the method for sample dissolution and separation and purification has tetrahydrofuran
[0036] Weigh 60 grams of 10-DAB III powder (content is 53%) of the raw material, prepare a chromatographic column with a dynamic axial compression liquid phase of 100mm, the packing is spherical silica gel of 20-45um, the aperture is 70A, and a total of 1650 grams are filled Packing (10-DAB III: the weight ratio of packing is about 1.92%), the length of separation chromatographic column is 35cm, and the mobile phase is 26:73:1=tetrahydrofuran:n-hexane:methanol (volume ratio).
[0037] Weigh 60 grams of 10-DAB III raw material powder with a content of 53%, promote dissolution with tetrahydrofuran at 55° C. by ultrasonic waves, filter, and inject 30 grams each time. A mixed solution of tetrahydrofuran, n-hexane and methanol is used as the mobile phase, and the separation time is 55 minu...
Embodiment 3
[0040] This embodiment is the same as the steps of embodiment 2, only THF:n-hexane:methanol (volume ratio)=30:68:2.