CN108467373A - A method of extracting taxol and 10-DAB III simultaneously from Chinese yew - Google Patents

A method of extracting taxol and 10-DAB III simultaneously from Chinese yew Download PDF

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Publication number
CN108467373A
CN108467373A CN201810491721.5A CN201810491721A CN108467373A CN 108467373 A CN108467373 A CN 108467373A CN 201810491721 A CN201810491721 A CN 201810491721A CN 108467373 A CN108467373 A CN 108467373A
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China
Prior art keywords
taxol
extraction
dab iii
chinese yew
extracting
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Application number
CN201810491721.5A
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Chinese (zh)
Inventor
李志良
李海池
葛发欢
张湘东
叶岸青
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MEIZHOU ZHONGDA MEDICAL DEVELOPMENT Co Ltd
Guangzhou Zhongda Nansha Technology Innovation Industrial Park Co Ltd
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MEIZHOU ZHONGDA MEDICAL DEVELOPMENT Co Ltd
Guangzhou Zhongda Nansha Technology Innovation Industrial Park Co Ltd
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Priority to CN201810491721.5A priority Critical patent/CN108467373A/en
Publication of CN108467373A publication Critical patent/CN108467373A/en
Withdrawn legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D305/00Heterocyclic compounds containing four-membered rings having one oxygen atom as the only ring hetero atoms
    • C07D305/14Heterocyclic compounds containing four-membered rings having one oxygen atom as the only ring hetero atoms condensed with carbocyclic rings or ring systems

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Epoxy Compounds (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
  • Medicines Containing Plant Substances (AREA)

Abstract

The method that the invention discloses a kind of to extract taxol and 10 DAB III simultaneously from Chinese yew, branches and leaves of yew is crushed to powder, Extraction solvent is added to impregnate, mixed liquor is injected into extraction 1~3 time in broken extraction element, extraction is crushed under cryogenic high pressure, taxol and 10 DAB III are added in Extraction solvent rapidly, are the extracting solution of taxol and 10 DAB III using supernatant and sediment, gained supernatant is centrifuged.The present invention can extract taxol and 10 DABIII simultaneously by cryogenic high pressure in a technical process, and the recovery rate of gained taxol and 10DABIII are up to 96%.The method of the present invention has many advantages, such as that stability is good, easy to operate, preparation time is short, and extraction efficiency is high, safe and non-toxic, simultaneously effective avoids taxol and 10DABIII by oxidative degradation.

Description

A method of extracting taxol and 10-DAB III simultaneously from Chinese yew
Technical field
The present invention relates to Chinese medicine chemical composition extractive technique fields, and in particular to one kind extracting purple simultaneously from Chinese yew The method of China fir alcohol and 10-DAB III.
Background technology
Bearing taxanes are a kind of chemical combination at the positions such as bark, root and the leaf for being extracted from high gymnosperm Chinese yew Object mainly contains taxol, 10-DAB III etc., there are many having been demonstrated with cytotoxicity and antitumor activity, and for carrying Take the natural taxus resource of taxol etc. limited, thus the production and supply of natural Japanese yew raw polyol medicine is restricted, much The application of taxol clinic cannot be met.Present people's large-scale plantation Chinese yew, therefrom extracts taxol, 10-DAB III etc. How taxane substances, make full use of resource taxus resource, therefrom obtains more active principles and is of great significance.It is existing The method for having extraction taxanes active ingredient, as application No. is the " a kind of using super of CN201410676291.6 for granted patent Application No. is " the one of CN201510299837.5 for the method that sound wave extracts taxol from Chinese yew " patent and granted patent The method of kind extraction separation 10- deacetylates baccatin III (10-DAB III) from Chinese yew ".General taxanes active ingredient Extracting method include:Crude extract → process-scale chromatography separation → crystallization → liquefaction → normal-phase chromatography is made in leaching → degreasing → extraction Separation.These methods are not taxol and 10-DABIII to be extracted in the same technological process, therefore increase technique Difficulty also increases process costs.
Taxol and the method for 10-DABIII can be extracted simultaneously in a technical process therefore, it is necessary to a kind of, improved The purity of taxol and 10-DABIII, simple for process, rapid and stability is good, saves economic cost.
Invention content
In order to solve the above the deficiencies in the prior art, the present invention one kind is disclosed from Chinese yew and meanwhile extract taxol and The method of 10-DABIII can extract taxol and 10-DABIII simultaneously in a technical process, and this method is easy to operate, Cost is relatively low, resin can Reusability, also, the purity of gained taxol and 10-DABIII are up to 96% or more.
The purpose of the present invention will be realized by following technical method:One kind extracting taxol and 10- simultaneously from Chinese yew Branches and leaves of yew is crushed to powder by the method for DAB III, and Extraction solvent is added and impregnates, mixed liquor is injected into broken extraction element Interior extraction 1~3 time, is crushed extraction under cryogenic high pressure, and taxol and 10-DAB III be added in Extraction solvent rapidly, using from It is the extracting solution of taxol and 10-DAB III that the heart, which detaches supernatant and sediment, gained supernatant,.
Preferably, a kind of method for extracting taxol and 10-DAB III simultaneously from Chinese yew, the Chinese yew Branches and leaves are crushed to 50~200 mesh.
Preferably, a kind of method for extracting taxol and 10-DAB III simultaneously from Chinese yew, the Chinese yew Branches and leaves are crushed to 100 mesh.
Preferably, a kind of method for extracting taxol and 10-DAB III simultaneously from Chinese yew, the extraction are molten Agent is the ethyl alcohol of volume fraction 60~100%.
Preferably, a kind of method for extracting taxol and 10-DAB III simultaneously from Chinese yew, the extraction are molten Agent is the ethyl alcohol of volume fraction 80%.
Preferably, a kind of method for extracting taxol and 10-DAB III simultaneously from Chinese yew, the low temperature are high It crushes in broken extraction process, cracking pressure is 50~200MPa, and breaking temperature is 4~16 DEG C.
Preferably, a kind of method for extracting taxol and 10-DAB III simultaneously from Chinese yew, the low temperature are high It crushes in broken extraction process, cracking pressure 125MPa.
Preferably, a kind of method for extracting taxol and 10-DAB III simultaneously from Chinese yew, the Chinese yew Solid-liquid ratio with Extraction solvent is 1:10~50 (g/ml).
Preferably, a kind of method for extracting taxol and 10-DAB III simultaneously from Chinese yew, the Chinese yew With the solid-liquid ratio 1 of Extraction solvent:20.
Preferably, a kind of method for extracting taxol and 10-DAB III simultaneously from Chinese yew, it is characterised in that: The mixed liquor is injected into extraction 2 times in broken extraction element, and solution is poured into broken extraction element again after the completion of to be extracted Interior extraction.
Compared with prior art, the present invention has following advantageous effect:The present invention can be at one by cryogenic high pressure Taxol and 10-DABIII are extracted simultaneously in technical process, and the recovery rate of gained taxol and 10-DABIII are up to 96%.The method of the present invention has many advantages, such as that stability is good, easy to operate, preparation time is short, and extraction efficiency is high, safe and non-toxic, together When be effectively prevented from taxol and 10-DABIII by oxidative degradation.
Description of the drawings
Fig. 1 is the high-efficient liquid phase chromatogram of extracting solution in the embodiment of the present invention 3.
Specific implementation mode
To more fully understand the present invention, further specific elaboration is made to the present invention below by following embodiment, but not Limitation of the invention is can be regarded as, some are nonessential according to made by foregoing invention content for those skilled in the art It improves and adjusts, be also considered as being within the scope of the present invention.
Embodiment 1
First, branches and leaves of yew is crushed to 50 mesh, the ethyl alcohol that volume fraction 90% is added impregnates, Chinese yew powder with carry Take the solid-liquid ratio 1 of solvent:50(g/ml).Then, mixed liquor is injected into extraction in broken extraction element, and extraction temperature is 16 DEG C, Extracting pressure is 200MPa, and extraction is crushed under cryogenic high pressure, and rapid be added to of the taxol and 10-DAB III in Chinese yew carries It takes in solvent.Finally, it is the extraction of taxol and 10-DAB III using supernatant and sediment, gained supernatant is centrifuged Liquid.
Embodiment 2
First, branches and leaves of yew is crushed to 200 mesh, the ethyl alcohol that volume fraction 60% is added impregnates, Chinese yew powder with The solid-liquid ratio 1 of Extraction solvent:10(g/ml).Then, mixed liquor is injected into extraction in broken extraction element, it is to be extracted after the completion of again Solution is poured into broken extraction element and is extracted, continuous extraction 3 times, extraction temperature is 4 DEG C, extracting pressure 50MPa, low Under warm condition of high voltage, taxol and 10-DAB III in Chinese yew are added in Extraction solvent rapidly.Finally, using centrifugation Supernatant and sediment, gained supernatant are the extracting solution of taxol and 10-DAB III.
Embodiment 3
First, branches and leaves of yew is crushed to 100 mesh, the ethyl alcohol that volume fraction 80% is added impregnates, Chinese yew powder with The solid-liquid ratio 1 of Extraction solvent:20(g/ml).Then, mixed liquor is injected into broken extraction element, again will be molten after the completion of to be extracted Liquid is poured into extraction in broken extraction element, continuous extraction 2 times, and extraction temperature is 8 DEG C, extracting pressure 125MPa, in low temperature Extraction is crushed under high pressure, the taxol and 10-DAB III in Chinese yew are added in Extraction solvent rapidly.Finally, using centrifugation point From supernatant and sediment, gained supernatant is the extracting solution of taxol and 10-DAB III.
Embodiment 4
Liquid chromatogram inspection is carried out to the extracting solution of taxol and 10-DAB III in embodiment 1, embodiment 2, embodiment 3 respectively It surveys, and peak area is recorded according to the liquid chromatogram of detection, the peak area of active ingredient and the line of concentration in reference standards solution Sexual intercourse calculates the extracted amount of taxol and 10-DAB III in extracting solution.Again by taxol in Chinese yew (A) and 10-DAB III (B) content obtains the recovery rate of taxol (A) and 10-DAB III (B).Details as Follows table:
By above example 1, the data of embodiment 2 and embodiment 3, the recovery rate of taxol and 10-DAB III is calculated, Show that the average recoveries that the average recoveries of taxol are 96.02%, 10-DAB III are 96.76% respectively.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention With within principle, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention god.

Claims (10)

1. a kind of method for extracting taxol and 10-DAB III simultaneously from Chinese yew, it is characterised in that:By branches and leaves of yew powder It is broken to powder, Extraction solvent is added and impregnates, mixed liquor is injected into extraction 1~3 time in broken extraction element, is broken under cryogenic high pressure Broken extraction, taxol and 10-DAB III are added in Extraction solvent rapidly, using centrifuging supernatant and sediment, on gained Clear liquid is the extracting solution of taxol and 10-DAB III.
2. a kind of method for extracting taxol and 10-DAB III simultaneously from Chinese yew according to claim 1, feature It is:The branches and leaves of yew is crushed to 50~200 mesh.
3. a kind of method for extracting taxol and 10-DAB III simultaneously from Chinese yew according to claim 1, feature It is:The branches and leaves of yew is crushed to 100 mesh.
4. a kind of method for extracting taxol and 10-DAB III simultaneously from Chinese yew according to claim 1, feature It is:The Extraction solvent is the ethyl alcohol of volume fraction 60~100%.
5. a kind of method for extracting taxol and 10-DAB III simultaneously from Chinese yew according to claim 1, feature It is:The Extraction solvent is the ethyl alcohol of volume fraction 80%.
6. a kind of method for extracting taxol and 10-DAB III simultaneously from Chinese yew according to claim 1, feature It is:The cryogenic high pressure is crushed in extraction process, and cracking pressure is 50~200MPa, and breaking temperature is 4~16 DEG C.
7. a kind of method for extracting taxol and 10-DAB III simultaneously from Chinese yew according to claim 1, feature It is:The cryogenic high pressure is crushed in extraction process, cracking pressure 125MPa.
8. a kind of method for extracting taxol and 10-DAB III simultaneously from Chinese yew according to claim 1, feature It is:The solid-liquid ratio of the Chinese yew and Extraction solvent is 1:10~50 (g/ml).
9. a kind of method for extracting taxol and 10-DAB III simultaneously from Chinese yew according to claim 1, feature It is:The solid-liquid ratio 1 of the Chinese yew and Extraction solvent:20(g/ml).
10. a kind of method for extracting taxol and 10-DAB III simultaneously from Chinese yew according to claim 1, feature It is:The mixed liquor is injected into extraction 2 times in broken extraction element, and solution is poured into broken extraction again after the completion of to be extracted Extraction in device.
CN201810491721.5A 2018-05-22 2018-05-22 A method of extracting taxol and 10-DAB III simultaneously from Chinese yew Withdrawn CN108467373A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111167573A (en) * 2019-12-21 2020-05-19 普洱大华林业科技有限公司 High-efficient artificial cultivation of chinese yew improves collection system of taxol content
CN111253345A (en) * 2020-03-02 2020-06-09 东北林业大学 Method for extracting paclitaxel from branches and leaves of taxus chinensis
CN111253344A (en) * 2020-02-27 2020-06-09 东北林业大学 Method for extracting paclitaxel from branches and leaves of taxus chinensis

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111167573A (en) * 2019-12-21 2020-05-19 普洱大华林业科技有限公司 High-efficient artificial cultivation of chinese yew improves collection system of taxol content
CN111253344A (en) * 2020-02-27 2020-06-09 东北林业大学 Method for extracting paclitaxel from branches and leaves of taxus chinensis
CN111253345A (en) * 2020-03-02 2020-06-09 东北林业大学 Method for extracting paclitaxel from branches and leaves of taxus chinensis

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Application publication date: 20180831