Method for extracting homoharringtonine

A technology of homoharringtonine and leaching, which is applied in the field of extracting homoharringtonine, can solve problems such as unfavorable amplification and industrialized production, high operation requirements, destroying ecological balance, etc., so as to reduce the subsequent purification process and ensure the extraction yield. rate, the effect of ensuring product quality

Inactive Publication Date: 2019-06-28
YUNNAN HANDE BIO TECH
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0004] There are 9 species of plants in the genus Haerringtonaceae, 8 of which are produced in my country; this genus contains a variety of alkaloids, namely harringtonine, homoharringtonine, isoharringtonine and Deoxyharringtonine; harringtonine has a significant anticancer effect, because of its use value and economic value, in recent years, a series of researches have been carried out on the chemical, pharmacological and clinical aspects of this genus of plants at home and abroad. Research work, vying for development, has extracted and isolated harringtonine and homoharringtonine from the cloverleaf plant for clinical application; but due to the limited resources of cloverleaf plants, the esters with anticancer activity The content of alkaloids is extremely low, so it is far from meeting the clinical needs; at present, my country mainly uses these trees as raw materials, and extracts active ingredients from them for clinical use; A large number of felling, resulting in several endangered species, and seriously disrupted the ecological balance
[0006] (1) Homoharringtonine exists in a very low amount in nature, and contains a lot of impurities, making it difficult to extract;
[0007] (2) At present, there are many extraction methods for homoharringtonine. Although some methods extract high purity products, the yield is very low and the production volume is small, so it cannot be popularized for industrial production; that is, some extraction methods can increase the yield, but It is also not conducive to scale-up and industrial production because of high operating requirements, complicated control, and immature technology;
[0008] (3) Due to the long production cycle and low extraction efficiency of homoharringtonine, it is difficult to promote application and large-scale production, and it is difficult to obtain ideal curative effect for synthetic products;
[0009] (4) Due to the use of different fillers, problems such as low yield, poor impurity removal effect, and product degradation during column chromatography cannot be well applied to large-scale production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Embodiment 1: The method for extracting homoharringtonine from crude Torreya is as follows:

[0029] (1) Use 300kg, 10-20 mesh dry crude torreya as raw material, add industrial-grade methanol-chloroform mixture to the raw material at a ratio of mass volume ratio g:mL of 1:3 (the volume ratio of methanol and chloroform is 1: 2) Extract at room temperature for 6 hours, filter, continue to add methanol-chloroform mixture to the filter residue, repeat the extraction once, combine the filtrate, and concentrate until no recovered liquid flows out to obtain an extract containing homoharringtonine;

[0030] (2) In the homoharringtonine-containing extract, add chloroform at a mass volume ratio of g:mL of 1:3, heat to 55°C to dissolve completely, let it settle for 12 hours at room temperature, and pump under reduced pressure Filtration, and the filtrate was concentrated and drained at 65°C to obtain the crude product of homoharringtonine;

[0031] (3) Add acetonitrile to the cru...

Embodiment 2

[0034] Embodiment 2: The method for extracting homoharringtonine from crude Torreya is as follows:

[0035] (1) Use 300kg, 10-20 mesh dried crude torreya as raw material, add industrial-grade methanol-chloroform mixture to the raw material at a ratio of mass volume ratio g:mL of 1:4 (the volume ratio of methanol and chloroform is 1: 3), extract at room temperature for 7 hours, filter, continue to add methanol-chloroform mixture to the filter residue, repeat the extraction twice, combine the filtrate, concentrate until no recovered liquid flows out, and obtain an extract containing homoharringtonine;

[0036](2) In the homoharringtonine-containing extract, add chloroform at a ratio of mass volume ratio g:mL of 1:3.5, heat to 60°C to dissolve completely, let it settle at room temperature for 10 hours, pump under reduced pressure filtered, and the filtrate was concentrated and drained at 70°C to obtain the crude product of homoharringtonine;

[0037] (3) Add acetonitrile to the ...

Embodiment 3

[0040] Embodiment 3: The method for extracting homoharringtonine from crude Torreya is as follows:

[0041] (1) Use 300kg, 10-20 mesh dry crude torreya as raw material, add industrial-grade methanol-chloroform mixture to the raw material at a ratio of mass volume ratio g:mL of 1:5 (the volume ratio of methanol and chloroform is 1: 2.5), extract at room temperature for 8 hours, filter, continue to add methanol-chloroform mixture to the filter residue, repeat the extraction once, combine the filtrate, and concentrate until no recovered liquid flows out to obtain an extract containing homoharringtonine;

[0042] (2) In the homoharringtonine-containing extract, add chloroform at a mass volume ratio of g:mL of 1:4, heat to 65°C to dissolve completely, let it settle for 8 hours at room temperature, and pump under reduced pressure filtered, and the filtrate was concentrated and drained at 68°C to obtain the crude product of homoharringtonine;

[0043] (3) Add acetonitrile to the cru...

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Abstract

The invention discloses a method for extracting homoharringtonine. The method includes the steps that a dried and pulverized cephalotaxus sinensis raw material is extracted with methanol-chloroform mixed liquor, filtration is performed, filter liquor is concentrated to obtain extract, chloroform precipitation is performed, filtration is performed, filter liquor is concentrated at 65-70 DEG C to obtain crude homoharringtonine, and the crude homoharringtonine is subjected to reversed-phase column chromatography, concentration, extraction, recrystallization, separation and purification to obtainfinished homoharringtonine, wherein the homoharringtonine content is larger than 98%. The method is simple and easy to operate, short in production cycle, low in cost, high in yield, and suitable forindustrial application and market promotion.

Description

technical field [0001] The invention relates to an industrialized production method for extracting homoharringtonine from dried rough bark of Torreya bark. Background technique [0002] Homoharringtonine (Homoharringtonine) is an alkaloid obtained from the three-pointed plant Three-pointed Sequoia or its genus; it has inhibitory effect on the incorporation of 3H-labeled asparagine into proteins, and it has an inhibitory effect on the incorporation of 3H-labeled thymidine into Incorporation of DNA also affects; homoharringtonine can also induce cell differentiation, increase the content of cAMP, and inhibit glycoprotein synthesis; under the electron microscope, it can be seen that chromatin concentrates and condenses toward the edge of the nucleus, forming chromosome clumps that bulge outward , develop into "litter bodies" with nuclear separation, and finally nuclear fragmentation. [0003] Homoharringtonine has inhibitory effect on animal metastatic leukemia P-388 and L-121...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D491/20
Inventor 马回民杨青春赵泽熙
Owner YUNNAN HANDE BIO TECH
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