CN100374399C - Process of obtaining element - Google Patents
Process of obtaining element Download PDFInfo
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- CN100374399C CN100374399C CNB2006100525753A CN200610052575A CN100374399C CN 100374399 C CN100374399 C CN 100374399C CN B2006100525753 A CNB2006100525753 A CN B2006100525753A CN 200610052575 A CN200610052575 A CN 200610052575A CN 100374399 C CN100374399 C CN 100374399C
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- elemenum
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- elemene
- obtains
- crude product
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The process of preparing elemene includes the following steps: 1) collecting goldenrod; 2) crushing goldenrod into 0.6-1 mm size material; and 3) extracting the material through a steam distillation process, an organic solvent extraction process, an ultrasonic process or an supercritical extraction process to obtain coarse elemene product with high elemene content.
Description
Technical field
The present invention relates to a kind of method that obtains Elemenum, particularly from Herba Solidaginis, obtain the method for Elemenum.
Background technology
Malignant tumour is a kind of common disease and frequently-occurring disease, serious harm people ' s health and life.According to World Health Organization's statistics, the whole world has 1,000 ten thousand people's cancer strickens approximately, and about 7,000,000 people die from cancer; Cancer has become human second largest killer.The medicine of treatment tumour can be divided into chemical synthetic drug and natural drug by its source.Plant amedica, particularly herbal medicine provide abundant treasure-house for the research and development of PTS.In recent years, the medicine of plant-sourced especially comes into one's own, and not only because it is the important source of finding new drug, and can be the better new drug of design new unique chemical structure is provided. and the latter can be used as the lead compound of initiative new drug.Elemenum (Elemene) is a kind of anticarcinogen of new texture type of non-cytotoxicity.Present anticancer preparation is a main component with β one Elemenum, contains a small amount of δ-Elemenum and γ-Elemenum and other terpenoid simultaneously.β one Elemenum, δ-Elemenum and γ-Elemenum are anti-cancer active matter, do not have significant difference, so be referred to as Elemenum.At present, elemene emulsion is used clinically as national two kind new medicines, is the rare new drug with independent intellectual property right of China.
Existing Elemenum mainly is from zingiberaceous plant RADIX CURCUMAE (warm curcuma zedoary, Curcumazedoaria (Berg.) Rose), extract in the zddoary (Curcuma phaeocaul, Val.), Guangxi zedoary (C.kwangsinensis S.G.Lee et C., F.Lian) rhizome, extraction approach in addition is to extract from lemongrass, myrrh, the bighead atractylodes rhizome.Therefore but above-mentioned several plant is all little in the output of China, can't scale operation; And Elemenum output is also little in the corresponding vegetables oil of extraction gained, generally has only 5～10%, and the difficulty of subsequent development Elemenum is strengthened.Therefore urgent hope exploitation can obtain the production method of high-content Elemenum.
Former studies is thought, Herba Solidaginis (Solidago decurrens) has wind and heat dispersing, antisepsis and anti-inflammation, be used for flu, acute pharyngolaryngitis, tonsillitis, sore furuncle poison, liver cancer, cervical cancer, leukemia etc., the anti-tumor function composition mainly is kaempferol, glycoside, the phytomelin of flavonoid.But still from Herba Solidaginis, do not extract the report of anticancer active constituent Elemenum.
Summary of the invention
At the deficiencies in the prior art part, the invention provides a kind of method that from Herba Solidaginis (Solidagodecurrens), obtains Elemenum, utilize this kind extracting method can obtain high-load Elemenum.
The present invention is to realize by such technical scheme for reaching above purpose: a kind of method that obtains Elemenum from Herba Solidaginis (Solidago decurrens) is provided, may further comprise the steps:
1), gathers Herba Solidaginis; 2) it is ground into the primary product of 0.6～1mm; 3), adopt steam distillation, organic solvent extraction method, supersonic method or super critical extraction to extract the above-mentioned raw materials product, the Elemenum crude product.
Improvement as the method for acquisition Elemenum of the present invention: step 1) is gathered at least a in root, stem, leaf, flower and the seed of Herba Solidaginis.Can select the above-mentioned position in the Herba Solidaginis separately for use, also can select the mixture at these positions for use.Can select these fresh positions for use, directly carry out pulverising step; Also can carry out pulverising step again with after these position drying treatment.Step 2) but the using-system stamp mill, organize pulverizer or artificial chopping or the like these known ordinary methods to pulverize.
Adopt the Elemenum crude product of method gained of the present invention, for containing the water-fast oily or the paste mixture of 10～35% Elemenums.Can adopt currently known methodss such as column chromatography, continue the above-mentioned Elemenum crude product of separation and purification, can get the pure product of Elemenum.
Adopt the Elemenum crude product of the inventive method gained, be called Herba Solidaginis (Solidagodecurrens) oil again, through gas chromatograph-mass spectrometer check and analysis composition and content thereof, learn: ((total Elemenum of β-Elemene) form accounts for 10～35% of Elemenum crude product gross weight, is higher than the content of total Elemenum in the existing vegetables oil far away for δ-Elemene) and beta-elemene by δ-Elemenum; And the weight ratio of δ-Elemenum and beta-elemene is 1～4: 1, is different from the proportion of composing (it is a main component with β one Elemenum) of total Elemenum in the existing vegetables oil.
Because as its growth region difference of Herba Solidaginis, season of growth difference and the not equal factor of extracting method of raw material, therefore the content of δ-Elemenum and beta-elemene exists certain fluctuation in the Elemenum crude product that obtains.
Embodiment
Embodiment 1, a kind of method that obtains Elemenum, carry out following steps successively:
1), gathers fresh leaf 3000 grams of Herba Solidaginis (Solidago decurrens);
2), the using-system stamp mill is ground into the primary product of 1mm;
3), adopt steam distillation to extract 10 hours extraction times the above-mentioned raw materials product.With oily water separation; Promptly obtain Elemenum crude product 12.6 grams, be oily matter.
The Elemenum crude product of gained, through gas chromatograph-mass spectrometer check and analysis composition and content thereof, learn: total Elemenum content is 30%, and the weight ratio of δ-Elemenum and beta-elemene is 3: 1.
Get above-mentioned 10 gram Elemenum crude products and carry out purifies and separates, can adopt conventional silica gel column chromatography, the sherwood oil wash-out is collected elutriant, desolvates; Get pure product 2.4 grams of Elemenum, purity 96.2%.
Embodiment 2, a kind of method that obtains Elemenum, carry out following steps successively:
1), gathers fresh leaf 3000 grams of Herba Solidaginis (Solidago decurrens);
2), manually be chopped into the primary product of 1mm;
3), the ultrasonoscope that adopts frequency 15KHz, power 200W adds above-mentioned raw materials product and carries out supersound extraction in the entry in 1: 10 ratio, extraction time is 60 minutes, must feed liquid; Above-mentioned feed liquid is filtered, centrifugal, oily water separation; Promptly obtain Elemenum crude product 12 grams, be oily matter.
The Elemenum crude product of gained, through gas chromatograph-mass spectrometer check and analysis composition and content thereof, learn: total Elemenum content is 35%, and the weight ratio of δ-Elemenum and beta-elemene is 2.5: 1.
Get above-mentioned 10 gram Elemenum crude products and carry out purifies and separates, adopt conventional silica gel column chromatography, the sherwood oil wash-out is collected elutriant, desolvates; Get pure product 2.95 grams of Elemenum, purity 96.5%.
Embodiment 3: a kind of method that obtains Elemenum, carry out following steps successively:
1), gather Herba Solidaginis (Solidago decurrens) root, after drying dry rhizome 3000 grams;
2), the using-system pulverizer is crushed to dry root the primary product of 0.8mm;
3), the above-mentioned raw materials product are extracted in employing organic solvent extraction method in 1: 10 the ratio adding sherwood oil; Extraction time 24 hours, normal temperature lixiviate 3 times is filtered, and is centrifugal, and concentrating under reduced pressure gets paste, adds dehydrated alcohol purification, drying.Promptly obtain Elemenum crude product 30 grams, be oily matter.
The Elemenum crude product of gained, through gas chromatograph-mass spectrometer check and analysis composition and content thereof, learn: total Elemenum content is 10%, and the weight ratio of δ-Elemenum and beta-elemene is 1: 1.
Get above-mentioned 20 gram Elemenum crude products and carry out purifies and separates, adopt conventional silica gel column chromatography, the sherwood oil wash-out is collected elutriant, desolvates; Get pure product 4.2 grams of Elemenum, purity 97.3%.
Embodiment 4: a kind of method that obtains Elemenum, carry out following steps successively:
1), gather the new fresh flower of Herba Solidaginis (Solidago decurrens), after drying in the shade dried floral 3000 grams;
2), the using-system pulverizer is broken to dry pollen the primary product of 1mm;
3), the above-mentioned raw materials product are extracted as the organic solvent extraction method of embodiment 3 in adopting in 1: 10 the ratio adding normal hexane; Promptly obtain Elemenum crude product 45 grams, be oily matter.
The Elemenum crude product of gained, through gas chromatograph-mass spectrometer check and analysis composition and content thereof, learn: total Elemenum content is 22%, and the ratio of δ-Elemenum and beta-elemene is 4: 1.
Get above-mentioned 20 gram Elemenum crude products and carry out purifies and separates, adopt conventional silica gel column chromatography, the sherwood oil wash-out is collected elutriant, desolvates; Get pure product 3.7 grams of Elemenum, purity 97.4%.
Embodiment 5: a kind of method that obtains Elemenum, carry out following steps successively:
1), gather the fresh complete stool of Herba Solidaginis (Solidago decurrens), after drying dry complete stool 1000 grams;
2), the using-system pulverizer is crushed to dry complete stool the primary product of 0.6mm;
3), the above-mentioned raw materials product are adopted supercritical CO
2Extraction method is extracted, and is specific as follows: the above-mentioned raw materials product are added in the supercritical CO 2 abstraction pool. pressure 15MPa, 50 ℃ of abstraction pool temperature, 30 ℃ of reception tank temperature, dynamic extraction 50min.Promptly obtain Elemenum crude product 16 grams, be oily matter.
The Elemenum crude product of gained, through gas chromatograph-mass spectrometer check and analysis composition and content thereof, learn: total Elemenum content is 15%, and the ratio of δ-Elemenum and beta-elemene is 1: 1.
Get above-mentioned 10 gram Elemenum crude products and carry out purifies and separates, adopt conventional silica gel column chromatography, the sherwood oil wash-out is collected elutriant, desolvates; Get pure product 1.7 grams of Elemenum, purity 96.4%.
At last, it is also to be noted that what more than enumerate only is several specific embodiments of the present invention.Obviously, the invention is not restricted to above embodiment, many distortion can also be arranged.All distortion that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.
Claims (3)
1. a method that obtains Elemenum is characterized in that, may further comprise the steps:
1), gathers Herba Solidaginis;
2), it is ground into the primary product of 0.6～1mm;
3), adopt steam distillation, organic solvent extraction method, supersonic method or super critical extraction to extract the above-mentioned raw materials product, the Elemenum crude product.
2. a kind of method that obtains Elemenum according to claim 1 is characterized in that described step 1): gather at least a in root, stem, leaf, flower and the seed of Herba Solidaginis.
3. a kind of method that obtains Elemenum according to claim 1 and 2 is characterized in that: the Elemenum crude product is carried out separation and purification, get the pure product of Elemenum.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100525753A CN100374399C (en) | 2006-07-21 | 2006-07-21 | Process of obtaining element |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006100525753A CN100374399C (en) | 2006-07-21 | 2006-07-21 | Process of obtaining element |
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| Publication Number | Publication Date |
|---|---|
| CN1887831A CN1887831A (en) | 2007-01-03 |
| CN100374399C true CN100374399C (en) | 2008-03-12 |
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| CNB2006100525753A Expired - Fee Related CN100374399C (en) | 2006-07-21 | 2006-07-21 | Process of obtaining element |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101492339B (en) * | 2009-03-06 | 2011-10-05 | 北京联合大学应用文理学院 | Process and apparatus for the extraction separation of beta-elemene, and process for producing stuffing |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1651366A (en) * | 2004-11-30 | 2005-08-10 | 河北科技大学 | Method of extracting elemene in curcuma zedoary by super critical carbon dioxide fluid extraction-rectification |
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- 2006-07-21 CN CNB2006100525753A patent/CN100374399C/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1651366A (en) * | 2004-11-30 | 2005-08-10 | 河北科技大学 | Method of extracting elemene in curcuma zedoary by super critical carbon dioxide fluid extraction-rectification |
Non-Patent Citations (1)
| Title |
|---|
| 加拿大一枝黄花的精油成分. 夏文孝；植物学通报，第（16）卷第2期. 1999 * |
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| CN1887831A (en) | 2007-01-03 |
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