CN101502610B - Method for extracting veratrum alkaloid from Veratrum nigrum by supercritical carbon dioxide - Google Patents
Method for extracting veratrum alkaloid from Veratrum nigrum by supercritical carbon dioxide Download PDFInfo
- Publication number
- CN101502610B CN101502610B CN2009100738857A CN200910073885A CN101502610B CN 101502610 B CN101502610 B CN 101502610B CN 2009100738857 A CN2009100738857 A CN 2009100738857A CN 200910073885 A CN200910073885 A CN 200910073885A CN 101502610 B CN101502610 B CN 101502610B
- Authority
- CN
- China
- Prior art keywords
- veratrum
- veratri
- radix
- rhizoma
- alkaloid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Landscapes
- Extraction Or Liquid Replacement (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention provides a method for extracting veratrum alkaloid from veratrum by supercritical carbon dioxide, which comprises the following steps of: A. crushing the veratrum, adding 150mL of ammonia into 100g of veratrum powder and soaking for 3 hours, drying at a shade and ventilating place and then sieving with 30 meshes; B. adding the crushed product of the veratrum after alkalized into a supercritical fluid extracting tank, opening a CO2 steel cylinder, starting to extract by taking ethanol as a carrying agent at the temperature of an extractor of 65 to 75 DEG C, at the extracting pressure of 30 to 38 MPa, at the flow rate of CO2 of 40 to 45Kg/h and with the extracting time of 2 to 4 hours, and implementing distillation by a separator and recovering a solvent so as to obtain crude products of veratrum alkaloid. The invention adopts early-phase alkaline treatment, extracts veratrum alkaloid from veratrum by supercritical carbon dioxide, can separate the combined alkaloid and acid which are hard to separate from each other in veratrum by utilizing high pressure and high seepage pressure of CO2, and dissolves out effective ingredients, the yield of the veratrum alkaloid is higher than that of veratrum alkaloid extracted by soaking of organic solvent; in addition, the invention has simple process, stable operation and recycled solvent and has a certain economic benefit and environmental benefit.
Description
Technical field
The present invention relates to a kind of method that from Rhizoma et radix veratri (Radix Rhizoma Veratri), extracts veratrum alkaloid, belong to the extracting method technical field of active ingredient of natural plant.
Background technology
Veratrum alkaloid is naturally occurring a kind of important biomolecule active substance in the Rhizoma et radix veratri (Radix Rhizoma Veratri), possesses numerous important physical functions and great development and application values.It has various insects tags and stomach poison function, can develop biological pesticide; Low dose of veratrum alkaloid all has therapeutical effect to hypertension, apoplexy, epilepsy, fracture, can develop healthcare products, medicine, is one of native compound that receives much attention at present.At present, produce the method for veratrum alkaloid, adopt traditional organic solvent to soak extraction both at home and abroad, from Rhizoma et radix veratri (Radix Rhizoma Veratri), extract the veratrum alkaloid crude extract.The patent of invention of the patent No. 200610170802 discloses in a kind of Rhizoma et radix veratri (Radix Rhizoma Veratri) the technology of extracting veratrum alkaloid, continues to use said method, and this method extraction time is long, the organic solvent consumption is big.
Summary of the invention
The object of the present invention is to provide a kind of supercritical CO
2The method of extraction veratrum alkaloid from Rhizoma et radix veratri (Radix Rhizoma Veratri), because the alkaloids substance in the Rhizoma et radix veratri (Radix Rhizoma Veratri) mainly contains materials such as veratridine, cevadine, polarity is strong, single CO with low pole
2Be difficult to extract, the present invention selects to adopt alkalization back supercritical CO in early stage
2From extraction process.
Technical scheme of the present invention is achieved in that this supercritical carbon dioxide extracts the method for veratrum alkaloid from Rhizoma et radix veratri (Radix Rhizoma Veratri), is characterized in that adopting following steps to finish:
A, earlier Rhizoma et radix veratri (Radix Rhizoma Veratri) is pulverized, the ratio that adds 150mL ammonia according to 100g Rhizoma et radix veratri (Radix Rhizoma Veratri) powder was soaked 3 hours, dried the back in the shady and cool ventilation place and crossed 30 mesh sieves;
B, the Rhizoma et radix veratri (Radix Rhizoma Veratri) after will alkalizing are pulverized in the product adding supercritical fluid extraction jar, open the CO2 steel cylinder, begin extraction with ethanol for carrying agent, the extractor temperature is 65～75 ℃, extracting pressure is 30～38MPa, the CO2 flow is 40～45Kg/h, and the extraction time is 2～4h, revolves steaming recovery solvent through separator and gets the veratrum alkaloid crude product.
Described supercritical carbon dioxide extracts the method for veratrum alkaloid from Rhizoma et radix veratri (Radix Rhizoma Veratri), the described CO of step B
2Behind the gas process depurator I, enter condenser liquefaction, enter depurator II again by the plunger displacement pump pressurization then and further liquefy, enter the extractor bottom, be dissolved with the CO of solute by pipeline
2Fluid comes out to enter separator by the extractor top, forms to reflux, and sets extractor pressure 35MPa, 65 ℃ of temperature, static extracting 0.5 hour; Then, start the entrainer pump and inject 95% ethanol simultaneously, dynamic extraction 2～3 hours, carrying agent flux is 0.1L/h.
Described supercritical carbon dioxide extracts the method for veratrum alkaloid from Rhizoma et radix veratri (Radix Rhizoma Veratri), the pressure of setting primary separator I is 8MPa, and temperature is 40 ℃; The pressure of second-stage separator II is 6MPa, and temperature is 40 ℃, obtains the veratrum alkaloid crude product from two separators.
Described supercritical carbon dioxide extracts the method for veratrum alkaloid from Rhizoma et radix veratri (Radix Rhizoma Veratri), step B is described, and to carry agent be 95% ethanol or dehydrated alcohol.
Technological progress effect of the present invention shows: adopt the basification in early stage, supercritical carbon dioxide extracts veratrum alkaloid from Rhizoma et radix veratri (Radix Rhizoma Veratri), utilize CO
2High pressure, hyperosmosis power, can make that difficult isolating combined state alkaloid separates with acid in the Rhizoma et radix veratri (Radix Rhizoma Veratri), the stripping effective ingredient, the yield of veratrum alkaloid is higher than organic solvent and soaks the veratrum alkaloid yield of extracting, and flow process is simple, stable operation, solvent can be recycled, and possesses certain economic benefits and environmental benefit.
Description of drawings
Fig. 1 is a supercritical CO of the present invention
2Fluid extraction part flow chart
The specific embodiment
Embodiment 1, supercritical carbon dioxide of the present invention extract the method for veratrum alkaloid from Rhizoma et radix veratri (Radix Rhizoma Veratri)
A, Rhizoma et radix veratri (Radix Rhizoma Veratri) is pulverized, the ratio that adds 150ml ammonia according to every 100g Rhizoma et radix veratri (Radix Rhizoma Veratri) is soaked 3h, dries the back in the shady and cool ventilation place and crosses 30 mesh sieves;
In B, the adding supercritical fluid extraction jar, open CO
2Steel cylinder behind the gas process depurator I, enters condenser liquefaction, enters depurator II again with the plunger displacement pump pressurization then and further liquefies, and enters the extractor bottom by pipeline, sets extractor pressure 35MPa, 65 ℃ of temperature, and static extracting 0.5 hour utilizes CO
2High pressure, high penetration, make in the Rhizoma et radix veratri (Radix Rhizoma Veratri) alkaloid separate the stripping effective ingredient; Then, start the entrainer pump and inject 95% ethanol simultaneously, dynamic extraction 2～3 hours, entrainer flow are 0.1L/h, and the pressure of setting primary separator I is 8MPa, and temperature is 40 ℃, and the pressure of second-stage separator II is 40 ℃ of 6MPa, temperature.From two separators, obtain product.
The thick alkali yield 2.03%～3.14% of separator I, wherein alkaloid is 6.87%～9.36%;
The thick alkali yield 1.21%～1.67% of separator II, wherein alkaloid is 19.30%～21.42%.The total thick alkali yield of present embodiment can reach 3.53%～4.02%, and alkaloid can reach 14.38%～15.13%, and alkaloidal main physical and chemical is: faint yellow amorphous powder, through 130 ℃ dry after product, 175 ℃～186 ℃ of its fusing points.Usually water insoluble, be slightly soluble in ether, be dissolved in ethanol.
Embodiment 2, Rhizoma et radix veratri (Radix Rhizoma Veratri) are without the direct supercritical carbon dioxide extraction of basification
A, Rhizoma et radix veratri (Radix Rhizoma Veratri) is pulverized, cross 30 mesh sieves;
B, with the extracting process of embodiment 1.
The thick alkali yield of Rhizoma et radix veratri (Radix Rhizoma Veratri) is 1.91%～2.42%, and wherein alkaloid is 1.18%～2.34%.
Embodiment 3, Rhizoma et radix veratri (Radix Rhizoma Veratri) carry out supercritical carbon dioxide extraction again through Ethanol Treatment
A, take by weighing Rhizoma et radix veratri (Radix Rhizoma Veratri) and pulverize product 100g, 3 times (the shared 3000ml ethanol) of 35 ℃ of isothermal vibrations extractions of 95% ethanol with 1000ml extracted 24 hours at every turn;
B, with the extracting process of embodiment 1.
The thick alkali yield of Rhizoma et radix veratri (Radix Rhizoma Veratri) is 8.53%～10.53%, and wherein alkaloid is 4.53%～5.27%.
The veratrum alkaloid yield explanation the present invention who measures by comparative examples 1,2,3 adopts alkalization back supercritical CO in early stage
2The method of extraction veratrum alkaloid is higher than the organic solvent extraction method, and has significantly reduced the use amount of organic solvent from Rhizoma et radix veratri (Radix Rhizoma Veratri), has shortened the time.
Supercritical CO of the present invention
2Extraction equipment is selected from Huaan, Nantong supercritical extraction company limited; Rhizoma et radix veratri (Radix Rhizoma Veratri) belongs to a mao fringe Rhizoma et radix veratri (Radix Rhizoma Veratri).
Listed examples of the present invention is intended to further set forth supercritical carbon dioxide and extracts the process of veratrum alkaloid from Rhizoma et radix veratri (Radix Rhizoma Veratri), and scope of the present invention is not constituted any restriction.
Claims (2)
1. supercritical carbon dioxide extracts the method for veratrum alkaloid from Rhizoma et radix veratri (Radix Rhizoma Veratri), it is characterized in that adopting following steps to finish:
A, earlier Rhizoma et radix veratri (Radix Rhizoma Veratri) is pulverized, the ratio that adds 150ml ammonia according to 100g Rhizoma et radix veratri (Radix Rhizoma Veratri) powder was soaked 3 hours, dried the back in the shady and cool ventilation place and crossed 30 mesh sieves;
In B, the adding supercritical fluid extraction jar, open CO
2Steel cylinder behind the gas process depurator I, advances the liquefaction of people's condenser, enters depurator II again with the plunger displacement pump pressurization then and further liquefies, and enters people's extractor bottom by pipeline, sets extractor pressure 35MPa, 65 ℃ of temperature, and static extracting 0.5 hour utilizes CO
2High pressure, high penetration, make in the Rhizoma et radix veratri (Radix Rhizoma Veratri) alkaloid separate the stripping effective ingredient; Then, start the entrainer pump and inject 95% ethanol simultaneously, dynamic extraction 2～3 hours, entrainer flow are 0.1l/h, and the pressure of setting primary separator I is 8MPa, and temperature is 40 ℃, and the pressure of second-stage separator II is 40 ℃ of 6MPa, temperature; From two separators, obtain product.
2. supercritical carbon dioxide according to claim 1 extracts the method for veratrum alkaloid from Rhizoma et radix veratri (Radix Rhizoma Veratri), it is characterized in that: the pressure of setting primary separator (I) is 8MPa, and temperature is 40 ℃; The pressure of second-stage separator (II) is 6MPa, and temperature is 40 ℃, obtains the veratrum alkaloid crude product from two separators.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100738857A CN101502610B (en) | 2009-03-09 | 2009-03-09 | Method for extracting veratrum alkaloid from Veratrum nigrum by supercritical carbon dioxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009100738857A CN101502610B (en) | 2009-03-09 | 2009-03-09 | Method for extracting veratrum alkaloid from Veratrum nigrum by supercritical carbon dioxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101502610A CN101502610A (en) | 2009-08-12 |
| CN101502610B true CN101502610B (en) | 2011-07-20 |
Family
ID=40975073
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009100738857A Expired - Fee Related CN101502610B (en) | 2009-03-09 | 2009-03-09 | Method for extracting veratrum alkaloid from Veratrum nigrum by supercritical carbon dioxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101502610B (en) |
Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105076260A (en) * | 2015-07-20 | 2015-11-25 | 黑龙江东北亚林产品有限公司 | Special plant source insecticide for rice and preparation method for special plant source insecticide for rice |
| CN106036902B (en) * | 2016-06-07 | 2019-03-22 | 河南科技大学 | A kind of preparation method of quinoa leaf flavonoids health care buccal tablets |
| WO2019054671A1 (en) * | 2017-09-12 | 2019-03-21 | 주식회사 엘지화학 | Separation method and separation apparatus for solvent |
| KR102201310B1 (en) * | 2017-09-12 | 2021-01-11 | 주식회사 엘지화학 | Method and apparatus for separating solvent |
| CN110152350B (en) * | 2019-06-28 | 2021-05-14 | 山东大学 | Subcritical fluid continuous isobaric extraction separation device system and extraction separation process |
| CN110624273A (en) * | 2019-10-25 | 2019-12-31 | 北京和荣工程技术有限公司 | Supercritical CO improving agent2Method and system for extracting oil sludge extraction rate |
-
2009
- 2009-03-09 CN CN2009100738857A patent/CN101502610B/en not_active Expired - Fee Related
Non-Patent Citations (3)
| Title |
|---|
| 张涛，蔡建国.生物碱的超临界流体萃取研究进展.《世界科学技术－中医药现代化》.2003,第5卷(第3期),第41-43页. * |
| 李青山.超临界CO2流体萃取工艺的影响因素.《药物化学前沿导论》.科学出版社,2005,第366页. * |
| 谢霞等.藜芦生物碱萃取方法的研究.《齐齐哈尔大学学报》.2008,第24卷(第6期),第76-77页. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101502610A (en) | 2009-08-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN101502610B (en) | Method for extracting veratrum alkaloid from Veratrum nigrum by supercritical carbon dioxide | |
| CN102161932B (en) | Method for extracting soybean germ oil by using subcritical butane | |
| CN103386215B (en) | The method of supercritical continuous carbon dioxide extraction Taiwan Cortex seu Flos Hibisci taiwanenss active ingredient | |
| CN106993789B (en) | Method for extracting high-quality propolis by using subcritical multi-component mixed solvent | |
| CN101810658B (en) | Method for removing residual pesticide from ginseng | |
| CN102586004B (en) | Method for continuously extracting orange oil and limonin from citrus reticulata | |
| CN103393787B (en) | The method of supercritical continuous carbon dioxide extraction oriental cherry effective ingredient | |
| CN104073343A (en) | Supercritical CO2 aquilaria agallocha roxb seed oil extraction method | |
| CN101880597A (en) | Method for extracting rice bran oil by using ionic liquid and supercritical carbon dioxide (CO2) | |
| CN104140885B (en) | Oil plant seed is that raw material prepares the method with oxidation resistance long chain fat acid esters | |
| CN111097188A (en) | Pulse pressure cold extraction method of natural product | |
| CN103393741B (en) | The method of ultrasonic assistant supercritical continuous carbon dioxide extraction windmill blade of grass effective ingredient | |
| CN100451030C (en) | Process of preparing ganoderma tricterpinyl acid and ganoderma polyose from ganoderma | |
| TW200507867A (en) | Extract of plant dendrobii caulis and preparing process thereof | |
| CN102432619A (en) | Preparation method of sesamin | |
| CN104073355A (en) | Extraction method of pogostemon cablin essential oil | |
| CN103524520B (en) | A kind of method extracting parithenolide from plant material | |
| CN100360516C (en) | Method for extracting apple polyphenol from apple pomace by supercritical CO2 | |
| CN103450299A (en) | Method for simultaneously preparing esculoside and esculetin | |
| CN103897800A (en) | Process for extracting wheat germ oil by adopting supercritical extraction method | |
| CN101428052A (en) | Method for extracting radix gynurae segeti alkaloid with supercritical carbonic anhydride | |
| CN102070591A (en) | Process method for efficiently extracting apigenin from Chinese violet | |
| CN104230806B (en) | A kind of method that aconitine is extracted from plant | |
| CN101210018A (en) | Method for preparing deguelin | |
| CN102827129A (en) | Method for extracting and purifying gericudranin A |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20110720 Termination date: 20120309 |