CN102499953A - Process for extracting total phenyl propanoid from paulownia bark of paulownia tomentosa (original variety) by adopting supercritical CO2 fluid technology - Google Patents
Process for extracting total phenyl propanoid from paulownia bark of paulownia tomentosa (original variety) by adopting supercritical CO2 fluid technology Download PDFInfo
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- CN102499953A CN102499953A CN2011103738644A CN201110373864A CN102499953A CN 102499953 A CN102499953 A CN 102499953A CN 2011103738644 A CN2011103738644 A CN 2011103738644A CN 201110373864 A CN201110373864 A CN 201110373864A CN 102499953 A CN102499953 A CN 102499953A
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Abstract
The invention belongs to the technical field of the extraction of plant secondary metabolic active components, in particular to a process for extracting total phenyl propanoid from paulownia bark of paulownia tomentosa (original variety) by adopting a supercritical CO2 fluid technology. According to the invention, the paulownia bark of the paulownia tomentosa (original variety), which is washed clean, dried in the shade and crushed to have granularity of 20 to 80 meshes, is put into an extraction kettle, CO2 fluid in a supercritical state is taken as an extraction agent, and ethanol water solution with the concentration of 40 percent to 95 percent is used as an entrainer, so as to extract the total phenyl propanoid; the total phenyl propanoid is extracted under an extraction environment that the temperature is 30 to 60 DEG C and the pressure is 20 to 60Mpa for 1 to 5 hours; then the total phenyl propanoid is decompressed, resolved and separated in a separation kettle, the ethanol water solution containing the total phenyl propanoid is collected, and an extract of the total phenyl propanoid of the paulownia bark of the paulownia tomentosa (original variety) is obtained after the ethanol water solution is decompressed, concentrated, cooled and dried. The process has the advantages of simple operation process, short period, low cost, high extraction rate, no residual solvent, and the like, can be used in mass production, and is applied to the field of medicine, cosmetics, functional food, and the like.
Description
Technical field
The invention belongs to Secondary Metabolism of Plant active component extractive technique field, be specifically related to a kind of employing supercritical CO
2The technology of fluid technique extraction royal paulownia (former mutation) Cortex paulowniae total phenylpropanoid.
Background technology
Royal paulownia (former mutation) (Paulownia tomentosa Steud.var.tomentosa) is Scrophulariaceae (Scrophulariaceae) Paulownia (the Paulownia Sieb.et Zucc) broad-leaved arbor (chief editor of Chinese Plants will editorial board of the Chinese Academy of Sciences " Chinese Plants will "; The 2nd of the 67th volume; 33～35 pages; Science Press; Beijing; 1979); In the folk tradition medicine its Cortex paulowniae, Lignum paulowniae, Folium paulowniae, Flos paulowniae by extensively in order to relieving asthma, cough-relieving, eliminate the phlegm, hair growth promoting etc., (Si C.L. waits .Studies on the phenylpropanoid glycosides with anti-complement activity from Paulownia tomentosa var.tomentosa wood.Journal of Asian Natural Product Research in clinical, to be used for treating under bronchopneumonia, acute conjunctivitis, acute tonsillitis, upper respiratory tract infection, the pancreas multiple diseases such as adenitis, bacillary dysentery, acute enteritis in recent years in a large number; 2008,10 (11): 1003～1008).Therefore, royal paulownia (former mutation) is the huge valuable resources of medicinal plant of a kind of potentiality to be exploited.
Plain (Phenyl propanoid) chemical compound of phenylpropyl alcohol has effects such as antitumor, antiviral, antioxidation, pain relieving, antibiotic, antiinflammatory, hepatoprotective and base reparation, and, diabetes low to memory ability and relevant disease etc. all tool improve significantly.In recent years; Along with going deep into of domestic and international research; Increasing data shows that the plain chemical compound of phenylpropyl alcohol has the effect of control neurodegenerative diseases, especially improve aspect senile dementia, the parkinson disease effect obviously (Liu Jie is etc. the progress of the plain glycosides compound control of phenylpropyl alcohol neurodegenerative diseases. drug evaluation research; 2009,32 (1): 62～66).
The research document shows and contains plain composition (the Si C.L. of a large amount of phenylpropyl alcohol in royal paulownia (former mutation) Cortex paulowniae; Deng .Phenolic extractives with chemotaxonomic significance from the bark of paulownia tomentosa var.tomentosa.Bioresources; 2011; 6 (4): 5086～5098); Yet these researchs mainly are the methods that adopts conventional solvent extraction, have that extracting cycle is long, cost is high, yield is low, organic solvent residual, be unfavorable for shortcoming such as large-scale industrial production.Up to the present, to the supercritical CO of royal paulownia (former mutation) Cortex paulowniae total phenylpropanoid
2The fluid extraction technical study still belongs to blank.
Summary of the invention
The object of the present invention is to provide that a kind of operating procedure is simple, the cycle is short, cost is low, extraction yield is high, no solvent residue, be fit to the supercritical CO of large-scale production
2The technology of fluid technique extraction royal paulownia (former mutation) Cortex paulowniae total phenylpropanoid.
To achieve these goals, the technical scheme of the present invention's employing is:
The supercritical CO of royal paulownia (former mutation) the Cortex paulowniae total phenylpropanoid that the present invention proposes
2The fluid technique extraction process comprises following three steps in order:
A. royal paulownia (former mutation) Cortex paulowniae is cleaned, dried in the shade, being crushed to granularity then is 20～80 orders;
B. the royal paulownia after the pulverization process (former mutation) Cortex paulowniae is put into extraction kettle, with the CO of supercriticality
2Fluid is an extractant, and the ethanol water with 40%～95% is that entrainer extracts, the extraction environment be temperature Celsius 30～60 the degree, pressure 20～60 MPas condition under extracted 1～5 hour.Wherein, as the CO of the supercriticality of extractant
2Flow rate of fluid is 10～30 liters/hour.
C. the ethanol water that contains total phenylpropanoid is collected in decompression parsing separation in separating still then, after the concentrating under reduced pressure lyophilization, obtains royal paulownia (former mutation) Cortex paulowniae total phenylpropanoid extract.Wherein, carrying out one-level decompression separation temperature in the separating still is that 30～70 degree Celsius, pressure are 5～10 MPas; The second depressurized separation temperature is that 20～60 degree Celsius, pressure are 4～9 MPas.
The specific embodiment
With reference to the following example will be more easily, more fully understand the present invention, provide embodiment and be in order to illustrate the present invention, rather than limit the present invention by any way.
Embodiment 1
Get clean, to dry in the shade and be crushed to granularity be that 70 purpose royal paulownias (former mutation) Cortex paulowniae 150 gram drops in the extraction kettles, is the CO of 15 liters/hour supercriticality with flow velocity
2Fluid is as extractant, and the ethanol water with 70% is that entrainer extracts, and is that extraction is after 2 hours under the condition of temperature 35 degree Celsius, pressure 40 MPas at the extraction environment, and decompression resolve to separate in separating still.One-level decompression separation temperature is that 50 degree Celsius, pressure are 6 MPas; The second depressurized separation temperature is that 40 degree Celsius, pressure are 5 MPas.From flash trapping stage still and secondary separating still, obtain containing the ethanol water of total phenylpropanoid, after the concentrating under reduced pressure lyophilization, obtain royal paulownia (former mutation) Cortex paulowniae total phenylpropanoid extract 2.19 grams.
Embodiment 2
Get clean, to dry in the shade and be crushed to granularity be that 50 purpose royal paulownias (former mutation) Cortex paulowniae 150 gram drops in the extraction kettles, is the CO of 20 liters/hour supercriticality with flow velocity
2Fluid is as extractant, and the ethanol water with 80% is that entrainer extracts, and is that extraction is after 4 hours under the condition of temperature 40 degree Celsius, pressure 30 MPas at the extraction environment, and decompression resolve to separate in separating still.One-level decompression separation temperature is that 45 degree Celsius, pressure are 7 MPas; The second depressurized separation temperature is that 35 degree Celsius, pressure are 6 MPas.From flash trapping stage still and secondary separating still, obtain containing the ethanol water of total phenylpropanoid, after the concentrating under reduced pressure lyophilization, obtain royal paulownia (former mutation) Cortex paulowniae total phenylpropanoid extract 2.95 grams.
Embodiment 3
Get clean, to dry in the shade and be crushed to granularity be that 40 purpose royal paulownias (former mutation) Cortex paulowniae 150 gram drops in the extraction kettles, is the CO of 25 liters/hour supercriticality with flow velocity
2Fluid is as extractant, and the ethanol water with 75% is that entrainer extracts, and is that extraction is after 3 hours under the condition of temperature 45 degree Celsius, pressure 50 MPas at the extraction environment, and decompression resolve to separate in separating still.One-level decompression separation temperature is that 40 degree Celsius, pressure are 8 MPas; The second depressurized separation temperature is that 30 degree Celsius, pressure are 7 MPas.From flash trapping stage still and secondary separating still, obtain containing the ethanol water of total phenylpropanoid, after the concentrating under reduced pressure lyophilization, obtain royal paulownia (former mutation) Cortex paulowniae total phenylpropanoid extract 2.68 grams.
Claims (3)
1. one kind is adopted supercritical CO
2The technology of fluid technique extraction royal paulownia (former mutation) Cortex paulowniae total phenylpropanoid is characterized in that: will cleaning, dry in the shade, to be crushed to granularity then be that 20～80 purpose royal paulownias (former mutation) Cortex paulowniae is put into the CO of extraction kettle with supercriticality
2Fluid is an extractant; Ethanol water with 40%～95% is that entrainer extracts; The extraction environment be temperature Celsius 30～60 the degree, pressure 20～60 MPas condition under extracted 1～5 hour; Separation is resolved in decompression in separating still then, collects the ethanol water that contains total phenylpropanoid, after the concentrating under reduced pressure lyophilization, obtains royal paulownia (former mutation) Cortex paulowniae total phenylpropanoid extract.
2. according to the described supercritical CO of claim 1
2The technology of fluid extraction royal paulownia (former mutation) Cortex paulowniae total phenylpropanoid is characterized in that: as the CO of the supercriticality of extractant
2Flow rate of fluid is 10～30 liters/hour.
3. according to the described supercritical CO of claim 1
2The technology of fluid extraction royal paulownia (former mutation) Cortex paulowniae total phenylpropanoid is characterized in that: carrying out one-level decompression separation temperature in the separating still is that 30～70 degree Celsius, pressure are 5～10 MPas; The second depressurized separation temperature is that 20～60 degree Celsius, pressure are 4～9 MPas.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 201110373864 CN102499953B (en) | 2011-11-23 | 2011-11-23 | Process for extracting total phenyl propanoid from paulownia bark of paulownia tomentosa (original variety) by adopting supercritical CO2 fluid technology |
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| CN 201110373864 CN102499953B (en) | 2011-11-23 | 2011-11-23 | Process for extracting total phenyl propanoid from paulownia bark of paulownia tomentosa (original variety) by adopting supercritical CO2 fluid technology |
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| CN102499953A true CN102499953A (en) | 2012-06-20 |
| CN102499953B CN102499953B (en) | 2013-06-19 |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ES2110474T3 (en) * | 1991-09-30 | 1998-02-16 | Suntory Ltd | PROCEDURE FOR THE PRODUCTION OF 8,11-EICOSADIENOIC ACID. |
| CN1947757A (en) * | 2006-09-16 | 2007-04-18 | 四川美大康药业股份有限公司 | Leave of glutinous rehmannia extractive, its prepn. method and use, medicines prepd. with said extractives |
| CN101012212A (en) * | 2007-02-05 | 2007-08-08 | 中国人民解放军第三○二医院 | Method of extracting coumarin by supercritical carbon dioxide |
| CN101085129A (en) * | 2007-07-11 | 2007-12-12 | 石任兵 | Acorus gramineus total phenylpropanoid extraction and total phenols extraction and method for preparing simultaneously |
| KR20080077439A (en) * | 2007-02-20 | 2008-08-25 | 박명숙 | Thermal Poultice Composition Using Mineral, Soil and Herbal Medicine |
| CN101618114A (en) * | 2009-08-04 | 2010-01-06 | 天津科技大学 | Method for preparing total glycollic glucoside of royal paulownia (original variety) fortune paulownia wood applications of same to foods and medicines |
| CN101205248B (en) * | 2007-11-28 | 2010-09-08 | 付建明 | Method for preparing ursolic acid by using paulownia leaves as raw material |
-
2011
- 2011-11-23 CN CN 201110373864 patent/CN102499953B/en not_active Expired - Fee Related
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ES2110474T3 (en) * | 1991-09-30 | 1998-02-16 | Suntory Ltd | PROCEDURE FOR THE PRODUCTION OF 8,11-EICOSADIENOIC ACID. |
| CN1947757A (en) * | 2006-09-16 | 2007-04-18 | 四川美大康药业股份有限公司 | Leave of glutinous rehmannia extractive, its prepn. method and use, medicines prepd. with said extractives |
| CN101012212A (en) * | 2007-02-05 | 2007-08-08 | 中国人民解放军第三○二医院 | Method of extracting coumarin by supercritical carbon dioxide |
| KR20080077439A (en) * | 2007-02-20 | 2008-08-25 | 박명숙 | Thermal Poultice Composition Using Mineral, Soil and Herbal Medicine |
| CN101085129A (en) * | 2007-07-11 | 2007-12-12 | 石任兵 | Acorus gramineus total phenylpropanoid extraction and total phenols extraction and method for preparing simultaneously |
| CN101205248B (en) * | 2007-11-28 | 2010-09-08 | 付建明 | Method for preparing ursolic acid by using paulownia leaves as raw material |
| CN101618114A (en) * | 2009-08-04 | 2010-01-06 | 天津科技大学 | Method for preparing total glycollic glucoside of royal paulownia (original variety) fortune paulownia wood applications of same to foods and medicines |
Non-Patent Citations (7)
| Title |
|---|
| 司传领等: "毛泡桐(原变种)内桐皮的化学成分", 《纤维素科学与技术》 * |
| 司传领等: "泡桐(原变种)果实中抑菌性苯丙素苷成分的研究(英文)", 《林产化学与工业》 * |
| 沈国良: "超临界CO_2萃取的研究与应用", 《化工时刊》 * |
| 郭明勋: "超临界CO_2萃取工艺及装置", 《明胶科学与技术》 * |
| 雷小刚，梁意红，张天喜，孙日圣，黄能贤，黄文瀛: "超临界流体萃取工艺与装置的研究和开发", 《化工机械》 * |
| 马君昌: "超临界二氧化碳萃取的研究与应用", 《辽阳石油化工高等专科学校学报》 * |
| 马燮等: "超临界CO_2萃取在中药现代化研究中的应用", 《云南化工》 * |
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