CN1810756A - Supercritical CO2 extraction process of total rhubarb anthraquinone - Google Patents
Supercritical CO2 extraction process of total rhubarb anthraquinone Download PDFInfo
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- CN1810756A CN1810756A CNA2006100571605A CN200610057160A CN1810756A CN 1810756 A CN1810756 A CN 1810756A CN A2006100571605 A CNA2006100571605 A CN A2006100571605A CN 200610057160 A CN200610057160 A CN 200610057160A CN 1810756 A CN1810756 A CN 1810756A
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- anthraquinone
- rhubarb
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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 present invention belongs to the field of effective Chinese medicine component extracting technology, and is especially supercritical CO2 extraction process of total rhubarb anthraquinone. Rhubarb powder through or through no acid solution treatment is soaked in alcohol or other solvent and extracted in a extracting reactor with supercritical CO2 as extractant and alcohol as entrainer and solvent at pressure of 20-60 Mpa and temperature of 30-60 deg.c for 0.5-3 hr. The extracted matter is decompression separated in a separating tank at 15-45 deg.c, and alcohol solution of total rhubarb anthraquinone is collected and decompression concentrated and dried to obtain total rhubarb anthraquinone.
Description
Technical field
The invention belongs to extracts active ingredients technical field in the Chinese medicine, be specifically related to adopt the technical field of effective constituent general anthraquinone in the super critical CO 2 technology extraction rheum officinale.
Background technology
Rheum officinale is the dry root and rhizome of polygonum rheum palmatum Rheum palmatum L., Rheum tanguticum Rheum tanguticum Maxim.ex Balf. or Rheum officinale Rheum officinaleBaill..The rheum officinale logical intestines that purge heat, removing pattogenic heat from the blood and toxic material from the body is stimulated the menstrual flow by the stasis of blood.
Rheum officinale is one of four big the most frequently used Chinese medicines, has kind more than 800 to contain rheum officinale approximately in the national 8000 plurality of Chinese preparations.Rheum officinale has discharge function, promptly as cathartic, is used for the treatment of constipation due to dry stool, constipation with heat retention since ancient times, and most of lowering blood-fat and reducing weights, toxin-expelling and face nourishing class Chinese patent medicine and protective foods all contain rheum officinale.Contain free type anthraquinones such as Schuttgelb, chrysophanol, rhubarb yellow, rhabarberone, rheochrysidin in the rheum officinale, combined anthraquinones such as chrysophan, Schuttgelb glycosides, rheochrysidin glycosides, rheochrysidin two glycosides, Barbaloin, rheinoside, dianthracene quinones compositions such as anthraglucosennin.Anthraquinone component in the rheum officinale is the major cause that produces discharge function,
At present, obtain that the Radix Et Rhizoma Rhei anthraquinone constituents is commonly used to have organic solvent extraction such as alcohol, benzene, chloroform, pyridine to separate the method that combines with polyamide resin, this method exists that efficient is low, complicated operation, dissolvent residual, human body is produced a series of problems such as detrimentally affect.
Supercritical liquid extraction technique is to utilize to be in supercritical carbon dioxide fluidic excellent dissolution performance and bigger spread coefficient and to treat separate substance and carry out the extraction separation purifying, has advantages such as environmental protection, economy, no solvent residue.The extraction ability that can improve the supercritical state carbonic acid gas by the condition and the technology of change extraction.
According to literature search, up to the present still there is not the report that adopts supercritical carbon dioxide extraction general rhubarb anthraquinone extract.
Summary of the invention
The invention discloses a kind of method that adopts supercritical carbon dioxide extraction method to extract effective constituent general anthraquinone in the rheum officinale.
This method comprises following technical scheme:
A kind of method of supercritical carbon dioxide extraction general anthraquinone, this method comprises the steps:
1) with after the rheum officinale raw material pulverizing, Rhubarb is carried out pre-treatment, described pretreatment process is to select for use a kind of in ethanol, chloroform and/or the ether that Rhubarb spray was soaked into 1～3 hour, and described ethanol is that concentration is 50% to dehydrated alcohol; Described pretreated method also can be a kind of infiltration Rhubarb of selecting for use in 5～20% hydrochloric acid, dilute sulphuric acid and/or the acetic acid 1～3 hour, after the drying, soaked into 1～3 hour with a kind of Rhubarb is sprayed in ethanol, chloroform and/or the ether;
2) pretreated rheum officinale raw material is placed extraction kettle, with the supercritical carbon dioxide is extraction solvent, with flow velocity is that 0.2～0.5 times of rheum officinale volume of ethanol of 2～5 ml/min is as entrainment agent and solvent, at pressure is that 20～60Mpa, temperature are to extract 0.5～3 hour under 30～60 ℃ the condition, and described ethanol is that concentration is 60% to dehydrated alcohol;
3) in the separating still 15～45 ℃ of temperature down decompression resolve and separate, collect the ethanolic soln that contains general rhubarb anthraquinone, after the concentrating under reduced pressure drying, obtain the general anthraquinone extract.
The method of supercritical carbon dioxide extraction general anthraquinone extracts the application of general anthraquinone in containing the anthraquinone component Chinese medicinal materials.
The method of supercritical carbon dioxide extraction general anthraquinone is in the application of extraction in the general anthraquinone, and the wherein said Chinese medicinal materials that contains anthraquinone component is selected from a kind of in Tuber Fleeceflower Root, aloe, Semen Cassiae, sennae, giant knotweed and/or the madder.
The present invention compares with traditional method of obtaining the general anthraquinone extract, has the following advantages:
1) carbonic acid gas is as the supercritical extraction agent, environmental protection, nontoxic, organic solvent-free is residual, do not corrode extraction equipment.Supercritical carbon dioxide extraction has advantages such as efficient height, extraction time is short, service temperature is low, pollution is few as a kind of " green " extraction and separation technology.In recent years, supercritical carbon dioxide extraction is showing extraordinary application prospect aspect the Chinese herbal medicine extracting separation.
2) rhubarb medicinal material is carried out pre-treatment, and in leaching process, use ethanol to change the extraction ability of above-critical state carbonic acid gas, can increase its scope of application, extract the relatively large material of polarity, also can be used for the extraction of solid crystals.
3) utilize the method for supercritical carbon dioxide extraction general rhubarb anthraquinone, can avoid using a large amount of organic solvents, can avoid the pyrohydrolysis of combined anthraquinone, the sample yield is greater than 2.0%, the content of general anthraquinone can satisfy the demand of industrialized mass production greater than 30% in the sample.
Embodiment
Below in conjunction with embodiment the present invention is carried out specific description, but following embodiment does not represent limitation of the present invention.
Embodiment 1
Take by weighing rhubarb medicinal material powder 1.5kg, spray infiltration with 50% ethanol 300m1, after airtight vexed 0.5 hour, put into the supercritical extraction unit extraction kettle of 5L specification, with the supercritical carbon dioxide is extraction solvent, extraction process is that 20Mpa, temperature are that 30 ℃, time are to carry out in 0.5 hour the environment at pressure, in whole leaching process, is that 60% ethanol extracts as entrainment agent and solvent with the 300ml concentration of 5 ml/min flow velocitys; Under 15 ℃ of temperature, reduce pressure to resolve in the separating still and separate, collect the about 550ml of ethanolic soln of general rhubarb anthraquinone, obtain its extract 30.0g after the concentrating under reduced pressure drying, sample yield 2.00%, the content of general anthraquinone is 32.5% in the sample.
Embodiment 2
Take by weighing rhubarb medicinal material powder 1.5kg, spray infiltration with 95% ethanol 300ml, after airtight vexed 3 hours, put into the supercritical extraction unit extraction kettle of 5L specification, with the supercritical carbon dioxide is extraction solvent, extraction process is that 35Mpa, temperature are that 50 ℃, time are to carry out in 2 hours the environment at pressure, in whole leaching process, is that the concentration of 3 ml/min is that 95% ethanol extracts as entrainment agent and solvent with the 500ml flow velocity; Under 25 ℃ of temperature, reduce pressure to resolve in the separating still and separate, collect the about 800ml of ethanolic soln of general rhubarb anthraquinone, obtain its extract 32.1g after the concentrating under reduced pressure drying, sample yield 2.14%, the content of general anthraquinone is 36.4% in the sample.
Embodiment 3
Take by weighing rhubarb medicinal material 1.5kg and be ground into fine powder, spray infiltration with dehydrated alcohol 300ml, after airtight vexed 1 hour, put into the supercritical extraction unit extraction kettle of 5L specification, with the supercritical carbon dioxide is extraction solvent, extraction process is that 30Mpa, temperature are that 40 ℃, time are to carry out in 3 hours the environment at pressure, in whole leaching process, is that the concentration of 2 ml/min is that 90% ethanol extracts as entrainment agent and solvent with the 750ml flow velocity; Under 30 ℃ of temperature, reduce pressure to resolve in the separating still and separate, collect the about 1000ml of ethanolic soln of general rhubarb anthraquinone, obtain its extract 38.0g after the concentrating under reduced pressure drying, sample yield 2.53%, the content of general anthraquinone is 31.5% in the sample.
Embodiment 4
Take by weighing rhubarb medicinal material powder 1.5kg, soak into 5% hydrochloric acid soln 300ml, after airtight vexed 1 hour, drying; Dry Rhubarb is sprayed infiltration with 50% ethanol 300ml, after airtight vexed 0.5 hour, put into the supercritical extraction unit extraction kettle of 5L specification, with the supercritical carbon dioxide is extraction solvent, extraction process is that 20Mpa, temperature are that 30 ℃, time are to carry out in 0.5 hour the environment at pressure, in whole leaching process, be that the concentration of 5 ml/min is that 90% ethanol extracts as entrainment agent and solvent with the 300ml flow velocity; Under 15 ℃ of temperature, reduce pressure to resolve in the separating still and separate, collect the about 550ml of ethanolic soln of general rhubarb anthraquinone, obtain its extract 36.0g after the concentrating under reduced pressure drying, sample yield 2.40%, the content of general anthraquinone is 30.9% in the sample.
Embodiment 5
Take by weighing rhubarb medicinal material powder 1.5kg, soak into 8% hydrochloric acid soln 300ml, after airtight vexed 2 hours, drying; Dry Rhubarb is sprayed infiltration with 95% ethanol 300ml, after airtight vexed 3 hours, put into the supercritical extraction unit extraction kettle of 5L specification, with the supercritical carbon dioxide is extraction solvent, extraction process is that 35Mpa, temperature are that 50 ℃, time are to carry out in 2 hours the environment at pressure, in whole leaching process, be that the concentration of 3 ml/min is that 95% ethanol extracts as entrainment agent and solvent with the 500ml flow velocity; Under 25 ℃ of temperature, reduce pressure to resolve in the separating still and separate, collect the about 800ml of ethanolic soln of general rhubarb anthraquinone, obtain its extract 47.6g after the concentrating under reduced pressure drying, sample yield 3.17%, the content of general anthraquinone is 35.3% in the sample.
Embodiment 6
Take by weighing rhubarb medicinal material powder 1.5kg, soak into 20% hydrochloric acid soln 300ml, after airtight vexed 3 hours, drying; Dry Rhubarb is sprayed infiltration with dehydrated alcohol 300ml, after airtight vexed 1 hour, put into the supercritical extraction unit extraction kettle of 5L specification, with the supercritical carbon dioxide is extraction solvent, extraction process is that 30Mpa, temperature are that 40 ℃, time are to carry out in 3 hours the environment at pressure, in whole leaching process, be that the concentration of 2 ml/min is that 60% ethanol extracts as entrainment agent and solvent with the 750ml flow velocity; Under 25 ℃ of temperature, reduce pressure to resolve in the separating still and separate, collect the about 1000ml of ethanolic soln of general rhubarb anthraquinone, obtain its extract 48.0g after the concentrating under reduced pressure drying, sample yield 3.20%, the content of general anthraquinone is 32.3% in the sample.
Embodiment 7
Taking by weighing rhubarb medicinal material powder 1.5kg, is that 10% dilute sulphuric acid 300ml soaks into concentration, after airtight vexed 3 hours, and drying; Dry Rhubarb is sprayed infiltration with chloroform 300m1, after airtight vexed 3 hours, put into the supercritical extraction unit extraction kettle of 5L specification, with the supercritical carbon dioxide is extraction solvent, extraction process is that 35Mpa, temperature are that 50 ℃, time are to carry out in 2 hours the environment at pressure, in whole leaching process, be that the concentration of 3 ml/min is that 95% ethanol extracts as entrainment agent and solvent with the 500ml flow velocity; Under 25 ℃ of temperature, reduce pressure to resolve in the separating still and separate, collect the about 750ml of ethanolic soln of general rhubarb anthraquinone, obtain its extract 36.5g after the concentrating under reduced pressure drying, sample yield 2.43%, the content of general anthraquinone is 37.4% in the sample.
Claims (7)
1, a kind of method of supercritical carbon dioxide extraction general anthraquinone is characterized in that: this method comprises the steps:
1) with after the rheum officinale raw material pulverizing, Rhubarb is carried out pre-treatment;
2) pretreated rheum officinale raw material is placed extraction kettle, with the supercritical carbon dioxide is extraction solvent, with flow velocity be 0.2～0.5 times of rheum officinale volume of ethanol of 2～5 ml/min as entrainment agent and solvent, be that 20～60Mpa, temperature are to extract 0.5～3 hour under 30～60 ℃ the condition at pressure;
3) in the separating still 15～45 ℃ of temperature down decompression resolve and separate, collect the ethanolic soln that contains general rhubarb anthraquinone, after the concentrating under reduced pressure drying, obtain the general anthraquinone extract.
2, the method for the described supercritical carbon dioxide extraction general anthraquinone of claim 1 is characterized in that: the pretreatment process described in the step 1) is to select for use a kind of Rhubarb is sprayed in ethanol, chloroform and/or the ether to soak into 1～3 hour.
3, the method for the described supercritical carbon dioxide extraction general anthraquinone of claim 1, it is characterized in that: the pretreatment process described in the step 1) is a kind of infiltration Rhubarb 1～3 hour of selecting for use in 5～20% hydrochloric acid, dilute sulphuric acid and/or the acetic acid, after the drying, soaked into 1～3 hour with a kind of Rhubarb is sprayed in ethanol, chloroform and/or the ether.
4, the method for the described supercritical carbon dioxide extraction general anthraquinone of claim 2 is characterized in that: described ethanol is that concentration is 50% to dehydrated alcohol.
5, the method for the described supercritical carbon dioxide extraction general anthraquinone of claim 1 is characterized in that: step 2) described in ethanol be that concentration is 60% to dehydrated alcohol.
6, the method for the described supercritical carbon dioxide extraction general anthraquinone of claim 1 extracts the application of general anthraquinone in containing the anthraquinone component Chinese medicinal materials.
7, the described application of claim 6 is characterized in that: the described Chinese medicinal materials that contains anthraquinone component is selected from a kind of in Tuber Fleeceflower Root, aloe, Semen Cassiae, sennae, giant knotweed and/or the madder.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102240327A (en) * | 2011-04-29 | 2011-11-16 | 栗进才 | Method for extracting total anthraquinone in rhubarb from traditional Chinese medicine rhubarb by supercritical fluid |
| CN102558131A (en) * | 2010-12-24 | 2012-07-11 | 苏州宝泽堂医药科技有限公司 | Method for extracting swertiamarin with supercritical fluid |
| CN103656493A (en) * | 2013-11-22 | 2014-03-26 | 山东中大药业有限公司 | Preparation method and application of stasis removing and stomach tonifying tablet |
| CN101855330B (en) * | 2008-12-04 | 2014-05-07 | 马来西亚博特拉大学 | Extractions of fixed oil and thymoquinone rich fractions (TQRF) |
| CN103893283A (en) * | 2012-12-28 | 2014-07-02 | 西安世纪盛康药业有限公司 | Traditional Chinese medicine composition for treatment of chronic renal diseases and chronic renal failure and its preparation method and use |
| CN103893286A (en) * | 2012-12-28 | 2014-07-02 | 西安世纪盛康药业有限公司 | Traditional Chinese medicinal preparation for treating chronic renal disease and preparation method thereof |
| CN111205927A (en) * | 2020-01-16 | 2020-05-29 | 河北瑞龙生物科技有限公司 | Peony essential oil extraction method |
| CN111268862A (en) * | 2020-03-05 | 2020-06-12 | 东南大学 | Method for enhancing MFC power generation by using anthraquinone traditional Chinese medicine plant contents as redox mediator |
| FR3099170A1 (en) * | 2019-07-24 | 2021-01-29 | Christine D'INGRANDO | Extraction of anthraquinones from madder products |
| CN116077551A (en) * | 2023-02-24 | 2023-05-09 | 马鞍山市食品药品检验和药品不良反应监测中心 | Supercritical fluid CO 2 Method for extracting senna leaf effective component |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN100441557C (en) * | 2006-01-25 | 2008-12-10 | 北京盖雅环境科技有限公司 | Method for extracting rhubarb powder dissociated anthraquinone by supercritical acid hydrolysis |
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2006
- 2006-03-13 CN CNB2006100571605A patent/CN100408536C/en not_active Expired - Fee Related
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101855330B (en) * | 2008-12-04 | 2014-05-07 | 马来西亚博特拉大学 | Extractions of fixed oil and thymoquinone rich fractions (TQRF) |
| CN102558131A (en) * | 2010-12-24 | 2012-07-11 | 苏州宝泽堂医药科技有限公司 | Method for extracting swertiamarin with supercritical fluid |
| CN102240327A (en) * | 2011-04-29 | 2011-11-16 | 栗进才 | Method for extracting total anthraquinone in rhubarb from traditional Chinese medicine rhubarb by supercritical fluid |
| CN103893283B (en) * | 2012-12-28 | 2017-03-29 | 西安世纪盛康药业有限公司 | A kind of Chinese medicine composition for treating chronic kidney disease and chronic kidney hypofunction and preparation method thereof |
| CN103893283A (en) * | 2012-12-28 | 2014-07-02 | 西安世纪盛康药业有限公司 | Traditional Chinese medicine composition for treatment of chronic renal diseases and chronic renal failure and its preparation method and use |
| CN103893286A (en) * | 2012-12-28 | 2014-07-02 | 西安世纪盛康药业有限公司 | Traditional Chinese medicinal preparation for treating chronic renal disease and preparation method thereof |
| CN103893286B (en) * | 2012-12-28 | 2017-03-29 | 西安世纪盛康药业有限公司 | It is a kind of to treat Chinese medicine preparation of chronic renal disease and preparation method thereof |
| CN103656493A (en) * | 2013-11-22 | 2014-03-26 | 山东中大药业有限公司 | Preparation method and application of stasis removing and stomach tonifying tablet |
| FR3099170A1 (en) * | 2019-07-24 | 2021-01-29 | Christine D'INGRANDO | Extraction of anthraquinones from madder products |
| CN111205927A (en) * | 2020-01-16 | 2020-05-29 | 河北瑞龙生物科技有限公司 | Peony essential oil extraction method |
| CN111268862A (en) * | 2020-03-05 | 2020-06-12 | 东南大学 | Method for enhancing MFC power generation by using anthraquinone traditional Chinese medicine plant contents as redox mediator |
| CN111268862B (en) * | 2020-03-05 | 2022-02-15 | 东南大学 | Method for enhancing MFC power generation by using anthraquinone traditional Chinese medicine plant contents as redox mediator |
| CN116077551A (en) * | 2023-02-24 | 2023-05-09 | 马鞍山市食品药品检验和药品不良反应监测中心 | Supercritical fluid CO 2 Method for extracting senna leaf effective component |
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