CN103484254A - Method for extraction of ligusticum chuanxiong hort. volatile oil by utilizing supercritical carbon dioxide - Google Patents
Method for extraction of ligusticum chuanxiong hort. volatile oil by utilizing supercritical carbon dioxide Download PDFInfo
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- CN103484254A CN103484254A CN201310429061.5A CN201310429061A CN103484254A CN 103484254 A CN103484254 A CN 103484254A CN 201310429061 A CN201310429061 A CN 201310429061A CN 103484254 A CN103484254 A CN 103484254A
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- extraction
- volatile oil
- ligustilide
- chuanxiong hort
- ligusticum chuanxiong
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Abstract
The invention discloses a method for extraction of ligusticum chuanxiong hort. volatile oil by utilizing supercritical carbon dioxide. The method comprises the steps as follows: the ligusticum chuanxiong hort. crude medicine is crushed into 20-40 meshes, dried and placed into a supercritical extraction device, the extraction temperature is adjusted to be 40-60 DEG C, the extraction pressure is adjusted to be 15-25 MPa, the flow of CO2 is adjusted to be 20-30 kg/h, and the time lasts for 0.5-2 h, and the ligusticum chuanxiong hort. volatile oil is collected. According to the method provided by the invention, the recovery rate of ligustilide extracted from the ligusticum chuanxiong hort. crude medicine is improved, and meanwhile, the content of the ligustilide in the total extract is further improved, so that high-quality raw material can be provided for industrial preparation of the ligustilide.
Description
Technical field
The invention belongs to natural medicine field, particularly relate to a kind of supercritical co that adopts and extract the method for volatile oil from Ligusticum wallichii.
Background technology
Ligusticum wallichii (Ligusticum chuanxiong Hort.) is umbelliferae Ligustrum plant, and its medicinal part is rhizome.Ligusticum wallichii is China's traditional Chinese medicine, has blood-activating and qi-promoting, the effect of wind-expelling pain-stopping, and Eastern Han Dynasty's Shennong's Herbal is classified it as top grade, is Cure of depression and migrainous conventional Chinese medicine.
Z-ligustilide (Ligustilide) is the main component in Rhizoma Chuanxiong oil, and according to the literature, it all has pharmacological action preferably to cardiovascular and cerebrovascular, the recycle system, immunologic function etc.
The extraction of Rhizoma Chuanxiong oil at present adopts water at atmospheric pressure vapor distillation extraction method, organic solvent extraction method and supercritical extraction.The shortcoming of atmospheric steam distillation and extraction method is yield low (Z-ligustilide is at high temperature unstable), and needs to soak for a long time, consuming time long.The organic solvent extraction method is easy to inactive substance in Ligusticum wallichii is extracted as small organic molecules such as sugar, amino acid, has brought very large difficulty to the separating-purifying of Z-ligustilide afterwards.And organic reagent is difficult to remove fully.
Summary of the invention
Purpose of the present invention aims to provide a kind of supercritical co that adopts and extract the method for Rhizoma Chuanxiong volatile oil from Ligusticum wallichii.
Specifically, a first aspect of the present invention has been to provide a kind of method of supercritical carbon dioxide extraction Rhizoma Chuanxiong volatile oil, and described method comprises the steps:
Ligusticum chuanxiong Hort is crushed to 20～40 orders, and drying, drop in supercritical extraction unit, regulates 40～60 ℃ of extraction temperature, extracting pressure 15～25Mpa, CO
2flow 20～30kg/h, the time is 0.5～2 hour, collects Rhizoma Chuanxiong volatile oil.
In a preference, described drying step comprises the dry 6～10h under 35～50 ℃ of the Ligusticum chuanxiong Hort after pulverizing.
In another preference, described method comprises the steps: Ligusticum chuanxiong Hort is crushed to 40 orders, and dry 6h under 50 ℃ drops in supercritical extraction unit, regulates 55 ℃ of extraction temperature, extracting pressure 20Mpa, CO
2flow 25kg/h, the time is 1.5 hours, collects Rhizoma Chuanxiong volatile oil.
The details of all respects of the present invention will be able to detailed description in chapters and sections subsequently.By hereinafter and the description of claim, characteristics of the present invention, purpose and advantage will be more obvious.
Embodiment
The inventor for many years uses the experience of supercritical extraction Ligusticum chuanxiong Hort based on it, the available technology adopting supercritical co is extracted from Ligusticum wallichii to the method for Rhizoma Chuanxiong volatile oil and has done further optimization and improvement.
Specifically, the invention provides a kind of method of supercritical carbon dioxide extraction Rhizoma Chuanxiong volatile oil, described method comprises the steps:
Ligusticum chuanxiong Hort is crushed to 20～40 orders, and drying, drop in supercritical extraction unit, regulates 40～60 ℃ of extraction temperature, extracting pressure 15～25Mpa, CO
2flow 20～30kg/h, the time is 0.5～2 hour, collects Rhizoma Chuanxiong volatile oil.
Preferably, described drying step comprises the dry 6～10h under 35～50 ℃ of the Ligusticum chuanxiong Hort after pulverizing.
More preferably, described method comprises the steps: Ligusticum chuanxiong Hort is crushed to 40 orders, and dry 6h under 50 ℃ drops in supercritical extraction unit, regulates 55 ℃ of extraction temperature, extracting pressure 20Mpa, CO
2flow 25kg/h, the time is 1.5 hours, collects Rhizoma Chuanxiong volatile oil.
The content of the Z-ligustilide in Jehol Ligusticum Rhizome medicinal material and volatile oil thereof and the rate of transform thereof can record by liquid phase chromatography, concrete operation step as: get the brown bottle that 500mg Ligusticum chuanxiong Hort or its volatile oil are placed in 100ml, add 25ml methyl alcohol, airtight, weigh, take out after ultrasonic 90ml, weigh, supply weightlessness, shake up, after getting supernatant liquid filtering after standing, get 5ul feed liquor phase.
The liquid-phase condition of measuring Z-ligustilide is as follows: Agilent Zorbax C
18post (4.6mm * 250mm); Moving phase: acetonitrile-water (60:40); Detect wavelength: 350nm; Flow velocity 1.0mLmin
-1; Column temperature: 20 ℃; Sample size: 2uL.
The standard substance preparation: precision takes the about 10mg of wormwood artemisia benzene lactone reference substance, puts in the brown measuring bottle volumetric flask of 10mL, adds anhydrous methanol and is diluted to scale, shakes up, and makes the reference substance solution mother liquor of about 1.0mg/mL.Get wherein 2.5mL solution and put in the brown measuring bottle volumetric flask of 10mL, add anhydrous methanol and be diluted to scale, shake up, make the reference substance solution of about 0.25mg/mL, the demarcation liquid of using as assay commonly used.
The trial-product preparation: the close about 0.5g of Ligusticum chuanxiong Hort sample (20 order) that takes, to put in 60mL tool plug brown bottle, precision adds methyl alcohol 25mL, airtight, weighs.Supersound extraction 90min, taking-up is weighed, and supplies weightlessness.Shake up, standing, get supernatant liquor and filter filter through micropore, as need testing solution.
Compared with prior art, it has following advantage to method of the present invention:
1) method of the present invention operates at low temperatures, makes Z-ligustilide be difficult for transforming;
2) method of the present invention has been optimized the condition of supercritical extraction Ligusticum wallichii, makes Z-ligustilide more fully to be extracted, and has guaranteed the content of Z-ligustilide in total extract (Rhizoma Chuanxiong volatile oil) simultaneously;
3) method of the present invention (not adding properties-correcting agent) easy and simple to handle, short (minimum only need 0.5 hour) consuming time, reproducible.
Method of the present invention has improved the rate of recovery (more than 80%) of extraction Z-ligustilide from Ligusticum chuanxiong Hort, has also improved the content (40%～55%) of Z-ligustilide in total extract simultaneously, so can provide high-quality raw material for the industry preparation of Z-ligustilide.
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only are not used in and limit the scope of the invention for the present invention is described.The experimental technique of unreceipted actual conditions in the following example, usually according to normal condition or the condition of advising according to manufacturer.Unless otherwise indicated, otherwise all percentage ratio, ratio, ratio or umber by weight.
Unless otherwise defined, the same meaning that all specialties of using in literary composition and scientific words and one skilled in the art are familiar.In addition, any method similar or impartial to described content and material all can be applicable in the inventive method.The use that better implementation method described in literary composition and material only present a demonstration.
The above-mentioned feature that the present invention mentions, or the feature that embodiment mentions can arbitrary combination.All features that patent specification discloses can with any composition forms use, each feature disclosed in specification sheets, can anyly provide the alternative characteristics of identical, impartial or similar purpose to replace.Therefore except special instruction is arranged, the feature disclosed is only the general example of equalization or similar features.
The supercritical extraction of embodiment 1 Rhizoma Chuanxiong volatile oil
Ligusticum wallichii medicine materical crude slice 1kg, be ground into 40 order powder, and dry 6h under 50 ℃ drops into above-mentioned dried Ligusticum wallichii sample in supercritical extraction unit, regulates 55 ℃ of extraction temperature, extracting pressure 20Mpa, CO
2flow 25kg/h, the time is 1.5h, directly in the extraction kettle outlet, with brown wide-necked bottle, collects Rhizoma Chuanxiong volatile oil.The final Rhizoma Chuanxiong volatile oil 37.1g that obtains, the volatile oil yield is 3.71%, and through Liquid Detection (Step By Condition is as follows), wherein Z-ligustilide content is 51.7%, and the rate of transform of Z-ligustilide is 96.7%.
The step of measuring Z-ligustilide is as follows: gets the brown bottle that 500mg Ligusticum chuanxiong Hort or its volatile oil are placed in 100ml, adds 25ml methyl alcohol, and airtight, weigh, take out after ultrasonic 90ml, weigh, supply weightlessness, shake up, after getting supernatant liquid filtering after standing, get 5ul feed liquor phase.
The liquid-phase condition of measuring Z-ligustilide is as follows: Agilent Zorbax C
18post (4.6mm * 250mm); Moving phase: acetonitrile-water (60:40); Detect wavelength: 350nm; Flow velocity 1.0mLmin
-1; Column temperature: 20 ℃; Sample size: 2uL.
The standard substance preparation: precision takes the about 10mg of wormwood artemisia benzene lactone reference substance, puts in the brown measuring bottle volumetric flask of 10mL, adds anhydrous methanol and is diluted to scale, shakes up, and makes the reference substance solution mother liquor of about 1.0mg/mL.Get wherein 2.5mL solution and put in the brown measuring bottle volumetric flask of 10mL, add anhydrous methanol and be diluted to scale, shake up, make the reference substance solution of about 0.25mg/mL, the demarcation liquid of using as assay commonly used.
The trial-product preparation: the close about 0.5g of sample (20 order) that takes, to put in 60mL tool plug brown bottle, precision adds methyl alcohol 25mL, airtight, weighs.Supersound extraction 90min, taking-up is weighed, and supplies weightlessness.Shake up, standing, get supernatant liquor and filter filter through micropore, as need testing solution.
The supercritical extraction of embodiment 2 Rhizoma Chuanxiong volatile oils
Ligusticum wallichii medicine materical crude slice 1kg, be ground into 20 order powder, and dry 10h under 35 ℃ drops into above-mentioned dried Ligusticum wallichii sample in supercritical extraction unit, regulates 40 ℃ of extraction temperature, extracting pressure 15Mpa, CO
2flow 30kg/h, the time is 0.5 hour, directly in the extraction kettle outlet, with brown wide-necked bottle, collects Rhizoma Chuanxiong volatile oil.The final Rhizoma Chuanxiong volatile oil 32.4g that obtains, yield is 3.24%, and through Liquid Detection (step and condition are with embodiment 1), wherein Z-ligustilide content is 49.7%, and the rate of transform of Z-ligustilide is 81.2%.
The supercritical extraction of embodiment 3 Rhizoma Chuanxiong volatile oils
Ligusticum wallichii medicine materical crude slice 1kg, be ground into 40 order powder after removing impurity, dry 7h under 45 ℃, and above-mentioned dried Ligusticum wallichii sample drops in supercritical extraction unit, regulates 60 ℃ of extraction temperature, extracting pressure 25Mpa, CO
2flow 20kg/h, the time is 2 hours, directly in the extraction kettle outlet, with brown wide-necked bottle, collects Rhizoma Chuanxiong volatile oil.The final Rhizoma Chuanxiong volatile oil 42.3g that obtains, yield is 4.23%, and through Liquid Detection (step and condition are with embodiment 1), wherein Z-ligustilide content is 41.1%, and the rate of transform of Z-ligustilide is 87.7%.
The supercritical extraction of embodiment 4 Rhizoma Chuanxiong volatile oils
Ligusticum wallichii medicine materical crude slice 1kg, be ground into 30 order powder after removing impurity, dry 8h under 40 ℃, and above-mentioned dried Ligusticum wallichii sample drops in supercritical extraction unit, regulates 50 ℃ of extraction temperature, extracting pressure 20Mpa, CO
2flow 25kg/h, the time is 1 hour, directly in the extraction kettle outlet, with brown wide-necked bottle, collects Rhizoma Chuanxiong volatile oil.The final Rhizoma Chuanxiong volatile oil 38.6g that obtains, yield is 3.86%, and through Liquid Detection (step and condition are with embodiment 1), wherein Z-ligustilide content is 43.7%, and the rate of transform of Z-ligustilide is 85.1%.
Many aspects involved in the present invention have been done as above and have been set forth.Yet, it should be understood that before not departing from spirit of the present invention and put, those skilled in the art can be equal to and change and modify it, and described change and modification fall into the coverage of the application's claims equally.
Claims (3)
1. the method for a supercritical carbon dioxide extraction Rhizoma Chuanxiong volatile oil, is characterized in that, described method comprises the steps:
Ligusticum chuanxiong Hort is crushed to 20～40 orders, and drying, drop in supercritical extraction unit, regulates 40～60 ℃ of extraction temperature, extracting pressure 15～25Mpa, CO
2flow 20～30kg/h, the time is 0.5～2 hour, collects Rhizoma Chuanxiong volatile oil.
2. the method for claim 1, is characterized in that, described drying step comprises the dry 6～10h under 35～50 ℃ of the Ligusticum chuanxiong Hort after pulverizing.
3. method as claimed in claim 1 or 2, is characterized in that, it comprises the steps:
Ligusticum chuanxiong Hort is crushed to 40 orders, and dry 6h under 50 ℃, drop in supercritical extraction unit, regulates 55 ℃ of extraction temperature, extracting pressure 20Mpa, CO
2flow 25kg/h, the time is 1.5 hours, collects Rhizoma Chuanxiong volatile oil.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104971513A (en) * | 2015-06-15 | 2015-10-14 | 昆明理工大学 | Method for extracting volatile oil and polyphenol from tsaoko fruit |
| CN109078046A (en) * | 2018-10-12 | 2018-12-25 | 广州医科大学 | A kind of supercritical CO2The method for extracting volatile oil in the dizzy soup in town |
| CN109456830A (en) * | 2018-11-27 | 2019-03-12 | 河南羚锐制药股份有限公司 | The supercritical extraction method of volatile oil in a kind of activating meridians to stop pain plaster material |
| CN111481489A (en) * | 2020-05-20 | 2020-08-04 | 四川绿色本草科技发展有限公司 | Ligusticum wallichii extract with mosquito repelling and itching relieving effects and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1352980A (en) * | 2001-11-30 | 2002-06-12 | 广州中医药大学科技产业园有限公司 | Medicine for treating hemicrania and its preparing process |
| CN1502353A (en) * | 2002-11-20 | 2004-06-09 | 北京瑞康医药技术有限公司 | Compound chuanxiong and angelica total extract and preparation, use thereof |
| CN1565601A (en) * | 2003-07-04 | 2005-01-19 | 成都永泽药物研究开发有限责任公司 | Application of sichuan lovage rhizome oil by supercritical CO2 extraction method in pharmacy |
| CN1572310A (en) * | 2003-06-11 | 2005-02-02 | 山东绿叶天然药物研究开发有限公司 | Chuanxiong rhizome volatile oil soft capsule and its preparation method |
| CN1857346A (en) * | 2006-03-29 | 2006-11-08 | 广州合诚三先生物科技有限公司 | Extraction process of effective Chuanxiong component |
-
2013
- 2013-09-18 CN CN201310429061.5A patent/CN103484254A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1352980A (en) * | 2001-11-30 | 2002-06-12 | 广州中医药大学科技产业园有限公司 | Medicine for treating hemicrania and its preparing process |
| CN1502353A (en) * | 2002-11-20 | 2004-06-09 | 北京瑞康医药技术有限公司 | Compound chuanxiong and angelica total extract and preparation, use thereof |
| CN1572310A (en) * | 2003-06-11 | 2005-02-02 | 山东绿叶天然药物研究开发有限公司 | Chuanxiong rhizome volatile oil soft capsule and its preparation method |
| CN1565601A (en) * | 2003-07-04 | 2005-01-19 | 成都永泽药物研究开发有限责任公司 | Application of sichuan lovage rhizome oil by supercritical CO2 extraction method in pharmacy |
| CN1857346A (en) * | 2006-03-29 | 2006-11-08 | 广州合诚三先生物科技有限公司 | Extraction process of effective Chuanxiong component |
Non-Patent Citations (6)
| Title |
|---|
| 叶璟: "川芎有效成分的提取技术", 《中国高新技术企业》, no. 15, 1 August 2009 (2009-08-01), pages 55 - 56 * |
| 吴广通等: "超临界流体萃取法对川芎挥发油成分的研究", 《药学服务与研究》, no. 01, 30 November 2011 (2011-11-30), pages 61 - 62 * |
| 张伟等: "超临界CO2流体提取复方川芎丹参中的有效成分", 《食品与发酵工业》, vol. 36, no. 11, 31 December 2010 (2010-12-31), pages 183 - 188 * |
| 张爱军等: "川芎超临界流体CO2萃取挥发油-β-环糊精包合物制备工艺研究", 《中国中药杂志》, vol. 29, no. 01, 31 January 2004 (2004-01-31) * |
| 王平等: "川芎、高良姜等挥发油的水蒸汽蒸馏法和超临界流体萃取法比较研究", 《中成药》, vol. 26, no. 06, 30 June 2004 (2004-06-30), pages 440 - 443 * |
| 许玫等: "超临界提取与色谱技术联用制备藁本内酯及相关研究", 《中成药》, vol. 29, no. 11, 30 November 2007 (2007-11-30), pages 1671 - 1673 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104971513A (en) * | 2015-06-15 | 2015-10-14 | 昆明理工大学 | Method for extracting volatile oil and polyphenol from tsaoko fruit |
| CN104971513B (en) * | 2015-06-15 | 2016-10-12 | 昆明理工大学 | A kind of extract volatile oil and the method for polyphenol in Fructus Tsaoko fruit |
| CN109078046A (en) * | 2018-10-12 | 2018-12-25 | 广州医科大学 | A kind of supercritical CO2The method for extracting volatile oil in the dizzy soup in town |
| CN109078046B (en) * | 2018-10-12 | 2021-06-25 | 广州医科大学 | Supercritical CO2Method for extracting volatile oil from anti-dizziness decoction |
| CN109456830A (en) * | 2018-11-27 | 2019-03-12 | 河南羚锐制药股份有限公司 | The supercritical extraction method of volatile oil in a kind of activating meridians to stop pain plaster material |
| CN111481489A (en) * | 2020-05-20 | 2020-08-04 | 四川绿色本草科技发展有限公司 | Ligusticum wallichii extract with mosquito repelling and itching relieving effects and application thereof |
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Application publication date: 20140101 |