CN103710152A - Method for using supercritical carbon dioxide for extraction of chrysanthemum essential oil - Google Patents
Method for using supercritical carbon dioxide for extraction of chrysanthemum essential oil Download PDFInfo
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- CN103710152A CN103710152A CN201310512626.6A CN201310512626A CN103710152A CN 103710152 A CN103710152 A CN 103710152A CN 201310512626 A CN201310512626 A CN 201310512626A CN 103710152 A CN103710152 A CN 103710152A
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Abstract
The invention discloses a method for using supercritical carbon dioxide for extraction of chrysanthemum essential oil, dry and crushed chrysanthemum is used as a raw material, the supercritical carbon dioxide uses anhydrous ethanol as an entrainer to extract a chamomile essential oil raw thick liquid, then the raw thick liquid is frozen, filtered and concentrated to obtain the high purity chamomile essential oil. The high purity chamomile essential oil product has high extraction yield, high purity, no toxicity, no residue, pure color, stable characters, pure naturalness and other characteristics, and is simple in process and low in energy consumption.
Description
Technical field
The present invention relates to a kind of vegetable oil extraction method, be specifically related to a kind of method with supercritical carbon dioxide extraction chrysanthemum essential oil.
Background technology
Chrysanthemum is feverfew, is Chinese conventional Chinese medicine, has the effect of dispelling wind, heat-clearing, improving eyesight, removing toxic substances.The diseases such as primary treatment headache, dizzy, hot eyes, ambition dysphoria with smothery sensation, furunculosis, pyogenic infections.Modern pharmacological research shows, chrysanthemum has treatment coronary heart disease, reduces blood pressure, prevents hyperlipidemia, antibacterial, antiviral, anti-inflammatory, the anti-ageing multiple pharmacologically active of waiting for a long time.China's Chrysanthemum morifolium has eight large main flow merchandise resourceses on market, be respectively Hang Ju, Bo chrysanthemum, tribute chrysanthemum, Chu chrysanthemum, Qi Ju, bosom chrysanthemum, Ji chrysanthemum, Huang Ju, and < < Chinese Pharmacopoeia > > I portion (version in 2000) is according to the difference of the chrysanthemum place of production and working method, Bo chrysanthemum, Chu chrysanthemum, tribute chrysanthemum and Hang Ju four strains have been recorded.Chrysanthemum is medicinal and edible plant, both at home and abroad to its classification, identify, all there is report the aspect such as chemical, clinical, pharmacology.
The chemical composition more complicated of chrysanthemum, wherein flavonoid compound, triterpene compound and volatile oil are its main effective constituent.Volatile oil--to four kinds, different places of production chrysanthemum: in Bo chrysanthemum, bosom chrysanthemum, Chu chrysanthemum and Hang Ju, volatile oil has carried out assay, finds that in Chu chrysanthemum, content is the highest; Adopt gas chromatography mass spectrometry technology to carry out preliminary study to volatile oil component simultaneously, identify more than 20 and plant ter penoids.Application gas chromatography mass spectrometry technology is to bosom chrysanthemum and the chemical composition of volatile oil of cherishing greatly chrysanthemum forms and character is analyzed, and experimental result shows that the main component of volatile oil of chrysanthemum is monoterpene, sesquiterpenoids and containing oxygen derivative thereof; In addition from the volatile oil of chrysanthemum of bosom, identify 40 compounds, from the chrysanthemum of large bosom, identified 27 compounds.Also adopt gas chromatography mass spectrometry technology, chemical composition of volatile oil in Hang Ju is analyzed, identify 50 compounds, and determined the relative percentage composition of each composition.
The effect that chrysanthemum has wind-dispelling heat-dissipating, detoxify and promote the subsdence of swelling, relieve sore throat improving eyesight, reduces blood pressure.Research shows, chrysanthemum essential oil can strengthen capillary resistance, reduces metabolism of lipid and cholesterol content in blood, has the effect that improves myocardial nutrition, anti-inflammatory, Scavenger of ROS free radical; To suppressing tumour, delaying senility and strengthening body immunity has certain effect.
The extracting method of chrysanthemum essential oil is mainly water extraction and ultrasonic-assisted extraction at present, and this extracting method energy consumption is large, and need to use the reagent such as normal hexane, sodium sulfate, ethanol, easily causes reagent residual, and purity is not high.
Summary of the invention
The object of the present invention is to provide a kind of nontoxic, purity is high, extraction yield is high chrysanthemum essential oil extracting process, the method adopts supercritical carbon dioxide extraction.
It is raw material that the chrysanthemum that is dried, pulverizes is take in the present invention, and with supercritical co, take dehydrated alcohol is the crude product dope of entrainment agent extraction chrysanthemum essential oil, then by dope carry out freezing, filter, concentratedly obtain highly purified chrysanthemum essential oil.Its concrete steps comprise:
A, by the fresh chrysanthemum of plucking, dry being less than at the temperature of 50 ℃-60 ℃;
B, the chrysanthemum of oven dry is pulverized, be controlled at 10-40 order;
C, the material after pulverizing pack supercritical extraction reactor into, from extraction kettle bottom, are pressed into the carbonic acid gas of carrying dehydrated alcohol secretly, at pressure, are 10-30Mpa, and temperature is under the supercritical state of 40-50 ℃, extraction 1-4 hour;
D, the CO 2 fluid with chrysanthemum essential oil flowing out from extraction kettle top enter extraction-container, at pressure 5-10Mpa, under the condition of temperature 30-40 ℃, resolve, and obtain essential oil dope;
The composition that e, essential oil dope low-grade fever obtain extraction fully dissolves, and then puts into freezing chamber, freezing 10-14 hour;
After f, taking-up, first use filter paper suction filtration, then filter with organic micro film, obtain filtered liquid;
G, filtered liquid are 40-70 ℃ in temperature, and underpressure distillation under the condition that vacuum tightness is 500-750mmHg, obtains pure chrysanthemum essential oil.
Further, in described step c, the 30%-50% that the amount of carbon dioxide of carrying dehydrated alcohol secretly is chrysanthemum.
Further, the essential oil dope low-grade fever in described step e is to put into the hot water preheating 3-5 minute of 30-50 ℃ after packing essential oil dope into container.
Further, in described step e, freezing chamber's temperature is controlled between-18 ℃ to-22 ℃.
Further, in described step f, the aperture of organic micro film is 0.45 μ m.
Described chrysanthemum is one or more mixtures in Hang Ju, emblem chrysanthemum, Chu chrysanthemum, Bo chrysanthemum, bosom chrysanthemum, Ji chrysanthemum and Huang Ju kind.
The present invention adopts supercritical carbon dioxide extraction chrysanthemum essential oil, and product extraction yield is high, and product purity is high, nontoxic simultaneously, and noresidue, just has look, and proterties is stable, the characteristics such as pure natural.Whole process flow is simple, easy to operate, and energy consumption generation, organic solvent-free is residual, has guaranteed the pure natural property of chrysanthemum essential oil; Carbonic acid gas reusable edible, free from environmental pollution, applicable to suitability for industrialized production.
Embodiment
Embodiment 1:
1,, by the fresh chrysanthemum of plucking, dry being less than at 60 ℃.
2, the chrysanthemum of oven dry is pulverized, be controlled at 20 orders.
3, the material after pulverizing takes 400g and packs supercritical extraction reactor into, is pressed into the high-pureness carbon dioxide of food grade from extraction kettle bottom, after half an hour, by carrying agent pump, adds dehydrated alcohol 200ml, at 30Mpa, under the supercritical state of 50 ℃, extracts 3 hours.
4, the carbonic acid gas with chrysanthemum essential oil flowing out from extraction kettle top, enters extraction-container, at 5.5Mpa, under the condition of 40 ℃, parses, and obtains chrysanthemum essential oil crude product dope 300ml.
5, essential oil dope is put into after container 50 ℃ of hot water low-grade fevers 4 minutes, and the composition that extraction is obtained fully dissolves, and then puts into freezing chamber, at-18 ℃ freezing 12 hours.
6, after taking-up, first use filter paper suction filtration, then filter with the organic micro film of 0.45 μ m.
7, filtered liquid is 50 ℃ in temperature, and underpressure distillation under the condition that vacuum tightness is 720mmHg obtains pure chrysanthemum essential oil 6.6g, and percentage extraction is 1.65%.
Embodiment 2:
1,, by the fresh chrysanthemum of plucking, dry being less than at 60 ℃.
2, the chrysanthemum of oven dry is pulverized, be controlled at 20 orders.
3, the material after pulverizing takes 400g and packs supercritical extraction reactor into, is pressed into the high-pureness carbon dioxide of food grade from extraction kettle bottom, after half an hour, by carrying agent pump, adds dehydrated alcohol 200ml, at 25Mpa, under the supercritical state of 50 ℃, extracts 3 hours.
4, the carbonic acid gas with chrysanthemum essential oil flowing out from extraction kettle top, enters extraction-container, at 5.5Mpa, under the condition of 40 ℃, parses, and obtains chrysanthemum essential oil crude product dope 200ml.
5, essential oil dope is put into after container 50 ℃ of hot water low-grade fevers 4 minutes, and the composition that extraction is obtained fully dissolves, and then puts into freezing chamber, at-18 ℃ freezing 12 hours.
6, after taking-up, first use filter paper suction filtration, then filter with the organic micro film of 0.45 μ m.
7, filtered liquid is 50 ℃ in temperature, and underpressure distillation under the condition that vacuum tightness is 720mmHg obtains pure chrysanthemum essential oil 5.6g, and percentage extraction is 1.4%.
Embodiment 3:
1,, by the fresh chrysanthemum of plucking, dry being less than at 60 ℃.
2, the chrysanthemum of oven dry is pulverized, be controlled at 20 orders.
3, the material after pulverizing takes 400g and packs supercritical extraction reactor into, is pressed into the high-pureness carbon dioxide of food grade from extraction kettle bottom, after half an hour, by carrying agent pump, adds dehydrated alcohol 200ml, at 20Mpa, under the supercritical state of 50 ℃, extracts 3 hours.
4, the carbonic acid gas with chrysanthemum essential oil flowing out from extraction kettle top, enters extraction-container, at 5.5Mpa, under the condition of 40 ℃, parses, and obtains chrysanthemum essential oil crude product dope 200ml.
5, essential oil dope is put into after container 50 ℃ of hot water low-grade fevers 4 minutes, and the composition that extraction is obtained fully dissolves, and then puts into freezing chamber, at-18 ℃ freezing 12 hours.
6, after taking-up, first use filter paper suction filtration, then filter with the organic micro film of 0.45 μ m.
7, filtered liquid is 50 ℃ in temperature, and underpressure distillation under the condition that vacuum tightness is 720mmHg obtains pure chrysanthemum essential oil 3.0g, and percentage extraction is 0.75%.
Embodiment 4:
1,, by the fresh chrysanthemum of plucking, dry being less than at 60 ℃.
2, the chrysanthemum of oven dry is pulverized, be controlled at 20 orders.
3, the material after pulverizing takes 400g and packs supercritical extraction reactor into, is pressed into the high-pureness carbon dioxide of food grade from extraction kettle bottom, after half an hour, by carrying agent pump, adds dehydrated alcohol 200ml, at 15Mpa, under the supercritical state of 50 ℃, extracts 3 hours.
4, the carbonic acid gas with chrysanthemum essential oil flowing out from extraction kettle top, enters extraction-container, at 5.5Mpa, under the condition of 40 ℃, parses, and obtains chrysanthemum essential oil crude product dope 200ml.
5, essential oil dope is put into after container 50 ℃ of hot water low-grade fevers 4 minutes, and the composition that extraction is obtained fully dissolves, and then puts into freezing chamber, at-18 ℃ freezing 12 hours.
6, after taking-up, first use filter paper suction filtration, then filter with the organic micro film of 0.45 μ m.
7, filtered liquid is 50 ℃ in temperature, and underpressure distillation under the condition that vacuum tightness is 720mmHg obtains pure chrysanthemum essential oil 2.8g, and percentage extraction is 0.7%.
Embodiment 5:
1, by the fresh chrysanthemum of plucking, at 60 ℃, dry.
2, the chrysanthemum of oven dry is pulverized, be controlled at 40 orders.
3, the material after pulverizing takes 400g and packs supercritical extraction reactor into, is pressed into the high-pureness carbon dioxide of food grade from extraction kettle bottom, after half an hour, by carrying agent pump, adds dehydrated alcohol 200ml, at 30Mpa, under the supercritical state of 50 ℃, extracts 3 hours.
4, the carbonic acid gas with chrysanthemum essential oil flowing out from extraction kettle top, enters extraction-container, at 5.5Mpa, under the condition of 40 ℃, parses, and obtains chrysanthemum essential oil crude product dope 300ml.
5, essential oil dope is put into after container 50 ℃ of hot water low-grade fevers 5 minutes, and the composition that extraction is obtained fully dissolves, and then puts into freezing chamber, at-18 ℃ freezing 12 hours.
6, after taking-up, first use filter paper suction filtration, then filter with the organic micro film of 0.45 μ m.
7, filtered liquid is 50 ℃ in temperature, and underpressure distillation under the condition that vacuum tightness is 600mmHg obtains pure chrysanthemum essential oil 3.3g, and percentage extraction is 0.82%.
Embodiment 6:
1, by the fresh chrysanthemum of plucking, at 50 ℃, dry.
2, the chrysanthemum of oven dry is pulverized, be controlled at 30 orders.
3, the material after pulverizing takes 400g and packs supercritical extraction reactor into, is pressed into the high-pureness carbon dioxide of food grade from extraction kettle bottom, after half an hour, by carrying agent pump, adds dehydrated alcohol 200ml, at 25Mpa, under the supercritical state of 50 ℃, extracts 3 hours.
4, the carbonic acid gas with chrysanthemum essential oil flowing out from extraction kettle top, enters extraction-container, at 8Mpa, under the condition of 35 ℃, parses, and obtains chrysanthemum essential oil crude product dope 200ml.
5, essential oil dope is put into after container 50 ℃ of hot water low-grade fevers 4 minutes, and the composition that extraction is obtained fully dissolves, and then puts into freezing chamber, at-17 ℃ freezing 12 hours.
6, after taking-up, first use filter paper suction filtration, then filter with the organic micro film of 0.45 μ m.
7, filtered liquid is 50 ℃ in temperature, and underpressure distillation under the condition that vacuum tightness is 720mmHg obtains pure chrysanthemum essential oil 4.2g, and percentage extraction is 1%.
Embodiment 7:
1, by the fresh chrysanthemum of plucking, at 54 ℃, dry.
2, the chrysanthemum of oven dry is pulverized, be controlled at 30 orders.
3, the material after pulverizing takes 400g and packs supercritical extraction reactor into, is pressed into the high-pureness carbon dioxide of food grade from extraction kettle bottom, after half an hour, by carrying agent pump, adds dehydrated alcohol 200ml, at 25Mpa, under the supercritical state of 46 ℃, extracts 3 hours.
4, the carbonic acid gas with chrysanthemum essential oil flowing out from extraction kettle top, enters extraction-container, at 6Mpa, under the condition of 40 ℃, parses, and obtains chrysanthemum essential oil crude product dope 200ml.
5, essential oil dope is put into after container 40 ℃ of hot water low-grade fevers 4 minutes, and the composition that extraction is obtained fully dissolves, and then puts into freezing chamber, at-16 ℃ freezing 12 hours.
6, after taking-up, first use filter paper suction filtration, then filter with the organic micro film of 0.45 μ m.
7, filtered liquid is 70 ℃ in temperature, and underpressure distillation under the condition that vacuum tightness is 750mmHg obtains pure chrysanthemum essential oil 5.1g, and percentage extraction is 1.2%.
Embodiment 8:
1,, by the fresh chrysanthemum of plucking, dry being less than at 60 ℃.
2, the chrysanthemum of oven dry is pulverized, be controlled at 10 orders.
3, the material after pulverizing takes 400g and packs supercritical extraction reactor into, is pressed into the high-pureness carbon dioxide of food grade from extraction kettle bottom, after half an hour, by carrying agent pump, adds dehydrated alcohol 200ml, at 12Mpa, under the supercritical state of 41 ℃, extracts 3 hours.
4, the carbonic acid gas with chrysanthemum essential oil flowing out from extraction kettle top, enters extraction-container, at 10Mpa, under the condition of 40 ℃, parses, and obtains chrysanthemum essential oil crude product dope 200ml.
5, essential oil dope is put into after container 50 ℃ of hot water low-grade fevers 3 minutes, and the composition that extraction is obtained fully dissolves, and then puts into freezing chamber, at-22 ℃ freezing 12 hours.
6, after taking-up, first use filter paper suction filtration, then filter with the organic micro film of 0.45 μ m.
7, filtered liquid is 40 ℃ in temperature, and underpressure distillation under the condition that vacuum tightness is 500mmHg obtains pure chrysanthemum essential oil 3.9g, and percentage extraction is 0.97%.
Although above the specific embodiment of the present invention has been given to describe in detail and explanation; but what should indicate is; we can carry out various equivalences to above-mentioned embodiment according to conception of the present invention and change and revise; when its function producing does not exceed spiritual that specification sheets contains yet, all should be within protection scope of the present invention.
Claims (6)
1. by a method for supercritical carbon dioxide extraction chrysanthemum essential oil, it is characterized in that preparation method's step is as follows:
A, by the fresh chrysanthemum of plucking, dry being less than at the temperature of 50 ℃-60 ℃;
B, the chrysanthemum of oven dry is pulverized, be controlled at 10-40 order;
C, the material after pulverizing pack supercritical extraction reactor into, from extraction kettle bottom, are pressed into the carbonic acid gas of carrying dehydrated alcohol secretly, at pressure, are 10-30Mpa, and temperature is under the supercritical state of 40-50 ℃, extraction 1-4 hour;
D, the CO 2 fluid with chrysanthemum essential oil flowing out from extraction kettle top enter extraction-container, at pressure 5-10Mpa, under the condition of temperature 30-40 ℃, resolve, and obtain essential oil dope;
The composition that e, essential oil dope low-grade fever obtain extraction fully dissolves, and then puts into freezing chamber, freezing 10-14 hour;
After f, taking-up, first use filter paper suction filtration, then filter with organic micro film, obtain filtered liquid;
G, filtered liquid are 40-70 ℃ in temperature, and underpressure distillation under the condition that vacuum tightness is 500-750mmHg, obtains pure chrysanthemum essential oil.
2. the method with supercritical carbon dioxide extraction chrysanthemum essential oil according to claim 1, is characterized in that: in described step c, and the 30%-50% that the amount of carbon dioxide of carrying dehydrated alcohol secretly is chrysanthemum.
3. according to right, ask the method with supercritical carbon dioxide extraction chrysanthemum essential oil described in 1, it is characterized in that the essential oil dope low-grade fever in described step e is to put into the hot water preheating 3-5 minute of 30-50 ℃ after packing essential oil dope into container.
4. the method with supercritical carbon dioxide extraction chrysanthemum essential oil according to claim 1, is characterized in that: in described step e, freezing chamber's temperature is controlled between-18 ℃ to-22 ℃.
5. the method with supercritical carbon dioxide extraction chrysanthemum essential oil according to claim 1, is characterized in that: in described step f, the aperture of organic micro film is 0.45 μ m.
6. the method with supercritical carbon dioxide extraction chrysanthemum essential oil according to claim 1, is characterized in that: the chrysanthemum in described step a is one or more mixtures in Hang Ju, emblem chrysanthemum, Chu chrysanthemum, Bo chrysanthemum, bosom chrysanthemum, Ji chrysanthemum and Huang Ju kind.
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| CN104450195A (en) * | 2014-11-18 | 2015-03-25 | 深圳市深宝华城科技有限公司 | Preparation method of solid chrysanthemum perfume |
| CN104498192A (en) * | 2014-12-15 | 2015-04-08 | 云南中烟工业有限责任公司 | Preparation method and application of florists chrysanthemum extract |
| CN104560401A (en) * | 2014-12-26 | 2015-04-29 | 高俊丽 | Extraction method of calendula volatile oil |
| CN104840398A (en) * | 2015-05-18 | 2015-08-19 | 陈丽丹 | Natural moringa oleifera health essential oil |
| CN105062680A (en) * | 2015-08-12 | 2015-11-18 | 滁州市滁菊研究所 | Chuzhou chrysanthemum essential oil extracting method |
| CN105132183A (en) * | 2015-08-26 | 2015-12-09 | 谢晓亮 | Fresh chrysanthemum aromatic water and preparation method thereof |
| CN105754723A (en) * | 2016-05-28 | 2016-07-13 | 黄宇松 | Method for extracting chrysanthemum essential oil |
| CN106281702A (en) * | 2016-08-25 | 2017-01-04 | 苏州森佰生物科技有限公司 | Artemisia argyi Levl. et Van. var. argyi cv. Qiai quintessence oil and its preparation method and application |
| CN106723032A (en) * | 2016-12-15 | 2017-05-31 | 岑溪市安安农业科技发展有限公司 | The preparation method of dragon fruit stem end essential oil |
| CN107281464A (en) * | 2017-07-05 | 2017-10-24 | 广州中医药大学 | A kind of pharmaceutical composition for treating tumour |
| CN107841381A (en) * | 2017-11-30 | 2018-03-27 | 安徽心缘康生物科技有限公司 | A kind of extracting method of peony essential oil |
| CN108018117A (en) * | 2017-12-25 | 2018-05-11 | 湖南宇山玉月农业科技有限公司 | A kind of extracting method of styrax essential oil |
| CN114231360A (en) * | 2021-12-29 | 2022-03-25 | 浙江康莱特药业有限公司 | Extraction method of hinoki essential oil |
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| CN104450195A (en) * | 2014-11-18 | 2015-03-25 | 深圳市深宝华城科技有限公司 | Preparation method of solid chrysanthemum perfume |
| CN104498192A (en) * | 2014-12-15 | 2015-04-08 | 云南中烟工业有限责任公司 | Preparation method and application of florists chrysanthemum extract |
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| CN105132183A (en) * | 2015-08-26 | 2015-12-09 | 谢晓亮 | Fresh chrysanthemum aromatic water and preparation method thereof |
| CN105754723A (en) * | 2016-05-28 | 2016-07-13 | 黄宇松 | Method for extracting chrysanthemum essential oil |
| CN106281702A (en) * | 2016-08-25 | 2017-01-04 | 苏州森佰生物科技有限公司 | Artemisia argyi Levl. et Van. var. argyi cv. Qiai quintessence oil and its preparation method and application |
| CN106723032A (en) * | 2016-12-15 | 2017-05-31 | 岑溪市安安农业科技发展有限公司 | The preparation method of dragon fruit stem end essential oil |
| CN107281464A (en) * | 2017-07-05 | 2017-10-24 | 广州中医药大学 | A kind of pharmaceutical composition for treating tumour |
| CN107841381A (en) * | 2017-11-30 | 2018-03-27 | 安徽心缘康生物科技有限公司 | A kind of extracting method of peony essential oil |
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