CN103710152B - A kind of method of supercritical carbon dioxide extraction chrysanthemum essential oil - Google Patents
A kind of method of supercritical carbon dioxide extraction chrysanthemum essential oil Download PDFInfo
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- CN103710152B CN103710152B CN201310512626.6A CN201310512626A CN103710152B CN 103710152 B CN103710152 B CN 103710152B CN 201310512626 A CN201310512626 A CN 201310512626A CN 103710152 B CN103710152 B CN 103710152B
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Abstract
The invention discloses a kind of method of supercritical carbon dioxide extraction chrysanthemum essential oil, the present invention with chrysanthemum that is dry, that pulverize for raw material, with the crude product dope that supercritical co take dehydrated alcohol as entrainment agent extraction chrysanthemum essential oil, then dope is carried out freezing, filter, concentratedly obtain highly purified chrysanthemum essential oil.Product extraction yield of the present invention is high, and product purity is high, nontoxic, noresidue; Product just has look, and proterties is stablized, the characteristics such as pure natural; Technique is simple, and energy consumption is low.
Description
Technical field
The present invention relates to a kind of vegetable oil extraction method, be specifically related to a kind of method of supercritical carbon dioxide extraction chrysanthemum essential oil.
Background technology
Chrysanthemum is feverfew, is Chinese conventional Chinese medicine, has effect of dispelling wind, heat-clearing, improving eyesight, removing toxic substances.The disease 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, anti-ageing multiple pharmacologically active of waiting for a long time.China's Chrysanthemum morifolium commercially has eight large main flow merchandise resourceses, be respectively Hang Ju, Bo chrysanthemum, tribute chrysanthemum, Chu chrysanthemum, Qi Ju, bosom chrysanthemum, Ji chrysanthemum, Huang Ju, and " Chinese Pharmacopoeia " I (version in 2000) is according to the difference of the chrysanthemum place of production and working method, has recorded Bo chrysanthemum, Chu chrysanthemum, tribute chrysanthemum and Hang Ju four strains.Chrysanthemum is medicinal and edible plant, all has report both at home and abroad to aspects such as its classification, qualification, chemical, clinical, pharmacology.
The chemical composition more complicated of chrysanthemum, wherein flavonoid compound, triterpene compound and volatile oil are its principle active component.Volatile oil--to Different sources four kinds of chrysanthemums: namely 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 low-polarity components to carry out preliminary study to volatile oil component simultaneously, identify more than 20 and plant ter penoids.Application low-polarity components is to Huai Chrysanthemi and the large chemical composition of volatile oil cherishing 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 Huai Chrysanthemi volatile oil, identify 40 compounds, from the chrysanthemum of large bosom, identify 27 compounds.Also adopt low-polarity components, chemical composition of volatile oil in Hang Ju is analyzed, identify 50 compounds, and determine the percentage contents of each composition.
Chrysanthemum has wind-dispelling heat-dissipating, detoxify and promote the subsdence of swelling, relieve sore throat improving eyesight, the effect that reduces blood pressure.Research shows, chrysanthemum essential oil can strengthen capillary resistance, reduces metabolism of lipid and cholesterol content in blood, has the effect improving myocardial nutrition, anti-inflammatory, scavenging capacity oxyradical; To Tumor suppression, delaying senility and strengthening body immunity has certain effect.
Extracting method mainly water extraction and the ultrasonic-assisted extraction of current chrysanthemum essential oil, this extracting method energy consumption is large, and needs to use the reagent such as normal hexane, sodium sulfate, ethanol, and easily cause reagent to remain, 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.
The present invention for raw material, is the crude product dope of entrainment agent extraction chrysanthemum essential oil with chrysanthemum that is dry, that pulverize with dehydrated alcohol with supercritical co, then dope is carried out freezing, filter, concentratedly obtain highly purified chrysanthemum essential oil.Its concrete steps comprise:
A, the fresh chrysanthemum of will pluck, dry at the temperature of 50 DEG C-60 DEG C;
B, the chrysanthemum of oven dry to be pulverized, control at 20-30 order;
Material after c, pulverizing loads supercritical extraction reactor, and bottom extraction kettle, the carbonic acid gas of dehydrated alcohol is carried in press-in secretly, and be 25-30Mpa at pressure, temperature is under the supercritical state of 40-50 DEG C, extraction 1-4 hour;
D, the CO 2 fluid with chrysanthemum essential oil flowed out from extraction kettle top enter extraction-container, resolve, obtain essential oil dope under the condition of pressure 5-10Mpa, temperature 30-40 DEG C;
E, essential oil dope put into the hot water preheating 3-5 minute of 30-50 DEG C after loading container, the composition that extraction is obtained fully dissolves, and then puts into freezing chamber, freezing 10-14 hour;
First use filter paper suction filtration after f, taking-up, then filter with organic micro film, obtain filtered liquid;
G, filtered liquid are 40-70 DEG C in temperature, and vacuum tightness is underpressure distillation under the condition of 500-750mmHg, obtains pure chrysanthemum essential oil.
Further, in described step c, the amount of carbon dioxide of carrying dehydrated alcohol secretly is the 30%-50% of chrysanthemum.
Further, in described step e, freezing chamber's temperature controls between-18 DEG C to-22 DEG C.
Further, in described step f, the aperture of organic micro film is 0.45 μm.
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 stablized, the characteristics such as pure natural.
Whole process flow is simple, and easy to operate, in energy consumption generation, organic solvent-free remains, and ensure that the pure natural property of chrysanthemum essential oil; Carbonic acid gas reusable edible, free from environmental pollution, be applicable to suitability for industrialized production.
Embodiment
Embodiment 1:
1, the fresh chrysanthemum will plucked, dries being less than at 60 DEG C.
2, the chrysanthemum of oven dry is pulverized, control at 20 orders.
3, the material after pulverizing takes 400g and loads supercritical extraction reactor, being pressed into the high-pureness carbon dioxide of food grade, adding dehydrated alcohol 200ml after half an hour by carrying agent pump, at 30Mpa, under the supercritical state of 50 DEG C, extract 3 hours bottom extraction kettle.
4, the carbonic acid gas with chrysanthemum essential oil flowed out from extraction kettle top, enters extraction-container, at 5.5Mpa, parses under the condition of 40 DEG C, obtain chrysanthemum essential oil crude product dope 300ml.
5, essential oil dope is put into 50 DEG C of hot water low-grade fevers 4 minutes after container, and the composition that extraction is obtained fully dissolves, and then puts into freezing chamber, at-18 DEG C freezing 12 hours.
6, first use filter paper suction filtration after taking out, then filter with the organic micro film of 0.45 μm.
7, filtered liquid is 50 DEG C in temperature, and vacuum tightness is underpressure distillation under the condition of 720mmHg, obtains pure chrysanthemum essential oil 6.6g, and percentage extraction is 1.65%.
Embodiment 2:
1, the fresh chrysanthemum will plucked, dries being less than at 60 DEG C.
2, the chrysanthemum of oven dry is pulverized, control at 20 orders.
3, the material after pulverizing takes 400g and loads supercritical extraction reactor, being pressed into the high-pureness carbon dioxide of food grade, adding dehydrated alcohol 200ml after half an hour by carrying agent pump, at 25Mpa, under the supercritical state of 50 DEG C, extract 3 hours bottom extraction kettle.
4, the carbonic acid gas with chrysanthemum essential oil flowed out from extraction kettle top, enters extraction-container, at 5.5Mpa, parses under the condition of 40 DEG C, obtain chrysanthemum essential oil crude product dope 200ml.
5, essential oil dope is put into 50 DEG C of hot water low-grade fevers 4 minutes after container, and the composition that extraction is obtained fully dissolves, and then puts into freezing chamber, at-18 DEG C freezing 12 hours.
6, first use filter paper suction filtration after taking out, then filter with the organic micro film of 0.45 μm.
7, filtered liquid is 50 DEG C in temperature, and vacuum tightness is underpressure distillation under the condition of 720mmHg, obtains pure chrysanthemum essential oil 5.6g, and percentage extraction is 1.4%.
Embodiment 3:
1, the fresh chrysanthemum will plucked, dries being less than at 60 DEG C.
2, the chrysanthemum of oven dry is pulverized, control at 20 orders.
3, the material after pulverizing takes 400g and loads supercritical extraction reactor, being pressed into the high-pureness carbon dioxide of food grade, adding dehydrated alcohol 200ml after half an hour by carrying agent pump, at 20Mpa, under the supercritical state of 50 DEG C, extract 3 hours bottom extraction kettle.
4, the carbonic acid gas with chrysanthemum essential oil flowed out from extraction kettle top, enters extraction-container, at 5.5Mpa, parses under the condition of 40 DEG C, obtain chrysanthemum essential oil crude product dope 200ml.
5, essential oil dope is put into 50 DEG C of hot water low-grade fevers 4 minutes after container, and the composition that extraction is obtained fully dissolves, and then puts into freezing chamber, at-18 DEG C freezing 12 hours.
6, first use filter paper suction filtration after taking out, then filter with the organic micro film of 0.45 μm.
7, filtered liquid is 50 DEG C in temperature, and vacuum tightness is underpressure distillation under the condition of 720mmHg, obtains pure chrysanthemum essential oil 3.0g, and percentage extraction is 0.75%.
Embodiment 4:
1, the fresh chrysanthemum will plucked, dries being less than at 60 DEG C.
2, the chrysanthemum of oven dry is pulverized, control at 20 orders.
3, the material after pulverizing takes 400g and loads supercritical extraction reactor, being pressed into the high-pureness carbon dioxide of food grade, adding dehydrated alcohol 200ml after half an hour by carrying agent pump, at 15Mpa, under the supercritical state of 50 DEG C, extract 3 hours bottom extraction kettle.
4, the carbonic acid gas with chrysanthemum essential oil flowed out from extraction kettle top, enters extraction-container, at 5.5Mpa, parses under the condition of 40 DEG C, obtain chrysanthemum essential oil crude product dope 200ml.
5, essential oil dope is put into 50 DEG C of hot water low-grade fevers 4 minutes after container, and the composition that extraction is obtained fully dissolves, and then puts into freezing chamber, at-18 DEG C freezing 12 hours.
6, first use filter paper suction filtration after taking out, then filter with the organic micro film of 0.45 μm.
7, filtered liquid is 50 DEG C in temperature, and vacuum tightness is underpressure distillation under the condition of 720mmHg, obtains pure chrysanthemum essential oil 2.8g, and percentage extraction is 0.7%.
Embodiment 5:
The fresh chrysanthemum of 1, will pluck, dries at 60 DEG C.
2, the chrysanthemum of oven dry is pulverized, control at 40 orders.
3, the material after pulverizing takes 400g and loads supercritical extraction reactor, being pressed into the high-pureness carbon dioxide of food grade, adding dehydrated alcohol 200ml after half an hour by carrying agent pump, at 30Mpa, under the supercritical state of 50 DEG C, extract 3 hours bottom extraction kettle.
4, the carbonic acid gas with chrysanthemum essential oil flowed out from extraction kettle top, enters extraction-container, at 5.5Mpa, parses under the condition of 40 DEG C, obtain chrysanthemum essential oil crude product dope 300ml.
5, essential oil dope is put into 50 DEG C of hot water low-grade fevers 5 minutes after container, and the composition that extraction is obtained fully dissolves, and then puts into freezing chamber, at-18 DEG C freezing 12 hours.
6, first use filter paper suction filtration after taking out, then filter with the organic micro film of 0.45 μm.
7, filtered liquid is 50 DEG C in temperature, and vacuum tightness is underpressure distillation under the condition of 600mmHg, obtains pure chrysanthemum essential oil 3.3g, and percentage extraction is 0.82%.
Embodiment 6:
The fresh chrysanthemum of 1, will pluck, dries at 50 DEG C.
2, the chrysanthemum of oven dry is pulverized, control at 30 orders.
3, the material after pulverizing takes 400g and loads supercritical extraction reactor, being pressed into the high-pureness carbon dioxide of food grade, adding dehydrated alcohol 200ml after half an hour by carrying agent pump, at 25Mpa, under the supercritical state of 50 DEG C, extract 3 hours bottom extraction kettle.
4, the carbonic acid gas with chrysanthemum essential oil flowed out from extraction kettle top, enters extraction-container, at 8Mpa, parses under the condition of 35 DEG C, obtain chrysanthemum essential oil crude product dope 200ml.
5, essential oil dope is put into 50 DEG C of hot water low-grade fevers 4 minutes after container, and the composition that extraction is obtained fully dissolves, and then puts into freezing chamber, at-17 DEG C freezing 12 hours.
6, first use filter paper suction filtration after taking out, then filter with the organic micro film of 0.45 μm.
7, filtered liquid is 50 DEG C in temperature, and vacuum tightness is underpressure distillation under the condition of 720mmHg, obtains pure chrysanthemum essential oil 4.2g, and percentage extraction is 1%.
Embodiment 7:
The fresh chrysanthemum of 1, will pluck, dries at 54 DEG C.
2, the chrysanthemum of oven dry is pulverized, control at 30 orders.
3, the material after pulverizing takes 400g and loads supercritical extraction reactor, being pressed into the high-pureness carbon dioxide of food grade, adding dehydrated alcohol 200ml after half an hour by carrying agent pump, at 25Mpa, under the supercritical state of 46 DEG C, extract 3 hours bottom extraction kettle.
4, the carbonic acid gas with chrysanthemum essential oil flowed out from extraction kettle top, enters extraction-container, at 6Mpa, parses under the condition of 40 DEG C, obtain chrysanthemum essential oil crude product dope 200ml.
5, essential oil dope is put into 40 DEG C of hot water low-grade fevers 4 minutes after container, and the composition that extraction is obtained fully dissolves, and then puts into freezing chamber, at-16 DEG C freezing 12 hours.
6, first use filter paper suction filtration after taking out, then filter with the organic micro film of 0.45 μm.
7, filtered liquid is 70 DEG C in temperature, and vacuum tightness is underpressure distillation under the condition of 750mmHg, obtains pure chrysanthemum essential oil 5.1g, and percentage extraction is 1.2%.
Embodiment 8:
1, the fresh chrysanthemum will plucked, dries being less than at 60 DEG C.
2, the chrysanthemum of oven dry is pulverized, control at 10 orders.
3, the material after pulverizing takes 400g and loads supercritical extraction reactor, being pressed into the high-pureness carbon dioxide of food grade, adding dehydrated alcohol 200ml after half an hour by carrying agent pump, at 12Mpa, under the supercritical state of 41 DEG C, extract 3 hours bottom extraction kettle.
4, the carbonic acid gas with chrysanthemum essential oil flowed out from extraction kettle top, enters extraction-container, at 10Mpa, parses under the condition of 40 DEG C, obtain chrysanthemum essential oil crude product dope 200ml.
5, essential oil dope is put into 50 DEG C of hot water low-grade fevers 3 minutes after container, and the composition that extraction is obtained fully dissolves, and then puts into freezing chamber, at-22 DEG C freezing 12 hours.
6, first use filter paper suction filtration after taking out, then filter with the organic micro film of 0.45 μm.
7, filtered liquid is 40 DEG C in temperature, and vacuum tightness is underpressure distillation under the condition of 500mmHg, obtains pure chrysanthemum essential oil 3.9g, and percentage extraction is 0.97%.
Although give detailed description and explanation to the specific embodiment of the present invention above; but what should indicate is; we can carry out various equivalence according to conception of the present invention to above-mentioned embodiment and change and amendment; its function produced do not exceed that specification sheets contains yet spiritual time, all should within protection scope of the present invention.
Claims (4)
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, the fresh chrysanthemum of will pluck, dry at the temperature of 50-60 DEG C;
B, the chrysanthemum of oven dry to be pulverized, control at 20-30 order;
Material after c, pulverizing loads supercritical extraction reactor, and bottom extraction kettle, the carbonic acid gas of dehydrated alcohol is carried in press-in secretly, and be 25-30Mpa at pressure, temperature is under the supercritical state of 40-50 DEG C, extraction 1-4 hour;
D, the CO 2 fluid with chrysanthemum essential oil flowed out from extraction kettle top enter extraction-container, resolve, obtain essential oil dope under the condition of pressure 5-10Mpa, temperature 30-40 DEG C;
E, essential oil dope put into the hot water preheating 3-5 minute of 30-50 DEG C after loading container, the composition that extraction is obtained fully dissolves, and then puts into freezing chamber, freezing 10-14 hour;
First use filter paper suction filtration after f, taking-up, then filter with organic micro film, obtain filtered liquid;
G, filtered liquid are 40-70 DEG C in temperature, and vacuum tightness is underpressure distillation under the condition of 500-750mmHg, obtains pure chrysanthemum essential oil.
2. the method for supercritical carbon dioxide extraction chrysanthemum essential oil according to claim 1, is characterized in that: in described step e, freezing chamber's temperature controls between-18 DEG C to-22 DEG C.
3. the method for 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 μm.
4. the method for 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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