CN109363969A - A kind of method of comprehensive utilization of wormwood effective component - Google Patents
A kind of method of comprehensive utilization of wormwood effective component Download PDFInfo
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Abstract
The present invention relates to plant resources technical field of comprehensive utilization more particularly to a kind of method of comprehensive utilization of wormwood effective component.The following steps are included: S0, folium artemisiae argyi, Chinese mugwort root preparation: wormwood is divided into folium artemisiae argyi and Ai Gen；S1, the preparation of folium artemisiae argyi raw material；S2, P-Cymene extract；S3, the purification of P-Cymene medicinal extract: the P-Cymene medicinal extract is further refined through molecular distillation, P-Cymene heavy oil and folium artemisiae argyi wax are obtained；S4, artemisia leaf total chromocor and Thick many candies extract；S5, the thick general flavone of folium artemisiae argyi, Thick many candies extracting solution are concentrated, separates, refine, obtaining artemisia leaf total chromocor and Thick many candies.The process route for the comprehensive utilization wormwood resource that the present invention develops can utmostly obtain the series of products such as main active essential oil in wormwood, general flavone, polysaccharide, Chinese mugwort root hydrosol, the utilization added value of significant increase wormwood resource.
Description
Technical field
The present invention relates to plant resources technical field of comprehensive utilization more particularly to a kind of comprehensive utilizations of wormwood effective component
Method.
Background technique
Wormwood comprehensive utilization can be divided into folium artemisiae argyi and Ai Gen two parts.Folium artemisiae argyi makes as a kind of Chinese traditional herbs in China extensively
With studying more folium artemisiae argyi main active at present is essential oil, flavones, polysaccharide.There is P-Cymene warming channel for arresting bleeding, cold dispelling to stop
Bitterly, miscarriage prevention, antibacterial, analgesia, calmness, it is antipyretic the effects of；Folium artemisiae argyi flavones, which has, eliminates oxygen radical, anti-oxidant, antitumor, disease-resistant
Poison, adjusts the effects of blood lipid at anti-inflammation and sterilization；Argyi leaf polysaccharide is a kind of immunomodulator, has the function such as very strong anti-tumor activity
Effect.Ai Genke preparation Chinese mugwort root hydrosol, document report is less, and Chinese mugwort root hydrosol can be used for the exploitation of armaticity cosmetic product.
P-Cymene, general flavone, polysaccharide belong to heat-sensitive substance, and for this feature, supercritical carbon dioxide fluid extraction can be
Under lower temperature P-Cymene, general flavone, polysaccharide are extracted, reduction high temperature is to P-Cymene, general flavone, polysaccharide as far as possible
Extent of the destruction.More with the research report of SCF-CO 2 P-Cymene at present, Chinese patent CN105412192A is reported
A kind of preparation method of volatile argyi leaf oil obtains volatile argyi leaf oil crude product using SCF-CO 2, then uses solvent dewaxing,
Entire technique, which does not refine P-Cymene, to be segmented；Chinese patent CN105395593A reports the preparation side of volatile argyi leaf oil
Method, extracting pressure are 15 ~ 20MPa, and extraction temperature is 30 ~ 35 DEG C, and extraction time is 1.5 ~ 2h, and decompression separation is made folium artemisiae argyi and waves
Hair oil, while it being prepared for alcohol extract using raffinate residue, this method has only obtained the head product of P-Cymene and alcohol extract, product
Added value is promoted unobvious；Chinese patent CN105535261A has reported a kind of folium artemisiae argyi health care essential oil and preparation method thereof, is faced with super
Boundary CO2 abstraction technique prepares folium artemisiae argyi medicinal extract, and using folium artemisiae argyi medicinal extract as raw material, by molecular clock P-Cymene, this is super to face
Boundary's extraction process does not refine P-Cymene, and a kind of product of volatile argyi leaf oil is only obtained by molecular distillation.In addition, document
It is less to SCF-CO 2 artemisia leaf total chromocor, polysaccharide researches.
The present invention is directed to wormwood resource, proposes the processing mode of comprehensive utilization, with SCF-CO 2, supercritical CO 2 essence
Evaporate, molecular distillation, steam distillation, film concentration etc. techniques be core technology, it is extracted, separation, purifying, respectively obtain folium artemisiae argyi essence
The series of products such as oily light oil, heavy oil, folium artemisiae argyi wax, folium artemisiae argyi flavones, argyi leaf polysaccharide, Chinese mugwort root hydrosol, are opened for subsequent cosmetics etc.
Hair utilizes, and promotes the added value of wormwood comprehensive utilization of resources.
Summary of the invention
The present invention in order to overcome at least one of the drawbacks of the prior art described above (deficiency), provides a kind of wormwood effective component
Method of comprehensive utilization.
In order to solve the above technical problems, technical scheme is as follows:
A kind of method of comprehensive utilization of wormwood effective component, which comprises the following steps: S0, folium artemisiae argyi, Chinese mugwort root preparation:
Wormwood is divided into folium artemisiae argyi and Ai Gen；S1, the preparation of folium artemisiae argyi raw material: folium artemisiae argyi is dried in the shade to water content≤8%, smashes to 20 ~ 100 mesh, obtains
Folium artemisiae argyi coarse powder；S2, P-Cymene extract: by the folium artemisiae argyi coarse powder using supercritical CO 2 extraction device extraction, supercritical CO 2 essence
Fractional distillation column separation, separating still isolate and purify to obtain P-Cymene light oil, P-Cymene heavy oil and medicinal extract, and obtain folium artemisiae argyi grouts；S3,
The purification of P-Cymene medicinal extract: the P-Cymene medicinal extract is further refined through molecular distillation, P-Cymene heavy oil and Chinese mugwort are obtained
Leaf wax；S4, artemisia leaf total chromocor and Thick many candies extract: supercritical CO 2 extraction device is added in the folium artemisiae argyi grouts, and folder is added
Band agent extraction artemisia leaf total chromocor and Thick many candies, 35 ~ 80 DEG C of extraction kettle temperature, extraction kettle 20 ~ 40MPa of pressure, extraction time 30 ~
180min, 20 ~ 35 DEG C of extraction-container temperature, 3 ~ 6MPa of extraction-container pressure, the entrainer is the ethyl alcohol that concentration is 20% ~ 95%, folder
Band 1 ~ 3mL/g of agent dosage, 10 ~ 30kg/h of gas flow, obtain the thick general flavone of folium artemisiae argyi, Thick many candies extracting solution；S5, total Huang thick to folium artemisiae argyi
Ketone, Thick many candies extracting solution are concentrated, are separated, are refined, and artemisia leaf total chromocor and Thick many candies are obtained.
Further, the thick general flavone of folium artemisiae argyi, the concentration of Thick many candies extracting solution, separation, the specific packet of purification in the step S5
It includes following steps: S51, depressurizing the thick general flavone of the folium artemisiae argyi, Thick many candies extracting solution in 30 ~ 60 DEG C of temperature in concentration tank
Be concentrated into original volume 1/5 ~ 1/2 obtains concentrate；S52, by the ethyl alcohol alcohol precipitation of concentrate concentration 80% ~ 100%, 4 DEG C
Overnight, alcohol precipitation filtrate and alcohol precipitation filter residue are filtered to obtain later；S53, the alcohol precipitation filtrate is concentrated under reduced pressure at a temperature of 30 ~ 60 DEG C
Concentrated extract is obtained, obtains thick general flavone after concentrated extract is dry；S54, be 20% by the concentrated extract distilled water or concentration ~
95% ethyl alcohol dissolved dilution obtains sample solution, adsorbs through macroporous absorbent resin, then with 3 ~ 4 times of column volume distilled water, concentration be 60% ~
Macroreticular resin after 80% ethanol elution absorption, collects ethanol eluate, true under the conditions of 60 DEG C of temperature after eluent is concentrated
Empty dry smart general flavone；S55, it is centrifugated the alcohol precipitation filter residue to obtain precipitating, precipitating obtains Thick many candies after drying；S56, general
The precipitating is successively with 2 ~ 4 times of volumes, and the ethyl alcohol of concentration 80%, 90%, 95%, 100% carries out classification alcohol precipitation, often inferior to 4 DEG C of alcohol
Heavy 4h, is centrifuged off supernatant later, must precipitate through dry primary essence polysaccharide.
Further, in step S52, macroporous absorbent resin S-8, D-101, XDA-1, AB-8, LSA-20, NKA-9,
One of NKA- II or a variety of, sample solution concentration be 0.2 ~ 0.5 mg/mL, loading 1 ~ 2BV/h of speed, sample solution pH value 4 ~
6, applied sample amount is 0.5g crude product/100g macroporous absorbent resin, elution flow rate about 1 ~ 3BV/h.
Further, in the step S2, the process conditions of SCF-CO 2 be extraction kettle inlet pressure be 20 ~
28MPa, outlet pressure are 19 ~ 26MPa, and extraction temperature is 35 ~ 60 DEG C；The process conditions of Supercritical CO2 rectification separation are rectifying
Column 18 ~ 26MPa of inlet pressure, rectifying column outlet pressure be 8 ~ 25MPa, 15 ~ 65 DEG C of temperature；Separating still process conditions be 5 ~
25MPa, 15 ~ 75 DEG C of temperature；The small P-Cymene medicinal extract of solubility is precipitated from rectifying column bottom, wherein containing P-Cymene wax
Matter, P-Cymene heavy oil composition；The big P-Cymene light oil of solubility is flowed out from tower top, until separating in separating still.Wherein, folium artemisiae argyi
Light oil essentially consists in fragrant utilization, such as massage oil, fragrant atmosphere, perfume product；Folium artemisiae argyi heavy oil is mainly used in cream kind product, such as
Newborn class, white class etc.；Mainly shield series, such as soaps, hand crura membranacea film product are washed in application to folium artemisiae argyi wax.
Further, in the step S3, it is 65 ~ 85 DEG C that molecular distillation process conditions, which are evaporating surface temperature, charging speed
Degree is 100 ~ 150 ml/h, and condensate layer temperature is 35 ~ 50 DEG C, 0.1 ~ 0.5Pa of pressure, by the P-Cymene medicinal extract heating water bath
Sample introduction after being in a liquid state, what light component bottle was collected into is P-Cymene heavy oil, and what recombination sub-bottle was collected into is folium artemisiae argyi wax.
Further, the thick general flavone of folium artemisiae argyi and thick total starches obtain simultaneously through SCF-CO 2.
Further, the folium artemisiae argyi grouts in step S4 can be the folium artemisiae argyi grouts for just extracting P-Cymene, be also possible to
Folium artemisiae argyi grouts after extraction essential oil after drying.
Further, P-Cymene extract and the thick general flavone of folium artemisiae argyi, Thick many candies can continuous extraction, extraction can also be interrupted.
The present invention also provides a kind of method of comprehensive utilization of wormwood effective component, comprising the following steps: S0, folium artemisiae argyi, Ai Gen
Preparation: wormwood is divided into folium artemisiae argyi and Ai Gen；S1, Chinese mugwort root is cleaned, is cleaned, it is spare to be crushed to 20 ~ 100 mesh；S2, will end root raw material
It is put into steam distillation apparatus and carries out steam extraction, temperature is 80 DEG C ~ 95 DEG C when distillation, and distillation time is 2 ~ 4.5h；S3,
It is collected after the distillate being collected into is cooling in cooler, cooling temperature is 20 DEG C ~ 30 DEG C；S4, collection distillate obtain Chinese mugwort root
Hydrosol, through reverse osmosis concentration, the reverse osmosis trapped fluid of gained is the Chinese mugwort root hydrosol of concentration, the pressure of reverse osmosis membrane is 0.85~
2.5MPa。
Further, in step s 4, the desalination rate for the reverse osmosis membrane that reverse osmosis treatment uses is 98.0 ~ 99.6%, filter membrane
Aperture is 0.15 ~ 1.6 um.
Compared with prior art, the present invention passes through SCF-CO 2, supercritical CO 2 essence using wormwood resource as raw material
It evaporates, the process route of molecular distillation, realizes the preparation of P-Cymene light oil, heavy oil and folium artemisiae argyi wax；It is carried secretly using supercritical CO 2
Agent extraction-concentration-alcohol precipitation-macroporous resin adsorption separation/gradient alcohol precipitation process route prepares artemisia leaf total chromocor, total more
Sugar, smart general flavone, primary smart polysaccharide；Using steam distillation-film concentration process route, preparation Chinese mugwort root hydrosol.The present invention opens
The process route of the comprehensive utilization wormwood resource of hair can utmostly obtain main active essential oil in wormwood, general flavone, more
The series of products such as sugar, Chinese mugwort root hydrosol, the utilization added value of significant increase wormwood resource.
Detailed description of the invention
Fig. 1 is that wormwood effective component extracts frame diagram.
Specific embodiment
In order to facilitate the understanding of those skilled in the art, with reference to the accompanying drawings and examples to technical solution of the present invention do into
The explanation of one step.
Embodiment 1
Present embodiment discloses a kind of method of comprehensive utilization of wormwood effective component, comprising the following steps: S1, raw material preparation；S2,
The extraction and preparation of P-Cymene；The thick general flavone of S3, folium artemisiae argyi, Thick many candies extract and preparation.Wherein, it should be noted that raw material
The process of preparation is that wormwood is divided into folium artemisiae argyi and Ai Gen, after folium artemisiae argyi is dried in the shade to water content≤8%, 20 meshes are crossed after smashing, must be ended
Leaf coarse powder.
And in step S2 extraction and the preparation of P-Cymene specific steps are as follows:
S21, P-Cymene extract: folium artemisiae argyi coarse powder 5kg, and extraction kettle inlet pressure is 26MPa, outlet pressure 24MPa, extraction temperature
Degree is 50 DEG C；The process conditions of Supercritical CO2 rectification separation are rectifying column inlet pressure 23MPa, and rectifying column outlet pressure is
18MPa, temperature 45 C；Separating still process conditions are 10MPa, temperature 45 C.P-Cymene medicinal extract is precipitated from rectifying column bottom, Chinese mugwort
Leaf essential oil light oil is flowed out from tower top, until separating in separating still, obtains folium artemisiae argyi light oil 60g.
S22, P-Cymene crude product are produced: molecular distillation process conditions are that evaporating surface temperature is 75 DEG C, charging rate 120
Ml/h, condensate layer temperature are 40 DEG C, pressure 0.1Pa, and sample introduction, what light component bottle was collected into is P-Cymene heavy oil, heavy constituent
What bottle was collected into is folium artemisiae argyi wax.Wherein P-Cymene heavy oil 80g, wax 65g.
The specific steps that the thick general flavone of folium artemisiae argyi, Thick many candies are extracted and prepared in step S3 are as follows:
S31, the thick general flavone of Chinese mugwort liquid and Thick many candies extract: the folium artemisiae argyi grouts are extracted folium artemisiae argyi using CO2 supercritical extraction unit
General flavone and Thick many candies, extraction kettle temperature 50 C, extraction kettle are pressed 30Mpa, extraction time 120min, 30 DEG C of extraction-container temperature, are solved
Kettle pressure 4MPa is analysed, for the ethyl alcohol that concentration is 50% as entrainer, entrainer dosage 2mL/g, gas flow 20kg/h obtain folium artemisiae argyi
Thick general flavone, Thick many candies extracting solution.
The preparation of S32, folium artemisiae argyi thick general flavone and Thick many candies concentrate: by the thick general flavone of the folium artemisiae argyi, Thick many candies extracting solution
It carries out in concentration tank in 40 DEG C of temperature being concentrated under reduced pressure into the 1/3 of original volume and obtains concentrate.
The separation of solid and liquid of the concentrate of the thick general flavone of S33, folium artemisiae argyi and Thick many candies: by the concentrate second of concentration 90%
Alcohol alcohol precipitation, 4 DEG C overnight, are filtered to obtain alcohol precipitation filtrate and alcohol precipitation filter residue later.
The preparation of the thick general flavone of S34, folium artemisiae argyi: being concentrated under reduced pressure to obtain concentrated extract for the alcohol precipitation filtrate at a temperature of 40 DEG C,
Thick general flavone 40g is obtained after concentrated extract is dry.
The thick general flavone purification of S35, folium artemisiae argyi: obtaining sample solution with the ethyl alcohol dissolved dilution that concentration is 30% for the concentrated extract,
It is adsorbed through macroporous absorbent resin, then with the macroreticular resin after the absorption of the ethanol elution of 80% concentration that volume is 4BV, collects 80% second
The eluent of alcohol is dried in vacuo to obtain smart general flavone 33g under the conditions of 60 DEG C of temperature after eluent is concentrated.
The preparation of S36, folium artemisiae argyi Thick many candies: by the alcohol precipitation filter residue be centrifugated to obtain precipitating, precipitating after drying it is slightly more
Sugared 58g.
S37, the purification of folium artemisiae argyi Thick many candies: by 3 times of volumes of the precipitating, the ethyl alcohol of concentration 80%, 90%, 95%, 100% into
Row classification alcohol precipitation, 4 DEG C of alcohol precipitation 4h, are centrifuged off supernatant later every time, must precipitates through dry primary essence polysaccharide 40g.Implement
Example 2
Present embodiment discloses a kind of method of comprehensive utilization of wormwood effective component, comprising the following steps: S1, raw material preparation；S2,
The extraction and preparation of P-Cymene；The thick general flavone of S3, folium artemisiae argyi, Thick many candies extract and preparation.Wherein, it should be noted that raw material
The process of preparation is that wormwood is divided into folium artemisiae argyi and Ai Gen, after folium artemisiae argyi is dried in the shade to water content≤8%, 30 meshes are crossed after smashing, must be ended
Leaf coarse powder.
And in step S2 extraction and the preparation of P-Cymene specific steps are as follows:
S21, P-Cymene extract: folium artemisiae argyi coarse powder 4.8kg, and extraction kettle inlet pressure is 25MPa, outlet pressure 23.5MPa, extraction
Taking temperature is 50 DEG C；The process conditions of Supercritical CO2 rectification separation are rectifying column inlet pressure 22MPa, rectifying column outlet pressure
For 16MPa, temperature 50 C；Separating still process conditions are 10MPa, temperature 45 C.P-Cymene medicinal extract is precipitated from rectifying column bottom,
P-Cymene light oil is flowed out from tower top, until separating in separating still, obtains folium artemisiae argyi light oil 55g.
S22, P-Cymene crude product are produced: molecular distillation process conditions are that evaporating surface temperature is 70 DEG C, charging rate 120
Ml/h, condensate layer temperature are 40 DEG C, pressure 0.2Pa, and sample introduction, what light component bottle was collected into is P-Cymene heavy oil, heavy constituent
What bottle was collected into is folium artemisiae argyi wax.Wherein P-Cymene heavy oil 75g, wax 52g.
The specific steps that the thick general flavone of folium artemisiae argyi, Thick many candies are extracted and prepared in step S3 are as follows:
S31, the thick general flavone of Chinese mugwort liquid and Thick many candies extract: the folium artemisiae argyi grouts are extracted folium artemisiae argyi using CO2 supercritical extraction unit
General flavone and Thick many candies, extraction kettle temperature 50 C, extraction kettle are pressed 30Mpa, extraction time 120min, 30 DEG C of extraction-container temperature, are solved
Kettle pressure 4MPa is analysed, for the ethyl alcohol that concentration is 70% as entrainer, entrainer dosage 2mL/g, gas flow 22kg/h obtain folium artemisiae argyi
Thick general flavone, Thick many candies extracting solution.
The preparation of S32, folium artemisiae argyi thick general flavone and Thick many candies concentrate: by the thick general flavone of the folium artemisiae argyi, Thick many candies extracting solution
It carries out in concentration tank in 40 DEG C of temperature being concentrated under reduced pressure into the 1/4 of original volume and obtains concentrate.
The separation of solid and liquid of the concentrate of the thick general flavone of S33, folium artemisiae argyi and Thick many candies: by the concentrate second of concentration 90%
Alcohol alcohol precipitation, 4 DEG C overnight, are filtered to obtain alcohol precipitation filtrate and alcohol precipitation filter residue later.
The preparation of the thick general flavone of S34, folium artemisiae argyi: being concentrated under reduced pressure to obtain concentrated extract for the alcohol precipitation filtrate at a temperature of 40 DEG C,
Thick general flavone 32g is obtained after concentrated extract is dry.
The thick general flavone purification of S35, folium artemisiae argyi: obtaining sample solution with the ethyl alcohol dissolved dilution that concentration is 30% for the concentrated extract,
It is adsorbed through macroporous absorbent resin, then with the macroreticular resin after the absorption of the ethanol elution of 80% concentration that volume is 4BV, collects 80% second
The eluent of alcohol is dried in vacuo to obtain smart general flavone 24g under the conditions of 60 DEG C of temperature after eluent is concentrated.
The preparation of S36, folium artemisiae argyi Thick many candies: by the alcohol precipitation filter residue be centrifugated to obtain precipitating, precipitating after drying it is slightly more
Sugared 48g.
S37, the purification of folium artemisiae argyi Thick many candies: by 3 times of volumes of the precipitating, the ethyl alcohol of concentration 80%, 90%, 95%, 100% into
Row classification alcohol precipitation, 4 DEG C of alcohol precipitation 4h, are centrifuged off supernatant later every time, must precipitates through dry primary essence polysaccharide 34g.
Embodiment 3
Present embodiment discloses a kind of method of comprehensive utilization of wormwood effective component, comprising the following steps: S1, raw material preparation；S2,
The extraction and preparation of P-Cymene；The thick general flavone of S3, folium artemisiae argyi, Thick many candies extract and preparation.Wherein, it should be noted that raw material
The process of preparation is that wormwood is divided into folium artemisiae argyi and Ai Gen, after folium artemisiae argyi is dried in the shade to water content≤8%, 60 meshes are crossed after smashing, must be ended
Leaf coarse powder.
And in step S2 extraction and the preparation of P-Cymene specific steps are as follows:
S21, P-Cymene extract: folium artemisiae argyi coarse powder 4kg, and extraction kettle inlet pressure is 25MPa, outlet pressure 23MPa, extraction temperature
Degree is 50 DEG C；The process conditions of Supercritical CO2 rectification separation are rectifying column inlet pressure 22MPa, and rectifying column outlet pressure is
16MPa, temperature 45 C；Separating still process conditions be 8MPa, 40 DEG C of temperature.P-Cymene medicinal extract is precipitated from rectifying column bottom, Chinese mugwort
Leaf essential oil light oil is flowed out from tower top, until separating in separating still, obtains folium artemisiae argyi light oil 36g.
S22, P-Cymene crude product are produced: molecular distillation process conditions are that evaporating surface temperature is 85 DEG C, charging rate 130
Ml/h, condensate layer temperature are 40 DEG C, pressure 0.1Pa, and sample introduction, what light component bottle was collected into is P-Cymene heavy oil, heavy constituent
What bottle was collected into is folium artemisiae argyi wax.Wherein P-Cymene heavy oil 40g, wax 30g.
The specific steps that the thick general flavone of folium artemisiae argyi, Thick many candies are extracted and prepared in step S3 are as follows:
S31, the thick general flavone of Chinese mugwort liquid and Thick many candies extract: the folium artemisiae argyi grouts are extracted folium artemisiae argyi using CO2 supercritical extraction unit
General flavone and Thick many candies, extraction kettle temperature 50 C, extraction kettle are pressed 30Mpa, extraction time 120min, 30 DEG C of extraction-container temperature, are solved
Kettle pressure 4MPa is analysed, for the ethyl alcohol that concentration is 50% as entrainer, entrainer dosage 2mL/g, gas flow 20kg/h obtain folium artemisiae argyi
Thick general flavone, Thick many candies extracting solution.
The preparation of S32, folium artemisiae argyi thick general flavone and Thick many candies concentrate: by the thick general flavone of the folium artemisiae argyi, Thick many candies extracting solution
It carries out in concentration tank in 40 DEG C of temperature being concentrated under reduced pressure into the 1/5 of original volume and obtains concentrate.
The separation of solid and liquid of the concentrate of the thick general flavone of S33, folium artemisiae argyi and Thick many candies: by the concentrate second of concentration 95%
Alcohol alcohol precipitation, 4 DEG C overnight, are filtered to obtain alcohol precipitation filtrate and alcohol precipitation filter residue later.
The preparation of the thick general flavone of S34, folium artemisiae argyi: being concentrated under reduced pressure to obtain concentrated extract for the alcohol precipitation filtrate at a temperature of 40 DEG C,
Thick general flavone 28g is obtained after concentrated extract is dry.
The thick general flavone purification of S35, folium artemisiae argyi: obtaining sample solution with the ethyl alcohol dissolved dilution that concentration is 30% for the concentrated extract,
It is adsorbed through macroporous absorbent resin, then with the macroreticular resin after the absorption of the ethanol elution of 80% concentration that volume is 4BV, collects 80% second
The eluent of alcohol is dried in vacuo to obtain smart general flavone 19g under the conditions of 60 DEG C of temperature after eluent is concentrated.
The preparation of S36, folium artemisiae argyi Thick many candies: by the alcohol precipitation filter residue be centrifugated to obtain precipitating, precipitating after drying it is slightly more
Sugared 23g.
S37, the purification of folium artemisiae argyi Thick many candies: by 3 times of volumes of the precipitating, the ethyl alcohol of concentration 80%, 90%, 95%, 100% into
Row classification alcohol precipitation, 4 DEG C of alcohol precipitation 4h, are centrifuged off supernatant later every time, must precipitates through dry primary essence polysaccharide 15g.
Embodiment 4
Present embodiment discloses a kind of method of comprehensive utilization of wormwood effective component, comprising the following steps: S1, raw material preparation；S2,
The extraction and preparation of P-Cymene；The thick general flavone of S3, folium artemisiae argyi, Thick many candies extract and preparation.Wherein, it should be noted that raw material
The process of preparation is that wormwood is divided into folium artemisiae argyi and Ai Gen, after folium artemisiae argyi is dried in the shade to water content≤8%, 20 meshes are crossed after smashing, must be ended
Leaf coarse powder.
And in step S2 extraction and the preparation of P-Cymene specific steps are as follows:
S21, P-Cymene extract: folium artemisiae argyi coarse powder 6kg, and extraction kettle inlet pressure is 23MPa, outlet pressure 22MPa, extraction temperature
Degree is 45 DEG C；The process conditions of Supercritical CO2 rectification separation are rectifying column inlet pressure 20MPa, and rectifying column outlet pressure is
17MPa, temperature 45 C；Separating still process conditions are 8MPa, temperature 45 C.P-Cymene medicinal extract is precipitated from rectifying column bottom, Chinese mugwort
Leaf essential oil light oil is flowed out from tower top, until separating in separating still, obtains folium artemisiae argyi light oil 72g.
S22, P-Cymene crude product are produced: molecular distillation process conditions are that evaporating surface temperature is 85 DEG C, charging rate 120
Ml/h, condensate layer temperature are 40 DEG C, pressure 0.1Pa, and sample introduction, what light component bottle was collected into is P-Cymene heavy oil, heavy constituent
What bottle was collected into is folium artemisiae argyi wax.Wherein P-Cymene heavy oil 103g, wax 84g.
The specific steps that the thick general flavone of folium artemisiae argyi, Thick many candies are extracted and prepared in step S3 are as follows:
S31, the thick general flavone of Chinese mugwort liquid and Thick many candies extract: the folium artemisiae argyi grouts are extracted folium artemisiae argyi using CO2 supercritical extraction unit
General flavone and Thick many candies, extraction kettle temperature 60 C, extraction kettle are pressed 35Mpa, extraction time 120min, 30 DEG C of extraction-container temperature, are solved
Kettle pressure 4MPa is analysed, for the ethyl alcohol that concentration is 75% as entrainer, entrainer dosage 2mL/g, gas flow 20kg/h obtain folium artemisiae argyi
Thick general flavone, Thick many candies extracting solution.
The preparation of S32, folium artemisiae argyi thick general flavone and Thick many candies concentrate: by the thick general flavone of the folium artemisiae argyi, Thick many candies extracting solution
It carries out in concentration tank in 40 DEG C of temperature being concentrated under reduced pressure into the 1/3 of original volume and obtains concentrate.
The separation of solid and liquid of the concentrate of the thick general flavone of S33, folium artemisiae argyi and Thick many candies: by the concentrate second of concentration 90%
Alcohol alcohol precipitation, 4 DEG C overnight, are filtered to obtain alcohol precipitation filtrate and alcohol precipitation filter residue later.
The preparation of the thick general flavone of S34, folium artemisiae argyi: being concentrated under reduced pressure to obtain concentrated extract for the alcohol precipitation filtrate at a temperature of 40 DEG C,
Thick general flavone 48g is obtained after concentrated extract is dry.
The thick general flavone purification of S35, folium artemisiae argyi: obtaining sample solution with the ethyl alcohol dissolved dilution that concentration is 30% for the concentrated extract,
It is adsorbed through macroporous absorbent resin, then with the macroreticular resin after the absorption of the ethanol elution of 70% concentration that volume is 4BV, collects 70% second
The eluent of alcohol is dried in vacuo to obtain smart general flavone 39g under the conditions of 60 DEG C of temperature after eluent is concentrated.
The preparation of S36, folium artemisiae argyi Thick many candies: by the alcohol precipitation filter residue be centrifugated to obtain precipitating, precipitating after drying it is slightly more
Sugared 64g.
S37, the purification of folium artemisiae argyi Thick many candies: by 3 times of volumes of the precipitating, the ethyl alcohol of concentration 80%, 90%, 95%, 100% into
Row classification alcohol precipitation, 4 DEG C of alcohol precipitation 4h, are centrifuged off supernatant later every time, must precipitates through dry primary essence polysaccharide 52g.
Embodiment 5
Present embodiment discloses a kind of method of comprehensive utilization of wormwood effective component, comprising the following steps: S1, raw material preparation；S2,
The extraction and preparation of P-Cymene；The thick general flavone of S3, folium artemisiae argyi, Thick many candies extract and preparation.Wherein, it should be noted that raw material
The process of preparation is that wormwood is divided into folium artemisiae argyi and Ai Gen, after folium artemisiae argyi is dried in the shade to water content≤8%, 50 meshes are crossed after smashing, must be ended
Leaf coarse powder.
And in step S2 extraction and the preparation of P-Cymene specific steps are as follows:
S21, P-Cymene extract: folium artemisiae argyi coarse powder 3kg, and extraction kettle inlet pressure is 28MPa, outlet pressure 25MPa, extraction temperature
Degree is 50 DEG C；The process conditions of Supercritical CO2 rectification separation are rectifying column inlet pressure 24MPa, and rectifying column outlet pressure is
18MPa, temperature 45 C；Separating still process conditions are 8MPa, temperature 45 C.P-Cymene medicinal extract is precipitated from rectifying column bottom, Chinese mugwort
Leaf essential oil light oil is flowed out from tower top, until separating in separating still, obtains folium artemisiae argyi light oil 25g.
S22, P-Cymene crude product are produced: molecular distillation process conditions are that evaporating surface temperature is 85 DEG C, charging rate 120
Ml/h, condensate layer temperature are 30 DEG C, pressure 0.1Pa, and sample introduction, what light component bottle was collected into is P-Cymene heavy oil, heavy constituent
What bottle was collected into is folium artemisiae argyi wax.Wherein P-Cymene heavy oil 36g, wax 41g.
The specific steps that the thick general flavone of folium artemisiae argyi, Thick many candies are extracted and prepared in step S3 are as follows:
S31, the thick general flavone of Chinese mugwort liquid and Thick many candies extract: the folium artemisiae argyi grouts are extracted folium artemisiae argyi using CO2 supercritical extraction unit
General flavone and Thick many candies, extraction kettle temperature 50 C, extraction kettle are pressed 35Mpa, extraction time 120min, 30 DEG C of extraction-container temperature, are solved
Kettle pressure 4MPa is analysed, for the ethyl alcohol that concentration is 50% as entrainer, entrainer dosage 2mL/g, gas flow 20kg/h obtain folium artemisiae argyi
Thick general flavone, Thick many candies extracting solution.
The preparation of S32, folium artemisiae argyi thick general flavone and Thick many candies concentrate: by the thick general flavone of the folium artemisiae argyi, Thick many candies extracting solution
It carries out in concentration tank in 40 DEG C of temperature being concentrated under reduced pressure into the 1/4 of original volume and obtains concentrate.
The separation of solid and liquid of the concentrate of the thick general flavone of S33, folium artemisiae argyi and Thick many candies: by the concentrate second of concentration 90%
Alcohol alcohol precipitation, 4 DEG C overnight, are filtered to obtain alcohol precipitation filtrate and alcohol precipitation filter residue later.
The preparation of the thick general flavone of S34, folium artemisiae argyi: being concentrated under reduced pressure to obtain concentrated extract for the alcohol precipitation filtrate at a temperature of 40 DEG C,
Thick general flavone 31g is obtained after concentrated extract is dry.
The thick general flavone purification of S35, folium artemisiae argyi: obtaining sample solution with the ethyl alcohol dissolved dilution that concentration is 30% for the concentrated extract,
It is adsorbed through macroporous absorbent resin, then with the macroreticular resin after the absorption of the ethanol elution of 70% concentration that volume is 4BV, collects 70% second
The eluent of alcohol is dried in vacuo to obtain smart general flavone 22g under the conditions of 60 DEG C of temperature after eluent is concentrated.
The preparation of S36, folium artemisiae argyi Thick many candies: by the alcohol precipitation filter residue be centrifugated to obtain precipitating, precipitating after drying it is slightly more
Sugared 34g.
S37, the purification of folium artemisiae argyi Thick many candies: by 3 times of volumes of the precipitating, the ethyl alcohol of concentration 80%, 90%, 95%, 100% into
Row classification alcohol precipitation, 4 DEG C of alcohol precipitation 4h, are centrifuged off supernatant later every time, must precipitates through dry primary essence polysaccharide 22g.
Embodiment 6
Present embodiment discloses a kind of method of comprehensive utilization of wormwood effective component, comprising the following steps: S0, folium artemisiae argyi, Chinese mugwort root system
It is standby: wormwood is divided into folium artemisiae argyi and Ai Gen；S1, Chinese mugwort root is cleaned, is cleaned, it is spare to be crushed to 50 mesh；S2,10kg Chinese mugwort root raw material is ended
Root raw material, which is put into steam distillation apparatus, carries out steam extraction, and temperature is 95 DEG C when distillation, distillation time 3h；S3, receipts
It is collected after the distillate collected is cooling in cooler, cooling temperature is 30 DEG C；S4, collection distillate obtain Chinese mugwort root hydrosol, warp
Reverse osmosis concentration, the reverse osmosis trapped fluid of gained are the Chinese mugwort root hydrosol of concentration.
Embodiment 7
Present embodiment discloses a kind of method of comprehensive utilization of wormwood effective component, comprising the following steps: S0, folium artemisiae argyi, Chinese mugwort root system
It is standby: wormwood is divided into folium artemisiae argyi and Ai Gen；S1, Chinese mugwort root is cleaned, is cleaned, it is spare to be crushed to 70 mesh；S2, end 30kg root raw material
It is put into steam distillation apparatus and carries out steam extraction, temperature is 95 DEG C when distillation, distillation time 3h；S3, it is collected into
It is collected after distillate is cooling in cooler, cooling temperature is 30 DEG C；S4, collection distillate obtain Chinese mugwort root hydrosol, through reverse osmosis
Concentration, the reverse osmosis trapped fluid of gained are the Chinese mugwort root hydrosol of concentration.
Embodiment 8
Present embodiment discloses a kind of method of comprehensive utilization of wormwood effective component, comprising the following steps: S0, folium artemisiae argyi, Chinese mugwort root system
It is standby: wormwood is divided into folium artemisiae argyi and Ai Gen；S1, Chinese mugwort root is cleaned, is cleaned, it is spare to be crushed to 100 mesh；S2,8kg Chinese mugwort root raw material is put
Enter and carry out steam extraction in steam distillation apparatus, temperature is 95 DEG C when distillation, distillation time 4h；S3, evaporating of being collected into
It is collected after liquid is cooling in cooler out, cooling temperature is 30 DEG C；S4, collection distillate obtain Chinese mugwort root hydrosol, through reverse osmosis concentrated
Contracting, the reverse osmosis trapped fluid of gained are the Chinese mugwort root hydrosol of concentration.
Embodiment 9
Present embodiment discloses a kind of method of comprehensive utilization of wormwood effective component, comprising the following steps: S0, folium artemisiae argyi, Chinese mugwort root system
It is standby: wormwood is divided into folium artemisiae argyi and Ai Gen；S1, Chinese mugwort root is cleaned, is cleaned, it is spare to be crushed to 60 mesh；S2,20kg Chinese mugwort root raw material is put
Enter and carry out steam extraction in steam distillation apparatus, temperature is 95 DEG C when distillation, distillation time 2h；S3, evaporating of being collected into
It is collected after liquid is cooling in cooler out, cooling temperature is 30 DEG C；S4, collection distillate obtain Chinese mugwort root hydrosol, through reverse osmosis concentrated
Contracting, the reverse osmosis trapped fluid of gained are the Chinese mugwort root hydrosol of concentration.
Embodiment 10
Present embodiment discloses a kind of method of comprehensive utilization of wormwood effective component, comprising the following steps: S0, folium artemisiae argyi, Chinese mugwort root system
It is standby: wormwood is divided into folium artemisiae argyi and Ai Gen；S1, Chinese mugwort root is cleaned, is cleaned, it is spare to be crushed to 80 mesh；S2,10kg Chinese mugwort root raw material is put
Enter and carry out steam extraction in steam distillation apparatus, temperature is 90 DEG C when distillation, distillation time 4h；S3, evaporating of being collected into
It is collected after liquid is cooling in cooler out, cooling temperature is 25 DEG C；S4, collection distillate obtain Chinese mugwort root hydrosol, through reverse osmosis concentrated
Contracting, the reverse osmosis trapped fluid of gained are the Chinese mugwort root hydrosol of concentration.
Obviously, the above embodiment of the present invention is only intended to clearly illustrate examples made by the present invention, and is not to this
The restriction of the embodiment of invention.It for those of ordinary skill in the art, on the basis of the above description can be with
It makes other variations or changes in different ways.There is no necessity and possibility to exhaust all the enbodiments.It is all in this hair
Made any modifications, equivalent replacements, and improvements etc., should be included in the claims in the present invention within bright spirit and principle
Within protection scope.
Claims (10)
1. a kind of method of comprehensive utilization of wormwood effective component, which comprises the following steps:
S0, folium artemisiae argyi, Chinese mugwort root preparation: wormwood is divided into folium artemisiae argyi and Ai Gen；
S1, the preparation of folium artemisiae argyi raw material: folium artemisiae argyi is dried in the shade to water content≤8%, smashes to 20 ~ 100 mesh, obtains folium artemisiae argyi coarse powder；
S2, P-Cymene extract: by the folium artemisiae argyi coarse powder using supercritical CO 2 extraction device extraction, Supercritical CO2 rectification column point
It isolates and purifies to obtain P-Cymene light oil, P-Cymene heavy oil and medicinal extract, and obtains folium artemisiae argyi grouts from, separating still；
S3, the purification of P-Cymene medicinal extract: the P-Cymene medicinal extract is further refined through molecular distillation, P-Cymene weight is obtained
Oil and folium artemisiae argyi wax；
S4, artemisia leaf total chromocor and Thick many candies extract: supercritical CO 2 extraction device is added in the folium artemisiae argyi grouts, and entrainment is added
Agent extraction artemisia leaf total chromocor and Thick many candies, 35 ~ 80 DEG C of extraction kettle temperature, extraction kettle 20 ~ 40MPa of pressure, extraction time 30 ~
180min, 20 ~ 35 DEG C of extraction-container temperature, 3 ~ 6MPa of extraction-container pressure, the entrainer is the ethyl alcohol that concentration is 20% ~ 95%, folder
Band 1 ~ 3mL/g of agent dosage, 10 ~ 30kg/h of gas flow, obtain the thick general flavone of folium artemisiae argyi, Thick many candies extracting solution；
S5, the thick general flavone of folium artemisiae argyi, Thick many candies extracting solution are concentrated, separates, refine, obtaining artemisia leaf total chromocor and Thick many candies.
2. the method for comprehensive utilization of wormwood effective component according to claim 1, which is characterized in that end in the step S5
The thick general flavone of leaf, the concentration of Thick many candies extracting solution, separation, purification specifically includes the following steps:
S51, the thick general flavone of the folium artemisiae argyi, Thick many candies extracting solution are concentrated under reduced pressure into concentration tank in 30 ~ 60 DEG C of temperature
The 1/5 ~ 1/2 of original volume obtains concentrate；
S52, by the ethyl alcohol alcohol precipitation of concentrate concentration 80% ~ 100%, 4 DEG C overnight, are filtered to obtain alcohol precipitation filtrate and alcohol later
Heavy filter residue；
S53, the alcohol precipitation filtrate is concentrated under reduced pressure to obtain at a temperature of 30 ~ 60 DEG C to concentrated extract, is obtained after concentrated extract is dry slightly total
Flavones；
S54, the ethyl alcohol dissolved dilution that concentrated extract distilled water or concentration are 20% ~ 95% is obtained into sample solution, is inhaled through macropore
Attached resin adsorption, then with 3 ~ 4 times of column volume distilled water, concentration be 60% ~ 80% ethanol elution absorption after macroreticular resin, collect
Ethanol eluate is dried in vacuo to obtain smart general flavone under the conditions of 60 DEG C of temperature after eluent is concentrated；
S55, it is centrifugated the alcohol precipitation filter residue to obtain precipitating, precipitating obtains Thick many candies after drying；
S56, by the precipitating successively with 2 ~ 4 times of volumes, the ethyl alcohol of concentration 80%, 90%, 95%, 100% carries out classification alcohol precipitation, often
Inferior to 4 DEG C alcohol precipitation 4h, are centrifuged off supernatant later, must precipitate through dry primary smart polysaccharide.
3. the method for comprehensive utilization of wormwood effective component according to claim 2, which is characterized in that in step S52, greatly
Macroporous adsorbent resin is one of S-8, D-101, XDA-1, AB-8, LSA-20, NKA-9, NKA- II or a variety of, sample solution concentration
For 0.2 ~ 0.5 mg/mL, loading 1 ~ 2BV/h of speed, sample solution pH value 4 ~ 6, applied sample amount is 0.5g crude product/100g macroporous absorption
Resin, elution flow rate about 1 ~ 3BV/h.
4. the method for comprehensive utilization of wormwood effective component according to claim 1, which is characterized in that in the step S2
In, the process conditions of SCF-CO 2 are that extraction kettle inlet pressure is 20 ~ 28MPa, and outlet pressure is 19 ~ 26MPa, extraction
Temperature is 35 ~ 60 DEG C；The process conditions of Supercritical CO2 rectification separation are 18 ~ 26MPa of rectifying column inlet pressure, rectifying column outlet
Pressure be 8 ~ 25MPa, 15 ~ 65 DEG C of temperature；Separating still process conditions be 5 ~ 25MPa, 15 ~ 75 DEG C of temperature；The small folium artemisiae argyi of solubility
Essential oil medicinal extract is precipitated from rectifying column bottom, wherein containing P-Cymene wax, P-Cymene heavy oil composition；The big folium artemisiae argyi of solubility
Essential oil light oil is flowed out from tower top, until separating in separating still.
5. the method for comprehensive utilization of wormwood effective component according to claim 1, which is characterized in that in the step S3
In, molecular distillation process conditions are that evaporating surface temperature is 65 ~ 85 DEG C, and charging rate is 100 ~ 150 ml/h, and condensate layer temperature is
35 ~ 50 DEG C, 0.1 ~ 0.5Pa of pressure, sample introduction after the P-Cymene medicinal extract heating water bath is in a liquid state, light component bottle is collected into
As P-Cymene heavy oil, what recombination sub-bottle was collected into is folium artemisiae argyi wax.
6. the method for comprehensive utilization of wormwood effective component according to claim 1, which is characterized in that the thick general flavone of folium artemisiae argyi and
What thick total starches obtained simultaneously through SCF-CO 2.
7. the method for comprehensive utilization of wormwood effective component according to claim 1, which is characterized in that the folium artemisiae argyi in step S4
Grouts can be and just extract the folium artemisiae argyi grouts of P-Cymene, be also possible to extract it is dry after essential oil after folium artemisiae argyi grouts.
8. the method for comprehensive utilization of wormwood effective component according to claim 1, which is characterized in that P-Cymene extract and
The thick general flavone of folium artemisiae argyi, Thick many candies can continuous extraction, extraction can also be interrupted.
9. a kind of method of comprehensive utilization of wormwood effective component, which comprises the following steps:
S0, folium artemisiae argyi, Chinese mugwort root preparation: wormwood is divided into folium artemisiae argyi and Ai Gen；
S1, Chinese mugwort root is cleaned, is cleaned, it is spare to be crushed to 20 ~ 100 mesh；
S2, Chinese mugwort root raw material is put into steam distillation apparatus and carries out steam extraction, temperature is 80 DEG C ~ 95 DEG C when distillation, is steamed
Evaporating the time is 2 ~ 4.5h；
It is collected after S3, the distillate being collected into are cooling in cooler, cooling temperature is 20 DEG C ~ 30 DEG C；
S4, collection distillate obtain Chinese mugwort root hydrosol, and through reverse osmosis concentration, the reverse osmosis trapped fluid of gained is the Chinese mugwort root hydrosol of concentration,
The pressure of reverse osmosis membrane is 0.85~2.5MPa.
10. the method for comprehensive utilization of wormwood effective component according to claim 9, which is characterized in that in step s 4, instead
The desalination rate for the reverse osmosis membrane that infiltration processing uses is 98.0 ~ 99.6%, and filter sizes are 0.15 ~ 1.6 um.
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