CN1269547C - Method for extracting effective substance from folium Artemisiae Argyi by supercritical carbon dioxide extraction - Google Patents
Method for extracting effective substance from folium Artemisiae Argyi by supercritical carbon dioxide extraction Download PDFInfo
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Abstract
The invention discloses a method for extracting effective substances of folium artemisiae argyi by supercritical carbon dioxide. The method comprises the steps of taking supercritical carbon dioxide as an extracting agent, carrying out forward or reverse circulation extraction on a raw material moxa which is dried, appropriately chopped or smashed into fragments or velvet-like substances, carrying out one-stage or more than one-stage decompression analysis and separation on the obtained carbon dioxide rich in target extraction substances, continuously participating in supercritical extraction circulation on the separated carbon dioxide, and obtaining effective substances, namely the moxa volatile oil or the moxa volatile oil mixture. The method has the advantages of high extraction speed, high yield, simple flow, convenient operation, realization of separation in the extraction process, safety, reliability, no environmental pollution, and high yield and purity of the obtained product, and is a high-efficiency and energy-saving method for extracting and separating the moxa.
Description
Technical field
The present invention relates to the method for a kind of supercritical carbon dioxide extracting Chinese mugwort active principle, exactly is exactly to adopt CO 2 fluid under the supercriticality as extractant, the extraction and separation technology of its active principle of extraction from Chinese mugwort.
Background technology
Chinese mugwort derives from feverfew Chinese mugwort Artemisia argyi Levl.et Vant., and " dried leaves of recording main its aerial part of use of Chinese pharmacopoeia version in 2000 is called tarragon.Tarragon has special aroma, bitter, suffering, slightly warm in nature, tool dispelling cold and removing dampness, the effect of warming channel for arresting bleeding.Cure mainly few abdomen crymodynia, cold infertile, hematemesis and epistaxis, uterine bleeding be through many through cold uncomfortable, palace, diseases such as gestation hemorrhage, pruitus.In fact the former plant of commodity medicinal material tarragon has comprised the artemisia various plants, except that Chinese mugwort, Chinese mugwort, Korea Chinese mugwort, mugwort wormwood artemisia, wide leaf mountain wormwood artemisia, red sufficient wormwood artemisia, southern argy wormwood, Herba Artemisiae mongolicae, May, Chinese mugwort, stalwart wormwood artemisia and qi stem wormwood artemisia etc. were also used as Chinese mugwort in the locality, its quality is different and difference to some extent with the place of production, be good wherein, can be considered the authentic medicinal herbs of tarragon with cultivation of Qichun County, Hubei or wild Chinese mugwort quality.
Tarragon contains volatile oil, has multiple pharmacological actions such as antibiotic, antiviral, relieving cough and asthma, antiallergy, now has been widely used in the fields such as pharmacy, health and epidemic prevention, fine chemistry industry, essence and flavoring agent.According to relevant bibliographical information, the mid-boiling point position pharmacologically active of volatile argyi leaf oil than its higher boiling position slightly a little less than---its mid-boiling point position contains 1, compositions such as 8-cineole, terpinenol-4, α-terpinenol, β-cloves alkene, artemisol, trans-carveol, australene, sabinene, amphene, α-phellandrene, camphor, borneol, absinthol, isothujone, α-terpinene, piperitone, compositions such as α-Xue Songxi, farnesene, eugenol, dibutyl phthalate, palmitic acid, cloves olefinic oxide are then contained at its higher boiling position.
At present, extract the conventional method of separating volatile argyi leaf oil steam distillation, milling process and organic solvent extractionprocess are arranged.Wherein, steam distillation is simple to operate, can extract the low volatility essential oil, but causes the abundant high volatile volatile composition of content and a large amount of losses of thermal sensitivity component easily, influences the medicinal effects of tarragon; Milling process is fit to suitability for industrialized production, but products obtained therefrom impurity is many, and is perishable, and extraction efficiency is low; The organic solvent extractionprocess yield is higher, but products obtained therefrom easily causes chemical solvent and heavy-metal residual, has a strong impact on the purity and the quality of product, has reduced its medical value.
Supercritical liquid extraction technique is a kind of novel green extraction and separation technology, and its principle is to utilize the influence of pressure and temperature to the shooting flow volume density, improves the solvability of supercritical fluid to the target extraction of substance.Both had gas like lower viscosity, high diffusibility and be in the supercritical carbon dioxide fluid, had the high density and the fine solubility energy of similar liquids again.Under supercriticality, CO 2 fluid is contacted with material to be separated, can change the solvability that supercritical carbon dioxide fluid is treated separate substance by pressure, variation of temperature, make it extract, separate the target effective composition selectively.According to literature search, up to the present still do not have and adopt the method for volatilization wet goods active principle in the supercritical carbon dioxide extracting tarragon to come out.
Summary of the invention
Purpose of the present invention just provides a kind of method of supercritical carbon dioxide extracting Chinese mugwort active principle, adopt this method flow simple, easy to operate, in extraction process, realize simultaneously separating, producers and environment are had no adverse effects, and the yield and the purity of Chinese mugwort active principle are higher.
For achieving the above object, the method of the supercritical carbon dioxide extracting Chinese mugwort active principle that the present invention is designed, be earlier the raw material Chinese mugwort to be carried out drying to handle, then that the raw material of drying Chinese mugwort is broken or be ground into fragment or velvet-like thing, again it is carried out supercritical carbon dioxide extracting, at last the carbon dioxide that contains the target extract is carried out one-level or the parsing of the decompression more than one-level separation, the carbon dioxide after the separation continues to participate in the supercritical extract circulation, and the component that parses is the Chinese mugwort active principle.
Said method is that the CO 2 fluid that utilizes the CO 2 fluid be in different pressures and state of temperature chemical analysis in the Chinese mugwort to be had bigger dissolubility difference and equal state has different solvabilities to different chemical composition in the Chinese mugwort, realize to the extraction of target substance with separate.So selecting suitable process condition is further to improve the recovery rate of active principle in the raw material Chinese mugwort and the key factor of separation and purification degree.Therefore:
In the supercritical extraction process of said method, can adopt supercritical carbon dioxide endless form forward or backwards, the mass ratio of setting per hour the circulate consumption and the extraction entrainer consumption of raw material Chinese mugwort consumption and extractant carbon dioxide is followed successively by 1: 5～50: 0～0.5, extracting pressure is 7～50MPa, extraction temperature is 20～70 ℃, and the extraction time is 0.5～16h.Its optimum condition is: the mass ratio of per hour the circulate consumption and the extraction entrainer consumption of raw material Chinese mugwort consumption and extractant carbon dioxide is followed successively by 1: 10～30: 0～0.2, extracting pressure is 10～25MPa, extraction temperature is 35～55 ℃, and the extraction time is 1～10h.
Reduce pressure in the one-level of said method or more than the one-level in the parsing separating technology, can set one-level knockout drum pressure is 4～15MPa, and secondary and above knockout drum pressure are 2～12Mpa, and knockout drum temperature at different levels are 22～80 ℃.Its optimum condition is: knockout drum pressure at different levels are identical or reduce step by step, and identical or slow step by step liter of temperature resolved the target extract that obtains different components in each grade knockout drum.
In the supercritical extraction process of said method, preferably one of following solvent or its combination of extraction entrainer: absolute ethyl alcohol, hydrous ethanol, propyl alcohol, isopropyl alcohol, butanols, acetone, ethyl acetate, acetonitrile.Supercritical carbon dioxide is a non-polar solven, can regulate its polarity by adding the different extraction entrainer of polarity, improves the solubility of target extracting substance in supercritical carbon dioxide.The choice criteria of extraction entrainer is the solvent of its volatility between supercritical solvent and target extracting substance, selects the solvent that has the excellent dissolution performance as mentioned above usually for use.
In said method, the raw material optional usefulness that ends derives from plant Chinese mugwort, the Chinese mugwort of composite family, and at the local congener that uses as Chinese mugwort: end in Korea Chinese mugwort, mugwort wormwood artemisia, wide leaf mountain wormwood artemisia, red sufficient wormwood artemisia, southern argy wormwood, Herba Artemisiae mongolicae, May, stalwart wormwood artemisia and qi stem wormwood artemisia, the available part of raw material Chinese mugwort comprises the aerial part of plant, based on tarragon, Chinese mugwort stem etc. also can use.It is to adopt heated-air drying 0.5～5.0h of 30～60 ℃ that the drying of raw material Chinese mugwort is handled, and can remove residual moisture content in the raw material Chinese mugwort so as early as possible, and reduces the loss of active principle in the raw material Chinese mugwort.And the break process of raw material Chinese mugwort is with the available part chopping of raw material Chinese mugwort or is crushed to fragment or the velvet-like thing that particle diameter is 0.1～5mm, so that it fully contacts the efficient of raising supercritical extract with CO 2 fluid.
The invention has the advantages that:
1) adopt CO 2 fluid to be in the active principle in the extraction feed Chinese mugwort under high density that supercriticality has, the low viscosity condition at it, can extract Chinese mugwort volatile oil selectively, by the method for step-down solvent and solute are separated, the cycle of its production Chinese mugwort volatile oil is short, efficient is high again.
2) the employing supercritical carbon dioxide fluid can extract the volatile oil in the raw material Chinese mugwort under the cryogenic conditions of gentleness, entire work process is shrouded in high-pressure sealed carbon dioxide inert environments, can prevent from effectively the to end oxidation and the degraded of volatile oil, the extraction that is suitable for the thermal sensitivity active principle of high in the volatile argyi leaf oil, mid-boiling point especially separates.
3) utilize the control of temperature and pressure to make the Chinese mugwort active principle precipitation that is dissolved in the supercritical carbon dioxide fluid and separate, do not need to use chemical organic solvent, so no solvent residue in the gained Chinese mugwort volatilization wet goods active principle, environmentally safe, nonhazardous, and capable of reducing energy consumption.
4) for same Chinese mugwort raw material, it only is 0.6% that steam distillation extracts 5 hours recovery rates, take turns extraction, separation process and adopt this method can in 0.5～16 hour, finish one, Chinese mugwort volatile oil gets recovery rate and can reach more than 1.5%, and medicinal active principle wherein is also than adopting the corresponding raising of steam distillation.
5) this method treasury is got, separation of double acts on one, the phase transition process that does not have material, do not need the high temperature heating, need not reclaim solvent, easy to operate, simplified technological process greatly, saved energy consumption, reduced cost, and production safety is reliable, a kind of desirable Chinese mugwort active principle extraction separating method of can yet be regarded as.
Description of drawings
Accompanying drawing is the complete set of equipments connection diagram of the method for enforcement supercritical carbon dioxide extracting Chinese mugwort of the present invention active principle.
The specific embodiment
Be described in further detail below in conjunction with the method for accompanying drawing supercritical carbon dioxide extracting Chinese mugwort active principle of the present invention:
Supercritical carbon dioxide extracting complete set of equipments shown in the figure comprises the carbon dioxide steel cylinder 1 that is connected by pipeline successively, liquid carbon dioxide condensation basin 2, high-pressure pump 3, heat exchanger 4, extractor 5, one-level knockout drum 6, secondary knockout drum 7, three grades of knockout drums 8.Input at heat exchanger 4 is connected to entrainer pump 13 in addition.Be respectively equipped with one-level knockout drum bleeder valve 9, secondary knockout drum bleeder valve 10, three grades of knockout drum bleeder valves 11 in one, two, three knockout drum 6,7,8 lower ends.On extractor 5 and one, two, three knockout drum 6,7,8, be respectively equipped with Pressure gauge P1～P4.On the return of three grades of knockout drums 8 and liquid carbon dioxide condensation basin 2, be provided with flowmeter 12.This complete set of equipments also is provided with not shown thermometer, refrigerant condenser, automation control system and various pipelines etc.
During the invention process, get pre-dry tarragon and suitably shred or be crushed to fragment or the velvet-like thing that particle diameter is 0.1～5mm, in the extractor 5 of packing into, airtight.By the temperature of automation control system, open heating power supply separately by required condition enactment extractor 5, one-level knockout drum 6 or the above knockout drum 7,8 of one-level.Open valve then, carbon dioxide in the steel cylinder 1 is entered in the liquid carbon dioxide condensation basin 2, enter in the heat exchanger 4 by high-pressure pump 3 pressurizations, the extraction entrainer can enter extractor 5 by in entrainer pump 13 delivery heat exchangers 4 after heat exchanger 4 mixes, heats up.In extractor 5, extracting pressure is that 7～50Mpa, extraction temperature are that 20～70 ℃ supercritical carbon dioxide fluid fully contacts with raw material Chinese mugwort fragment or velvet-like thing through the type of flow forward or backwards, and volatile oil and other active principle in the raw material Chinese mugwort are dissolved in the CO 2 fluid.The CO 2 fluid that has dissolved volatilization wet goods active principle imports in the above knockout drum 6～8 of one-level or one-level again and carries out decompression separation, the pressure of one-level knockout drum 6 is 4～15MPa, the pressure of secondary and above knockout drum 7,8 is 2～12Mpa, the temperature of knockout drums at different levels is 22～80 ℃, the pressure of preferred knockout drums at different levels keeps identical or reduces step by step, and temperature then keeps identical or slow step by step and rises.In separation processes at different levels, Blumea oil and other active principle are separated successively by the ascending order of solubility, discharge from knockout drum bleeder valves 9,10,11 at different levels.CO 2 fluid after the parsing is returned in the liquid carbon dioxide condensing basin 2 by pipeline behind flowmeter 12, realizes recycling.After extraction finished, termination of pumping was carried out all pressing in the system, and remaining carbon dioxide in the discharging extractor 5 is opened extractor 5 and taken out residue, and purging system is in order to using next time.
Further specifically describe several preferred embodiments below again:
Embodiment 1: 1kg is dropped in the extractor through heated-air drying, the tarragon fragment that is chopped into 3mm, is that 16Mpa, temperature are to carry out supercritical carbon dioxide extracting under 45 ℃ the condition at pressure.Regulating one-level knockout drum pressure is 7MPa, temperature is 45 ℃, secondary knockout drum pressure is 5MPa, temperature is 50 ℃, carbon dioxide flow is 30kg/h, through extraction in 4 hours, can obtain Blumea oil 25.6g from the one-level knockout drum, obtain Blumea oil mixture 2.7g in the secondary knockout drum, total recovery rate is 2.83%.
Embodiment 2: the tarragon fragment of 1kg through drying in the shade, be chopped into 1mm dropped in the extractor, is that 25Mpa, temperature are to carry out supercritical carbon dioxide extracting under 35 ℃ the condition at pressure.Regulating one-level knockout drum pressure is 10MPa, temperature is 40 ℃, and secondary knockout drum pressure is 6MPa, and temperature is 50 ℃, three grades are separated pressure tank is 4MPa, temperature was 50 ℃, and carbon dioxide flow is 15kg/h, through extraction in 2 hours, can from the one-level knockout drum, obtain Blumea oil 17.2g, obtain Blumea oil mixture 2.9g in the secondary knockout drum, obtain Blumea oil mixture 0.6g in three grades of knockout drums, total recovery rate is 2.07%.
Embodiment 3: 1kg is dropped in the extractor through the velvet-like thing of the tarragon of drying, be ground into 0.5mm, is that 20Mpa, temperature are to carry out supercritical carbon dioxide extracting under 40 ℃ the condition at pressure, and the extraction entrainer adopts 95% ethanol 100g.Regulating one-level knockout drum pressure is 8MPa, temperature is 45 ℃, secondary knockout drum pressure is 5MPa, temperature is 50 ℃, carbon dioxide flow is 10kg/h, through extraction in 1 hour, can obtain Blumea oil 23.9g from the one-level knockout drum, obtain Blumea oil mixture 2.5g in the secondary knockout drum, total recovery rate is 2.64%.
Embodiment 4: 1kg is dropped in the extractor through the velvet-like thing of the tarragon of drying in the shade, be ground into 0.1mm, is 10MPa at pressure, and temperature is to extract under 50 ℃ the condition, and the extraction entrainer adopts absolute ethyl alcohol 100g.Regulating one-level knockout drum pressure is 6MPa, temperature is 50 ℃, and secondary knockout drum pressure is 4MPa, and temperature is 50 ℃, three grades are separated pressure tank is 4MPa, temperature was 50 ℃, and carbon dioxide flow is 30kg/h, through extraction in 10 hours, can from the one-level knockout drum, obtain Blumea oil 16.7g, obtain Blumea oil mixture 2.1g in the secondary knockout drum, obtain Blumea oil mixture 0.7g in three grades of knockout drums, total recovery rate is 1.95%.
Claims (6)
1. the method for supercritical carbon dioxide extracting Chinese mugwort active principle, it is characterized in that: this method is earlier the raw material Chinese mugwort to be carried out drying to handle, then that the raw material of drying Chinese mugwort is broken or be ground into fragment or velvet-like thing, again it is carried out supercritical carbon dioxide extracting, at last the carbon dioxide that contains the target extract is carried out one-level or the parsing of the decompression more than one-level separation, carbon dioxide after the separation continues to participate in the supercritical extract circulation, the component that parses is the Chinese mugwort active principle: wherein: in the described supercritical extraction process, adopt supercritical carbon dioxide endless form extraction forward or backwards Chinese mugwort active principle, the mass ratio of per hour the circulate consumption and the extraction entrainer consumption of raw material Chinese mugwort consumption and extractant carbon dioxide is followed successively by 1: 10～30: 0～0.2, extracting pressure is 10～25MPa, extraction temperature is 35～55 ℃, and the extraction time is 1～10h; The above decompression of described one-level or one-level is resolved in the separating technology, and one-level knockout drum pressure is 4～15MPa, and secondary and above knockout drum pressure are 2～12Mpa, and knockout drum temperature at different levels are 22～80 ℃.
2. the method for supercritical carbon dioxide extracting Chinese mugwort active principle according to claim 1, it is characterized in that: the above decompression of said one-level or one-level is resolved in the separating technology, knockout drum pressure at different levels are identical or reduce step by step, identical or slow step by step liter of temperature resolved the target extract that obtains different components in each grade knockout drum.
3. the method for supercritical carbon dioxide extracting Chinese mugwort active principle according to claim 1 and 2, it is characterized in that: said raw material Chinese mugwort is selected plant Chinese mugwort, the Chinese mugwort that derives from composite family for use, and at the local congener that uses as Chinese mugwort: end in Korea Chinese mugwort, mugwort wormwood artemisia, wide leaf mountain wormwood artemisia, red sufficient wormwood artemisia, southern argy wormwood, Herba Artemisiae mongolicae, May, stalwart wormwood artemisia and qi stem wormwood artemisia, the available part of raw material Chinese mugwort comprises the aerial part of plant, based on tarragon.
4. the method for supercritical carbon dioxide extracting Chinese mugwort active principle according to claim 1 and 2 is characterized in that: it is to adopt heated-air drying 0.5～5.0h of 30～60 ℃ that said drying to the raw material Chinese mugwort is handled.
5. the method for supercritical carbon dioxide extracting Chinese mugwort active principle according to claim 1 and 2 is characterized in that: said break process to the raw material Chinese mugwort is with the available part chopping of raw material Chinese mugwort or is crushed to fragment or the velvet-like thing that particle diameter is 0.1～5mm.
6. the method for supercritical carbon dioxide extracting Chinese mugwort active principle according to claim 1 and 2, it is characterized in that: in the said supercritical extraction process, the extraction entrainer is selected one of following solvent or its combination for use: absolute ethyl alcohol, hydrous ethanol, propyl alcohol, isopropyl alcohol, butanols, acetone, ethyl acetate, acetonitrile.
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