CN105296143A - Preparation method of artemisia argyi essential oil - Google Patents
Preparation method of artemisia argyi essential oil Download PDFInfo
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- CN105296143A CN105296143A CN201510878581.3A CN201510878581A CN105296143A CN 105296143 A CN105296143 A CN 105296143A CN 201510878581 A CN201510878581 A CN 201510878581A CN 105296143 A CN105296143 A CN 105296143A
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Abstract
The invention relates to a preparation method of artemisia argyi essential oil. The preparation method comprises the steps of carrying out physical smashing to obtain crude artemisia argyi powder; carrying out enzymolysis treatment to obtain fine artemisia argyi powder; then, carrying out supercritical CO2 extraction and oil-gas separation to obtain the artemisia argyi essential oil. The artemisia argyi essential oil extracted by using supercritical CO2 as an extracting agent is low in extraction temperature, so that thermosensitive substances are effectively prevented from being oxidized and dissipated, and the essential and pure components in a stock solution and the essential oil are remained to the maximum extent; according to the preparation method, extraction and separation steps are combined into one step, and CO2 which is in the supercritical state flows out and is rapidly gasified to ensure that gas-liquid separation of CO2 and an extract is rapidly generated and CO2 and the extract are immediately separated, so that the oil yield is high, and the purity of the extract is high; in addition, CO2 belongs to a noncombustible gas and is tasteless, odorless, nontoxic and good in safety, so that the extracted artemisia argyi essential oil is particularly suitable for the fields of medical treatment, sanitation and daily chemical products.
Description
Technical field
The present invention relates to a kind of preparation method of essential oil, be specifically related to a kind of preparation method of argy wormwood essential oil.
Background technology
Argy wormwood (formal name used at school: Artemisiaargyi) also known as perfume (or spice) Chinese mugwort, wormwood, moxa, hold back grass, moxibustion grass or Chinese mugwort etc., belong to composite family, per nnial herb, very extensive in whole nation distribution, except arid is with except extremely frigid zones, have wild from Heilungkiang to Hainan Island.The whole strain of argy wormwood has special aromatic odour, has sleepingly to help the effect of sleeping and recovering from fatigue; The traditional Chinese medical science with all herbal medicine, have Wen Jing, dry, loose cold, hemostasis, anti-inflammatory, relieving asthma, cough-relieving, the effect such as antiabortive, antianaphylaxis.The traditional culture of argy wormwood and our people is lived closely related, the Dragon Boat Festival argy wormwood is placed in family with reach keep away pest heresy, mosquito repellent fly, anti-all kinds of diseases and ailments object make use of the pharmacological property of these excellences of argy wormwood just.In order to explore the source of the excellent pharmacological properties of argy wormwood, modern study utilizes multiple extracting and purifying technology to extract wormwood essential oil, analysis shows to mix matter, flavonoid, lactone other active substance together containing alkaloid, Jiao's property catechol in argy wormwood essential oil, has the multiple advantages such as regulating blood condition, Wen Jing, dispelling cold, pain relieving, antibacterial, anti-inflammatory, relieving cough and reducing sputum, lifting immunizing power.
The method of current extraction essential oil has solvent-extraction process, steam distillation, microwave extraction method, supercritical carbon dioxide extraction method, and wherein, supercritical carbon dioxide extraction method is that one is subject to extensive concern as a kind of emerging technology.Supercritical CO
2be the one of supercutical fluid, specifically refer to that carbonic acid gas is higher than state when critical temperature and emergent pressure (Tc=31.1 DEG C, Pc=7.37MPa), CO at this moment
2the character such as low viscosity high diffusivity can be embodied.Supercritical CO
2the lot of advantages of self, as lower in Tc (304.1K), Pc lower (7.38MPa), nontoxic, tasteless, harmless, easy to operate, this supercutical fluid making it become to be widely used in practical application.Use supercritical CO compared with the other technologies used containing organic solvent
2the product that technology obtains easily is separated, nontoxic, noresidue organic solvent, and CO
2nonflammable safer, solvent can recycle, is suitable for thermolability material, is particularly useful for pharmaceutical industry and foodstuffs industry.Have reaction conditions gentleness, extraction efficiency is high, no solvent residue, can change the advantages such as device parameter flexibly, is that the one extracting essential oil method is well selected, uses supercritical CO at present
2technology has no report to the technique that argy wormwood essential oil extracts.
Summary of the invention
There is provided a kind of preparation method of argy wormwood essential oil for above-mentioned technical problem object of the present invention, the argy wormwood essential oil prepared by the method, oil yield is high, purity is high, biological activity is good.
In order to realize above-mentioned technical object, the present invention by the following technical solutions:
A preparation method for argy wormwood essential oil, described preparation method comprises the following steps:
1) physical pulverization: argy wormwood prophyll is washed immersion 5 ~ 10 minutes in the deionized water of 10 ~ 20 DEG C, pulverized 50 ~ 100 mesh sieves, obtain argy wormwood meal;
2) enzymolysis processing: make magma by the argy wormwood meal of deionized water implantation step 1, slurries a is made after magma being mixed with the enzymolysis solution adding cellulose mycophenolate, and described slurries a is injected reactor, control temperature 40 ~ 60 DEG C, rotating speed 200 ~ 500r/min, keep filtration after 2-3 hour, drying, obtain argy wormwood fine powder;
3) extract: argy wormwood fine powder is added in reactor, is placed in water-bath through reactor, use high-pressure pump to reactor, to pass into CO from the bottom of reactor with the speed of 10 ~ 30ml/min
2, regulate the temperature of reaction system, pressure to preset value, make argy wormwood fine powder static extracting 2 ~ 4 hours in a kettle.;
4) essential oil obtains: keep the service temperature in step 4 and pressure, make CO
2gas passes into from reactor top, opens outlet valve simultaneously, regulates and keeps CO
2take-off rate, argy wormwood essential oil is with CO
2taken out of, argy wormwood essential oil is collected in cooling.
Further, add the aqueous solution of metal-salt in the enzymolysis solution of step 2, described metal-salt is MgCl
2, ZnCl
2, CaCl
2, at least one in NaCl, KCl.
Further, the concentration of described metal-salt in slurries a is 0.3 × 10
-3~ 1.0 × 10
-3mol/L.
Further, the solid obtained after filtering in step 2, obtains argy wormwood fine powder through vacuum lyophilization.
Further, described vacuum drying temperature is-10 DEG C ~-30 DEG C.
Further, in described step 3, reactor reaction system preset pressure is 8 ~ 20MPa, and temperature of reaction is 30 ~ 80 DEG C, and the time reaching preset pressure is 5 ~ 20min.
Further, CO in step 4
2take-off rate be 5 ~ 20ml/min.
Further, after argy wormwood fine powder stops 1 hour in a kettle. in described step 3, use high-pressure pump to inject ethanol in still, then continue to keep static extracting 2 ~ 3 hours.
Further, the ethanol of injection and reactor CO
2mol ratio be 1 ~ 2.5:10 ~ 15.
Further, the static extracting of step 3 keeps stirring 30 ~ 60min early stage, process in keep stirring.
Beneficial effect of the present invention is: the present invention uses supercritical CO
2as the argy wormwood essential oil of extraction agent extraction, low oxidation and the loss effectively preventing heat-sensitive substance of extraction temperature, maintains the consummate and activeconstituents of stoste and essential oil to greatest extent; Extraction and fractionation unites two into one by the present invention, is in the CO of supercritical state
2flow out, gasification makes CO rapidly
2produce gas-liquid separation rapidly with extract and separate immediately, oil yield is high, and extract purity is high, and due to CO
2belong to non-flammable gases, tasteless, odorless, nontoxic, safety performance is good, and the argy wormwood essential oil extracted can be specially adapted to medical treatment, health, daily chemical products field.
Embodiment
Embodiment 1:
A preparation method for argy wormwood essential oil, described preparation method comprises the following steps:
Argy wormwood prophyll is washed immersion 5 minutes in the deionized water of 10 DEG C, pulverized 100 mesh sieves, obtain argy wormwood meal.Deionized water is injected above-mentioned argy wormwood meal and make magma, make slurries a after magma being mixed with the enzymolysis solution adding cellulose mycophenolate, and described slurries a is injected reactor, control temperature 40 DEG C, rotating speed 200r/min, keeps filtration, drying after 2 hours to obtain argy wormwood fine powder; Extraction: add in reactor by argy wormwood fine powder, be placed in water-bath through reactor, uses high-pressure pump to reactor, to pass into CO from the bottom of reactor with the speed of 10ml/min
2, regulate the temperature to 50 DEG C of reaction system, pressure to 8MPa, make argy wormwood fine powder static extracting 2 ~ 4 hours in a kettle.; Keep 50 DEG C, the service temperature of 8MPa and pressure, make CO
2gas passes into from reactor top, opens outlet valve simultaneously, regulates and keeps CO
2take-off rate, argy wormwood essential oil is with CO
2taken out of, argy wormwood essential oil is collected in cooling.
Utilize the argy wormwood essential oil oil yield that in the present embodiment, method is extracted to be 2.1%, obtain light brown transparent essential oil, essential oil fragrance keeps the fragrant icy of the medicine of argy wormwood, the relative density (20/20 DEG C) of this product: 0.9015, specific rotation (20 DEG C) :-4.5; Acid number (mgKOH): 1.7.The essential oil obtained is applied to daily chemical products, and as the preparation of the products such as bathing agents, perfumed soap, Liquid soap, bath mud, antibacterial, sterilization, antianaphylaxis, deodorizing, calm effect are optimized greatly.
Embodiment 2:
A preparation method for argy wormwood essential oil, described preparation method comprises the following steps:
Argy wormwood prophyll is washed immersion 10 minutes in the deionized water of 20 DEG C, pulverized 100 mesh sieves, obtain argy wormwood meal; Deionized water is injected above-mentioned argy wormwood meal and make magma, make slurries a after magma being mixed with the enzymolysis solution adding cellulose mycophenolate, and described slurries a is injected reactor, control temperature 60 DEG C, rotating speed 500r/min, keeps filtration after 3 hours, drying, obtains argy wormwood fine powder; Argy wormwood fine powder is added in reactor, is placed in water-bath through reactor, use high-pressure pump to reactor, to pass into CO from the bottom of reactor with the speed of 30ml/min
2, regulate the temperature to 70 DEG C of reaction system, pressure to 12MPa, make argy wormwood fine powder static extracting 4 hours in a kettle.; Keep 70 DEG C, 12MPa service temperature and pressure, make CO
2gas passes into from reactor top, opens outlet valve simultaneously, regulates and keeps CO
2take-off rate, argy wormwood essential oil is with CO
2taken out of, argy wormwood essential oil is collected in cooling.
Utilize the argy wormwood essential oil oil yield that in the present embodiment, method is extracted to be 2.9%, obtain light brown transparent essential oil, essential oil fragrance keeps the fragrant icy of the medicine of argy wormwood, the relative density (20/20 DEG C) of this product: 0.8946, specific rotation (20 DEG C) :-4.5; Acid number (mgKOH): 1.6.The essential oil obtained is applied to daily chemical products, and as the preparation of the products such as bathing agents, perfumed soap, Liquid soap, bath mud, antibacterial, sterilization, antianaphylaxis, deodorizing, calm effect are optimized greatly.
Embodiment 3:
A preparation method for argy wormwood essential oil, described preparation method comprises the following steps:
Argy wormwood prophyll is washed immersion 10 minutes in the deionized water of 20 DEG C, pulverized 100 mesh sieves, obtain argy wormwood meal; Deionized water is injected above-mentioned argy wormwood meal and make magma, add containing ZnCl in the enzymolysis solution of interpolation cellulose mycophenolate
2the aqueous solution, make slurries a after magma being mixed with the enzymolysis solution that with the addition of metal-salt, control the content of deionized water and make ZnCl
2concentration in slurries a is 0.3 × 0
-3mol/L, injects reactor by described slurries a, control temperature 45 DEG C of rotating speed 300r/min, keeps filtering after 3 hours, and vacuum lyophilization at-10 DEG C, obtains argy wormwood fine powder; Argy wormwood fine powder is added in reactor, is placed in water-bath through reactor, use high-pressure pump to reactor, to pass into CO from the bottom of reactor with the speed of 25ml/min
2, regulate temperature of reaction system 75 DEG C, pressure 15MPa, make argy wormwood fine powder static extracting 2 ~ 4 hours in a kettle.; Keep Buwen's degree 75 DEG C, pressure 15MPa, make CO
2gas passes into from reactor top, opens outlet valve simultaneously, regulates and keeps CO
2flow velocity be 20ml/min, argy wormwood essential oil is with CO
2taken out of, argy wormwood essential oil is collected in cooling.
Utilize the argy wormwood essential oil oil yield that in the present embodiment, method is extracted to be 3.3%, obtain light brown transparent essential oil, essential oil fragrance keeps the fragrant icy of the medicine of argy wormwood, the relative density (20/20 DEG C) of this product: 0.8920, specific rotation (20 DEG C) :-4.5; Acid number (mgKOH): 1.6.The essential oil obtained is applied to daily chemical products, and as the preparation of the products such as bathing agents, perfumed soap, Liquid soap, bath mud, antibacterial, sterilization, antianaphylaxis, deodorizing, calm effect are optimized greatly.
Embodiment 4:
A preparation method for argy wormwood essential oil, described preparation method comprises the following steps:
Argy wormwood prophyll is washed immersion 10 minutes in the deionized water of 20 DEG C, pulverized 100 mesh sieves, obtain argy wormwood meal; Deionized water is injected above-mentioned argy wormwood meal and make magma, add containing CaCl in the enzymolysis solution of interpolation cellulose mycophenolate
2the aqueous solution, make slurries a after magma being mixed with the enzymolysis solution that with the addition of metal-salt, control the content of deionized water and make ZnCl
2concentration in slurries a is 0.5 × 10
-3mol/L, injects reactor by described slurries a, control temperature 45 DEG C of rotating speed 300r/min, keeps filtering after 3 hours, and vacuum lyophilization at-30 DEG C, obtains argy wormwood fine powder; Argy wormwood fine powder is added in reactor, is placed in water-bath through reactor, use high-pressure pump to reactor, to pass into CO from the bottom of reactor with the speed of 25ml/min
2, regulate temperature of reaction system 75 DEG C, pressure 15MPa, static extracting is after 1 hour in a kettle. to make argy wormwood fine powder, and practical high-pressure pump injects ethanol in still, CO in ethanol and reactor
2mol ratio be 1:15; Continuation keeps temperature 75 DEG C, pressure 15MPa static extracting makes CO in 2 hours
2gas passes into from reactor top, opens outlet valve simultaneously, and regulate and keep the flow velocity of CO2 to be 20ml/min, argy wormwood essential oil is with CO
2taken out of, argy wormwood essential oil is collected in cooling.
Utilize the argy wormwood essential oil oil yield that in the present embodiment, method is extracted to be 3.5%, obtain light brown transparent essential oil, essential oil fragrance keeps the fragrant icy of the medicine of argy wormwood, the relative density (20/20 DEG C) of this product: 0.8920, specific rotation (20 DEG C) :-4.4; Acid number (mgKOH): 1.4.The essential oil obtained is applied to daily chemical products, and as the preparation of the products such as bathing agents, perfumed soap, Liquid soap, bath mud, antibacterial, sterilization, antianaphylaxis, deodorizing, calm effect are optimized greatly.
Claims (10)
1. a preparation method for argy wormwood essential oil, is characterized in that: described preparation method comprises the following steps:
Physical pulverization: argy wormwood prophyll is washed immersion 5 ~ 10 minutes in the deionized water of 10 ~ 20 DEG C, pulverized 50 ~ 100 mesh sieves, obtain argy wormwood meal;
Enzymolysis processing: make magma by the argy wormwood meal of deionized water implantation step 1, slurries a is made after magma being mixed with the enzymolysis solution adding cellulose mycophenolate, and described slurries a is injected reactor, control temperature 40 ~ 60 DEG C, rotating speed 200 ~ 500r/min, keep filtration after 2-3 hour, drying, obtain argy wormwood fine powder;
Extraction: add in reactor by argy wormwood fine powder, be placed in water-bath through reactor, uses high-pressure pump to reactor, to pass into CO from the bottom of reactor with the speed of 10 ~ 30ml/min
2, regulate the temperature of reaction system, pressure to preset value, make argy wormwood fine powder static extracting 2 ~ 4 hours in a kettle.;
Essential oil obtains: keep the service temperature in step 4 and pressure, make CO
2gas passes into from reactor top, opens outlet valve simultaneously, regulates and keeps CO
2take-off rate, argy wormwood essential oil is with CO
2taken out of, argy wormwood essential oil is collected in cooling.
2. the preparation method of a kind of argy wormwood essential oil according to claim 1, is characterized in that: the aqueous solution adding metal-salt in the enzymolysis solution of step 2, and described metal-salt is MgCl
2, ZnCl
2, CaCl
2, at least one in NaCl, KCl.
3. the preparation method of a kind of argy wormwood essential oil according to claim 2, is characterized in that: the concentration of described metal-salt in slurries a is 0.3 × 10
-3~ 1.0 × 10
-3mol/L.
4. the preparation method of a kind of argy wormwood essential oil according to claim 1, is characterized in that: the solid obtained after filtering in step 2, obtains argy wormwood fine powder through vacuum lyophilization.
5. the preparation method of a kind of argy wormwood essential oil according to claim 4, is characterized in that: described vacuum drying temperature is-10 DEG C ~-30 DEG C.
6. the preparation method of a kind of argy wormwood essential oil according to claim 1, is characterized in that: in described step 3, reactor reaction system preset pressure is 8 ~ 20MPa, and temperature of reaction is 30 ~ 80 DEG C, the time reaching preset pressure is 5 ~ 20min.
7. the preparation method of a kind of argy wormwood essential oil according to claim 1, is characterized in that: CO in step 4
2take-off rate be 5 ~ 20ml/min.
8. the preparation method of a kind of argy wormwood essential oil according to claim arbitrary in claim 1-7, it is characterized in that: after in described step 3, argy wormwood fine powder stops 1 hour in a kettle., use high-pressure pump to inject ethanol in still, then continue to keep static extracting 2 ~ 3 hours.
9. the preparation method of a kind of argy wormwood essential oil according to claim 8, is characterized in that: the ethanol of injection and reactor CO
2mol ratio be 1 ~ 2.5:10 ~ 15.
10. the preparation method of a kind of argy wormwood essential oil according to claim 1, is characterized in that: the static extracting of step 3 keeps stirring 30 ~ 60min early stage, process in keep stirring.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106833903A (en) * | 2017-03-29 | 2017-06-13 | 董兰田 | Blue or green argy wormwood distillation, sedimentation separation are quenched take Chinese mugwort essential oil method respectively |
| CN107446702A (en) * | 2017-08-12 | 2017-12-08 | 安徽楚艾农业科技有限公司 | A kind of extracting method of wormwood essential oil |
| CN107460057A (en) * | 2017-08-23 | 2017-12-12 | 安徽楚艾农业科技有限公司 | A kind of wormwood essence and preparation method thereof |
| CN107603735A (en) * | 2017-08-23 | 2018-01-19 | 安徽楚艾农业科技有限公司 | A kind of method that promoting blood circulation essence is prepared using wormwood |
| CN109363969A (en) * | 2018-10-08 | 2019-02-22 | 广东暨晴生物医药科技有限公司 | A kind of method of comprehensive utilization of wormwood effective component |
| CN109394584A (en) * | 2018-12-07 | 2019-03-01 | 安阳工学院 | A kind of preparation method of the biennial wormwood extract hand cleanser with antibacterial disinfection efficacy |
| CN110655990A (en) * | 2019-10-08 | 2020-01-07 | 宫鹏 | Preparation method and application of traditional Chinese medicine wormwood essential oil |
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| CN104194917A (en) * | 2014-09-05 | 2014-12-10 | 南京泽朗生物科技有限公司 | Method for extracting folium artemisiae argyi essential oil |
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| CN104194917A (en) * | 2014-09-05 | 2014-12-10 | 南京泽朗生物科技有限公司 | Method for extracting folium artemisiae argyi essential oil |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106833903A (en) * | 2017-03-29 | 2017-06-13 | 董兰田 | Blue or green argy wormwood distillation, sedimentation separation are quenched take Chinese mugwort essential oil method respectively |
| CN107446702A (en) * | 2017-08-12 | 2017-12-08 | 安徽楚艾农业科技有限公司 | A kind of extracting method of wormwood essential oil |
| CN107460057A (en) * | 2017-08-23 | 2017-12-12 | 安徽楚艾农业科技有限公司 | A kind of wormwood essence and preparation method thereof |
| CN107603735A (en) * | 2017-08-23 | 2018-01-19 | 安徽楚艾农业科技有限公司 | A kind of method that promoting blood circulation essence is prepared using wormwood |
| CN107603735B (en) * | 2017-08-23 | 2020-07-17 | 安徽楚艾农业科技有限公司 | Method for preparing blood circulation promoting essence from wormwood |
| CN107460057B (en) * | 2017-08-23 | 2020-07-17 | 安徽楚艾农业科技有限公司 | Wormwood essence and preparation method thereof |
| CN109363969A (en) * | 2018-10-08 | 2019-02-22 | 广东暨晴生物医药科技有限公司 | A kind of method of comprehensive utilization of wormwood effective component |
| CN109394584A (en) * | 2018-12-07 | 2019-03-01 | 安阳工学院 | A kind of preparation method of the biennial wormwood extract hand cleanser with antibacterial disinfection efficacy |
| CN110655990A (en) * | 2019-10-08 | 2020-01-07 | 宫鹏 | Preparation method and application of traditional Chinese medicine wormwood essential oil |
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Application publication date: 20160203 |