CN103695161B - Method for extracting cinnamomum micranthum hagata oil by using supercritical carbon dioxide and cinnamomum micranthum hagata oil - Google Patents
Method for extracting cinnamomum micranthum hagata oil by using supercritical carbon dioxide and cinnamomum micranthum hagata oil Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 50
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 229910002092 carbon dioxide Inorganic materials 0.000 title abstract description 6
- 239000001569 carbon dioxide Substances 0.000 title abstract description 6
- 241000386860 Cinnamomum micranthum Species 0.000 title abstract 8
- IGODOXYLBBXFDW-UHFFFAOYSA-N alpha-Terpinyl acetate Chemical compound CC(=O)OC(C)(C)C1CCC(C)=CC1 IGODOXYLBBXFDW-UHFFFAOYSA-N 0.000 claims abstract description 12
- RRAFCDWBNXTKKO-UHFFFAOYSA-N eugenol Chemical compound COC1=CC(CC=C)=CC=C1O RRAFCDWBNXTKKO-UHFFFAOYSA-N 0.000 claims abstract description 12
- CDOSHBSSFJOMGT-UHFFFAOYSA-N linalool Chemical compound CC(C)=CCCC(C)(O)C=C CDOSHBSSFJOMGT-UHFFFAOYSA-N 0.000 claims abstract description 7
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- LFJQCDVYDGGFCH-SNVBAGLBSA-N (+/-)-beta-Phellandrene Natural products CC(C)[C@H]1CCC(=C)C=C1 LFJQCDVYDGGFCH-SNVBAGLBSA-N 0.000 claims abstract description 6
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Abstract
The invention relates to a method for extracting cinnamomum micranthum hagata oil by using supercritical carbon dioxide and the cinnamomum micranthum hagata oil. The cinnamomum micranthum hagata oil comprises the following components by weight: 25 to 30 percent of cineole, 23 to 25 percent of terpinyl acetate, 13 to 15 percent of linalool, 12 to 13 percent of isoeugenol methyl ether, 5 to 7 percent of alpha-terpineol, 3 to 5 percent of eugenol, 2 to 4 percent of beta-phellandrene, 3 to 5 percent of alpha-cadinene and 2 to 4 percent of geraniolene. The method and the cinnamomum micranthum hagata oil have the advantages that the method is simple, convenient to implement and control and low in production cost, damage to active ingredients of the cinnamomum micranthum hagata oil, organic solvent residues and harm to human bodies and the environment are avoided, and the obtained cinnamomum micranthum hagata oil is purely natural and pollution-free.
Description
Technical field
The invention belongs to technical field of fine, be specifically related to a kind of separation and purification of effective ingredients in plant, particularly a kind of method of supercritical carbon dioxide extraction fragrant cassia oil and fragrant cassia oil.
Background technology
Fragrant osmanthus is canella, evergreen dungarunga, and up to more than 9m, tree crown is avette, and sprig is green, and complete stool has fragrance.Leaf alternate, keratin, wide lanceolar, marginal wavy, has sweet-smelling.Unisexual flower, dioecy, umbel clusters between axil, and little Hua is faint yellow.Drupe ellipticity is spherical, is puce time ripe.Four months florescences, nine months phases of fruit.Fragrant cassia twig leaf can extract and obtain essential oil.Fragrant cassia oil is a kind of weak yellow liquid with special aroma and slightly pungent taste, and a little as cinnamon essential oil, volatility is fast.To weak base and organic acid quite stable, can be dissolved in peruscabin, diethyl phthalate with any ratio; Dissolve in mineral oil and propylene glycol, but present opalescence; Be insoluble to G & W.It can be widely used in pharmaceutical raw material, pharmaceutical aids, health-care food raw material, daily use chemicals raw material, cosmetic material, essence and flavoring agent raw material etc.; Fragrant cassia oil all has production in Israel, Lebanon, Turkey, Former Yugoslavia area, Russia, Italy, Spain, France, Morocco, Pakistan, but it is all little to be subject to proposing limiting output of technique, world's annual production 4-18t.China due to cultivated area little, there is no scale production quantities.Extraction at present for fragrant cassia oil is generally: steam distillation and organic solvent extractionprocess, wherein utilize water vapor extract fragrant cassia oil also exist oil yield low, be generally 0.5%-2.0%, cost is high, production temperature is higher, heat-sensitive substance in fragrant cassia oil is oxidizable and loss, and the effective constituent of fragrant cassia oil destroys serious problem; And adopt organic solvent to carry out extracting and also exist that the fragrant cassia oil obtained can not ensure pure natural, it remains organic solvent, the problem larger to the harm of human body and environment.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art and provide a kind of production method simple, be convenient to implement and control, production cost is low, the effective constituent of fragrant cassia oil can not be destroyed, can not residual organic solvent, to human body and environment fanout free region, method and the fragrant cassia oil of the non-harmful supercritical carbon dioxide extraction fragrant cassia oil of fragrant cassia oil pure natural obtained can be ensured.
Technical solution of the present invention is:
A method for supercritical carbon dioxide extraction fragrant cassia oil, the method comprises the steps:
Step 1: fragrant osmanthus leaf of gathering in the morning of summer, Qiu Liangji, puts into bamboo basket, stand lamellar, at room temperature dry in the shade 12-16 days, keeps fragrant osmanthus leaf naturally green, the fragrant osmanthus leaf of removing browning look and black and impurity in the process of drying in the shade, put into the airtight preservation of clean container, for subsequent use;
Step 2: get step 1 and process the fragrant osmanthus leaf obtained and send into pulverizer and pulverize and obtain fragrant cassia leaf powder, controlling powder particle diameter is 20-40 order, for subsequent use;
Step 3: get the fragrant cassia leaf powder that step 2 obtains and insert in extraction kettle, and add ethanol as entrainment agent in extraction kettle, the add-on of ethanol is: the fragrant cassia leaf powder of every 100g adds 200mL ethanol;
Step 4: pass into carbonic acid gas with the flow velocity of 5-10L/h in extraction kettle, the temperature controlling extraction kettle is 40 DEG C-50 DEG C, pressure is 10-30MPa, and extract, the time of extraction is 60-120 minute, obtains fragrant osmanthus leaf extract;
Step 5: fragrant osmanthus leaf extract step 4 obtained is inserted in separating still, the pressure controlled in separating still is 10-12MPa, temperature 40 DEG C-50 DEG C, removes the wax component in the leaf extract of fragrant osmanthus, namely obtains fragrant cassia oil.
The add-on of described fragrant cassia leaf powder is: often liter of extraction kettle volume adds 80-150 gram of fragrant cassia leaf powder.
Described ethanol adopts volume fraction to be the ethanol of 95%.
The method of supercritical carbon dioxide extraction fragrant cassia oil extracts the fragrant cassia oil obtained, and it comprises each component accounting for following weight percentage: eucalyptol 25-30%, terpinyl acetate 23-25%, phantol 13-15%, isoeugenol methyl ether 12-13%, α-terpinol 5-7%, Eugenol 3-5%, β-phellandrene 2-4%, α-cadinene 3-5%, bicyclogermacrene 2-4%.
The present invention has the following advantages:
1) the present invention adopts the method extraction fragrant cassia oil of supercritical extraction, and production method is extracted under shrouding close to room temperature and carbonic acid gas, effectively prevent oxidation and the loss of the heat-sensitive substance in the leaf of fragrant osmanthus; Make fragrant cassia oil can remain the effective constituent of medicinal plant, and the material of high boiling point, low volatility, easily pyrolysis can be extracted under far below its boiling temperature; 2) because whole process is without organic solvent, the therefore vehicle substance that absolutely not remains of extract, thus prevent in leaching process the existence that produces harmful thing and the pollution to environment, ensure that the pure natural property of 100%; 3) extraction and fractionation unites two into one, when the CO 2 fluid of saturated solute enters separator, due to the decline of pressure or the change of temperature, carbonic acid gas and extract is made to become rapidly two-phase (gas-liquid separation) and separate immediately, the efficiency not only extracted is high but also energy consumption is less, improves production efficiency and also reduces expense cost; 4) carbonic acid gas is a kind of inactive gas, chemical reaction does not occur in extraction process, and tasteless, odorless, nontoxic, security is very good; 5) carbon dioxide low price, purity is high, easily produces, and can recirculation use aborning, thus significantly reduces cost; 6) in production method of the present invention, pressure and temperature, as the controling parameters regulating extraction process, reaches the object of extraction by changing temperature and pressure, is separated by fragrant cassia oil by change temperature or pressure; Technique is simply easily grasped, be convenient to implement and promote and extraction speed fast; 7) oil yield of the present invention is very high, and extraction time is shorter, facts have proved, oil yield of the present invention is 9-11%, extraction time is 60-120 minute.
The conventional purposes of fragrant cassia oil is as follows:
Fragrant cassia oil is pharmaceutically for sterilization, sterilization; Test shows, with fragrant cassia oil dip-coating 2cm diameter circle filter paper, lets alone volatilization in plate, and ware covers and adds rhinovirus 17 type diluent 0.02ml(containing sick 100TCID50), namely 33 DEG C of contacts have killing action in 60 minutes.Contact 30 minutes with rhinovirus on meche 17 type, influenza virus A3-elder brother army 75-five strain, adenovirus type VII, 60 minutes and 120 minutes, obvious with the effect contacting more than 60 minutes, human fetal trachea block is added 0.2ml rhinovirus 17 type 100 ~ 1000TCID50, adsorb 30 minutes, 90 minutes are contacted with the gas of fragrant cassia oil (dip-coating is in 2cm diameter circle filter paper) performance, can kill virus.As absorption is extended more than 3h, volatile oil then can not kill virus completely.Point out thus, have fractionated viral to invade in the cell of tracheae block, volatile oil then can not enter in cell.To people with fragrant cassia oil tannic acid preparation collunarium, and with tannic acid in contrast, show that this volatile oil has effect of the preventing cold of short-term, without side reaction.Fragrant cassia oil or pharmaceutical raw material and pharmaceutical aids: its nature and flavor: warm, pungent, effect: brain tonic, and stomach, ease constipation, relieving the exterior syndrome by diaphoresis, anti-inflammatory analgetic, stomach invigorating is regulated the flow of vital energy.Stomachache that main gastral cavity is swollen; Injury from falling down; Mange.Have to Digestive tract benefiting of showing, can help to open appetite, deswelling gas of dispelling, pacify stomachache, and nourishing liver, invigorating kidney, promote urine flowing.In addition, effect that fragrant osmanthus leaf is used in communicable disease is distinguished, may also contribute to treating bronchitis.Fragrant cassia oil can be used as pain killer, antineuralgic, antiseptic-germicide, Anticonvulsants, aperitive, astringent matter, promotion choleresis medicine, diuretic(s), emmenagogue, febricide, sharp liver agent, sterilant, practise midwifery agent, stimulant, sudorific, nourishing agent etc.
fragrant cassia oil has slight anaesthetic effect, makes soul be tending towards warm calmness.No matter be rheumatalgia, general pain or sprain, fragrant osmanthus leaf all has the effect of mitigation symptoms, is especially in harmonious proportion when using with rose, needle juniper.Also can nurse one's health reproductive system, the menstruation that adjust flux is very few, and stages of labor can be accelerated when producing.Also sb.'s illness took a favorable turn to help ear infections, and then alleviate dizzy sensation, restores balance.Simultaneously or the good tonic of hair and scalp, can stimulating hair growth remove dandruff.Allegedly also can break up extravasated blood, pacify inflammation, and reduce the scope scabbed.In addition, no matter somatosensory is crossed cold or overheated, regulate body temperature effect that fragrant osmanthus is good, can allow health comparatively comfortable.
Fragrant cassia oil is Chang Zuowei aromatic flvouring also, for food flavor(ing).Fragrant osmanthus blade then can be directly used in meat product, particularly as the correctives of canned meat.Though fragrant osmanthus leaf also claims osmanthus leaf, all different from the osmanthus leaf of the osmanthus leaf of xylocinnamomum, osmanthus fragrans, it belongs to western-style food condiment, and can batching, the personal value is far above Chinese cassia tree leaf and Sweet Osmanthus leaf.Fragrant osmanthus leaf is seasoning material very common in Europe, particularly Mediterranean Zone culinary art, and North America and France's culinary art have cuisine to reuse fragrant osmanthus leaf, as being used in soup, meat, vegetables, boiled dinner, seafood and vegetables etc., can say it is a kind of peptic.Directly one-piece blade can be used without cutting when generally cooking, or a few Shu Xianggui leaf connected stem and tie up to be placed in after cooking utensil is conveniently finished in other vanillas and removed, because general menu is required of the fragrance of fragrant osmanthus leaf but not taste, it is pungent too fierce for a person sponging on an aristocrat, chopping or the fragrant osmanthus leaf of claying into power discharge more fragrance than the blade without cutting, the fragrant osmanthus leaf of chopping is more difficult to remove from dish, sees gauze tea bag.The fragrant osmanthus leaf ground just need not remove after cooking.Fragrant osmanthus leaf is common in again the cuisine that India and the fragrant meal of Pakistani baking and other fragrance very enrich, and the formula of some India's curry powder also has the fragrant osmanthus leaf comprising and clay into power.Fragrant osmanthus leaf can become scattered about on dessert various addicted to sweet insect in order to drive away.
Fragrant cassia oil can be extracted the chemical material as perfume.Be applicable to be in harmonious proportion with it essential oil cdear, coriander, eucalyptus globolus, ginger, needle juniper, lavandula angustifolia, lemon, marjoram, sweet orange, rose, Rosmarinus officinalis, Thymus vulgaris, Yilan.
Embodiment
Below in conjunction with embodiment, the present invention is further illustrated.
Embodiment 1
A method for supercritical carbon dioxide extraction fragrant cassia oil, the method comprises the steps:
Step 1: fragrant osmanthus leaf of gathering in the morning of summer, Qiu Liangji, puts into bamboo basket, stand lamellar, at room temperature dry in the shade 12-16 days, keeps fragrant osmanthus leaf naturally green, the fragrant osmanthus leaf of removing browning look and black and impurity in the process of drying in the shade, put into the airtight preservation of clean container, for subsequent use;
Step 2: get step 1 and process the fragrant osmanthus leaf obtained and send into pulverizer and pulverize and obtain fragrant cassia leaf powder, controlling powder particle diameter is 20 orders, for subsequent use;
Step 3: get the fragrant cassia leaf powder that 200g step 2 obtains and insert in extraction kettle, and add ethanol as entrainment agent in extraction kettle, the add-on of ethanol is 400mL ethanol;
Step 4: pass into carbonic acid gas with the flow velocity of 5L/h in extraction kettle, the temperature controlling extraction kettle is 40 DEG C, pressure is 10MPa, and extract, the time of extraction is 60 minutes, obtains fragrant osmanthus leaf extract;
Step 5: fragrant osmanthus leaf extract step 4 obtained is inserted in separating still, the pressure controlled in separating still is 10MPa, temperature 40 DEG C, and remove the wax component in the leaf extract of fragrant osmanthus, namely obtain fragrant cassia oil, the fragrant cassia oil obtained with balance load-bearing is 18g.
Calculating percentage extraction formula is: percentage extraction=fragrant cassia oil weight (g)/fragrant cassia leaf powder weight (g) × 100 ﹪, can be obtained by above-mentioned formulae discovery: percentage extraction is 9%.
The component of the fragrant cassia oil that analytical extraction obtains obtains: adopt a kind of method of supercritical carbon dioxide extraction fragrant cassia oil to extract the fragrant cassia oil obtained, it comprises each component accounting for following weight percentage: eucalyptol 25%, terpinyl acetate 23%, phantol 13%, isoeugenol methyl ether 12%, α-terpinol 5%, Eugenol 3%, β-phellandrene 2%, α-cadinene 3%, bicyclogermacrene 2%.
The add-on of described fragrant cassia leaf powder is: often liter of extraction kettle volume adds 80-150 gram of fragrant cassia leaf powder.
Described ethanol adopts volume fraction to be the ethanol of 95%.
The purposes of the fragrant cassia oil that the present invention obtains is as follows: pharmaceutically for sterilization, sterilization, fragrant cassia oil or pharmaceutical raw material and pharmaceutical aids; Fragrant cassia oil has slight anaesthetic effect, makes soul be tending towards warm calmness; Fragrant cassia oil is Chang Zuowei aromatic flvouring also, for food flavor(ing).Fragrant cassia oil can be extracted the chemical material as perfume.
The present invention adopts the method extraction fragrant cassia oil of supercritical extraction, and production method is extracted under shrouding close to room temperature and carbonic acid gas, effectively prevent oxidation and the loss of the heat-sensitive substance in the leaf of fragrant osmanthus; Make fragrant cassia oil can remain the effective constituent of medicinal plant, and the material of high boiling point, low volatility, easily pyrolysis can be extracted under far below its boiling temperature; Because whole process is without organic solvent, the therefore vehicle substance that absolutely not remains of extract, thus prevent in leaching process the existence that produces harmful thing and the pollution to environment, ensure that the pure natural property of 100%; Extraction and fractionation unites two into one, when the CO 2 fluid of saturated solute enters separator, due to the decline of pressure or the change of temperature, carbonic acid gas and extract is made to become rapidly two-phase (gas-liquid separation) and separate immediately, the efficiency not only extracted is high but also energy consumption is less, improves production efficiency and also reduces expense cost; Carbonic acid gas is a kind of inactive gas, chemical reaction does not occur in extraction process, and tasteless, odorless, nontoxic, security is very good; Carbon dioxide low price, purity is high, easily produces, and can recirculation use aborning, thus significantly reduces cost; In production method of the present invention, pressure and temperature is as the controling parameters regulating extraction process, reaches the object of extraction by changing temperature and pressure, is separated by fragrant cassia oil by change temperature or pressure; Technique is simply easily grasped, be convenient to implement and promote and extraction speed fast; Oil yield of the present invention is very high, and extraction time is shorter, facts have proved, oil yield of the present invention is 9%, extraction time is 60 minutes.
Embodiment 2
A method for supercritical carbon dioxide extraction fragrant cassia oil, the method comprises the steps:
Step 1: fragrant osmanthus leaf of gathering in the morning of summer, Qiu Liangji, puts into bamboo basket, stand lamellar, at room temperature dry in the shade 12-16 days, keeps fragrant osmanthus leaf naturally green, the fragrant osmanthus leaf of removing browning look and black and impurity in the process of drying in the shade, put into the airtight preservation of clean container, for subsequent use;
Step 2: get step 1 and process the fragrant osmanthus leaf obtained and send into pulverizer and pulverize and obtain fragrant cassia leaf powder, controlling powder particle diameter is 30 orders, for subsequent use;
Step 3: get the fragrant cassia leaf powder that 200g step 2 obtains and insert in extraction kettle, and add ethanol as entrainment agent in extraction kettle, the add-on of ethanol is 400mL ethanol;
Step 4: pass into carbonic acid gas with the flow velocity of 8L/h in extraction kettle, the temperature controlling extraction kettle is 45 DEG C, pressure is 20MPa, and extract, the time of extraction is 90 minutes, obtains fragrant osmanthus leaf extract;
Step 5: fragrant osmanthus leaf extract step 4 obtained is inserted in separating still, the pressure controlled in separating still is 11MPa, temperature 45 C, and remove the wax component in the leaf extract of fragrant osmanthus, namely obtain fragrant cassia oil, the fragrant cassia oil obtained with balance load-bearing is 20g.
Calculating percentage extraction formula is: percentage extraction=fragrant cassia oil weight (g)/fragrant cassia leaf powder weight (g) × 100 ﹪, can be obtained by above-mentioned formulae discovery: percentage extraction is 10%.
The component of the fragrant cassia oil that analytical extraction obtains obtains: adopt a kind of method of supercritical carbon dioxide extraction fragrant cassia oil to extract the fragrant cassia oil obtained, it comprises each component accounting for following weight percentage: eucalyptol 28%, terpinyl acetate 24%, phantol 14%, isoeugenol methyl ether 12.5%, α-terpinol 6%, Eugenol 3.5%, β-phellandrene 3%, α-cadinene 4%, bicyclogermacrene 3%.
The add-on of described fragrant cassia leaf powder is: often liter of extraction kettle volume adds 80-150 gram of fragrant cassia leaf powder.
Described ethanol adopts volume fraction to be the ethanol of 95%.
The purposes of the fragrant cassia oil that the present invention obtains is as follows: pharmaceutically for sterilization, sterilization, fragrant cassia oil or pharmaceutical raw material and pharmaceutical aids; Fragrant cassia oil has slight anaesthetic effect, makes soul be tending towards warm calmness; Fragrant cassia oil is Chang Zuowei aromatic flvouring also, for food flavor(ing).Fragrant cassia oil can be extracted the chemical material as perfume.
The present invention adopts the method extraction fragrant cassia oil of supercritical extraction, and production method is extracted under shrouding close to room temperature and carbonic acid gas, effectively prevent oxidation and the loss of the heat-sensitive substance in the leaf of fragrant osmanthus; Make fragrant cassia oil can remain the effective constituent of medicinal plant, and the material of high boiling point, low volatility, easily pyrolysis can be extracted under far below its boiling temperature; Because whole process is without organic solvent, the therefore vehicle substance that absolutely not remains of extract, thus prevent in leaching process the existence that produces harmful thing and the pollution to environment, ensure that the pure natural property of 100%; Extraction and fractionation unites two into one, when the CO 2 fluid of saturated solute enters separator, due to the decline of pressure or the change of temperature, carbonic acid gas and extract is made to become rapidly two-phase (gas-liquid separation) and separate immediately, the efficiency not only extracted is high but also energy consumption is less, improves production efficiency and also reduces expense cost; Carbonic acid gas is a kind of inactive gas, chemical reaction does not occur in extraction process, and tasteless, odorless, nontoxic, security is very good; Carbon dioxide low price, purity is high, easily produces, and can recirculation use aborning, thus significantly reduces cost; In production method of the present invention, pressure and temperature is as the controling parameters regulating extraction process, reaches the object of extraction by changing temperature and pressure, is separated by fragrant cassia oil by change temperature or pressure; Technique is simply easily grasped, be convenient to implement and promote and extraction speed fast; Oil yield of the present invention is very high, and extraction time is shorter, facts have proved, oil yield of the present invention is 10%, extraction time is 90 minutes.
Embodiment 3
A method for supercritical carbon dioxide extraction fragrant cassia oil, the method comprises the steps:
Step 1: fragrant osmanthus leaf of gathering in the morning of summer, Qiu Liangji, puts into bamboo basket, stand lamellar, at room temperature dry in the shade 12-16 days, keeps fragrant osmanthus leaf naturally green, the fragrant osmanthus leaf of removing browning look and black and impurity in the process of drying in the shade, put into the airtight preservation of clean container, for subsequent use;
Step 2: get step 1 and process the fragrant osmanthus leaf obtained and send into pulverizer and pulverize and obtain fragrant cassia leaf powder, controlling powder particle diameter is 30 orders, for subsequent use;
Step 3: get the fragrant cassia leaf powder that 200g step 2 obtains and insert in extraction kettle, and add ethanol as entrainment agent in extraction kettle, the add-on of ethanol is 400mL ethanol;
Step 4: pass into carbonic acid gas with the flow velocity of 10L/h in extraction kettle, the temperature controlling extraction kettle is 50 DEG C, pressure is 30MPa, and extract, the time of extraction is 120 minutes, obtains fragrant osmanthus leaf extract;
Step 5: fragrant osmanthus leaf extract step 4 obtained is inserted in separating still, the pressure controlled in separating still is 12MPa, temperature 50 C, and remove the wax component in the leaf extract of fragrant osmanthus, namely obtain fragrant cassia oil, the fragrant cassia oil obtained with balance load-bearing is 22g.
Calculating percentage extraction formula is: percentage extraction=fragrant cassia oil weight (g)/fragrant cassia leaf powder weight (g) × 100 ﹪, can be obtained by above-mentioned formulae discovery: percentage extraction is 11%.
The component of the fragrant cassia oil that analytical extraction obtains obtains: adopt a kind of method of supercritical carbon dioxide extraction fragrant cassia oil to extract the fragrant cassia oil obtained, it comprises each component accounting for following weight percentage: eucalyptol 30%, terpinyl acetate 25%, phantol 15%, isoeugenol methyl ether 13%, α-terpinol 7%, Eugenol 5%, β-phellandrene 4%, α-cadinene 5%, bicyclogermacrene 4%.
The add-on of described fragrant cassia leaf powder is: often liter of extraction kettle volume adds 80-150 gram of fragrant cassia leaf powder.
Described ethanol adopts volume fraction to be the ethanol of 95%.
The purposes of the fragrant cassia oil that the present invention obtains is as follows: pharmaceutically for sterilization, sterilization, fragrant cassia oil or pharmaceutical raw material and pharmaceutical aids; Fragrant cassia oil has slight anaesthetic effect, makes soul be tending towards warm calmness; Fragrant cassia oil is Chang Zuowei aromatic flvouring also, for food flavor(ing).Fragrant cassia oil can be extracted the chemical material as perfume.
The present invention adopts the method extraction fragrant cassia oil of supercritical extraction, and production method is extracted under shrouding close to room temperature and carbonic acid gas, effectively prevent oxidation and the loss of the heat-sensitive substance in the leaf of fragrant osmanthus; Make fragrant cassia oil can remain the effective constituent of medicinal plant, and the material of high boiling point, low volatility, easily pyrolysis can be extracted under far below its boiling temperature; Because whole process is without organic solvent, the therefore vehicle substance that absolutely not remains of extract, thus prevent in leaching process the existence that produces harmful thing and the pollution to environment, ensure that the pure natural property of 100%; Extraction and fractionation unites two into one, when the CO 2 fluid of saturated solute enters separator, due to the decline of pressure or the change of temperature, carbonic acid gas and extract is made to become rapidly two-phase (gas-liquid separation) and separate immediately, the efficiency not only extracted is high but also energy consumption is less, improves production efficiency and also reduces expense cost; Carbonic acid gas is a kind of inactive gas, chemical reaction does not occur in extraction process, and tasteless, odorless, nontoxic, security is very good; Carbon dioxide low price, purity is high, easily produces, and can recirculation use aborning, thus significantly reduces cost; In production method of the present invention, pressure and temperature is as the controling parameters regulating extraction process, reaches the object of extraction by changing temperature and pressure, is separated by fragrant cassia oil by change temperature or pressure; Technique is simply easily grasped, be convenient to implement and promote and extraction speed fast; Oil yield of the present invention is very high, and extraction time is shorter, facts have proved, oil yield of the present invention is 11%, extraction time is 120 minutes.
Claims (3)
1., by a method for supercritical carbon dioxide extraction fragrant cassia oil, it is characterized in that: the method comprises the steps:
Step 1: fragrant osmanthus leaf of gathering in the morning of summer, Qiu Liangji, puts into bamboo basket, stand lamellar, at room temperature dry in the shade 12-16 days, keeps fragrant osmanthus leaf naturally green, the fragrant osmanthus leaf of removing browning look and black and impurity in the process of drying in the shade, put into the airtight preservation of clean container, for subsequent use;
Step 2: get step 1 and process the fragrant osmanthus leaf obtained and send into pulverizer and pulverize and obtain fragrant cassia leaf powder, controlling powder particle diameter is 20-40 order, for subsequent use;
Step 3: get the fragrant cassia leaf powder that step 2 obtains and insert in extraction kettle, and add ethanol as entrainment agent in extraction kettle, the add-on of ethanol is: the fragrant cassia leaf powder of every 100g adds 200mL ethanol;
Step 4: pass into carbonic acid gas with the flow velocity of 5-10L/h in extraction kettle, the temperature controlling extraction kettle is 40 DEG C-50 DEG C, pressure is 10-30MPa, and extract, the time of extraction is 60-120 minute, obtains fragrant osmanthus leaf extract;
Step 5: fragrant osmanthus leaf extract step 4 obtained is inserted in separating still, the pressure controlled in separating still is 10-12MPa, temperature 40 DEG C-50 DEG C, removes the wax component in the leaf extract of fragrant osmanthus, namely obtains fragrant cassia oil;
Described ethanol adopts volume fraction to be the ethanol of 95%.
2. the method for a kind of supercritical carbon dioxide extraction fragrant cassia oil as claimed in claim 1, is characterized in that: the add-on of described fragrant cassia leaf powder is: often liter of extraction kettle volume adds 80-150 gram of fragrant cassia leaf powder.
3. the method for a kind of supercritical carbon dioxide extraction fragrant cassia oil as claimed in claim 1 extracts the fragrant cassia oil obtained, and it is characterized in that: it comprises each component accounting for following weight percentage: eucalyptol 25-30%, terpinyl acetate 23-25%, phantol 13-15%, isoeugenol methyl ether 12-13%, α-terpinol 5-7%, Eugenol 3-5%, β-phellandrene 2-4%, α-cadinene 3-5%, bicyclogermacrene 2-4%.
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| 超临界CO2萃取桂枝中桂皮醛的研究;岳红坤等;《石家庄学院学报》;20100531;第12卷(第3期);第36页倒数第3段、第37页第2段 * |
| 香桂桂皮精油的超临界CO2萃取及其GC-MS分析;陈建华等;《中国调味品》;20130930;第38卷(第9期);全文 * |
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Address after: Located in Henan province Zhengzhou City 450000 middle road Yang Newton international A block 13 layer Co-patentee after: TIANJIN TIANXU FOREST SEEDS Co.,Ltd. Patentee after: Henan Hongfeng biological high tech Limited by Share Ltd Address before: Located in Henan province Zhengzhou City 450000 middle road Yang Newton international A block 13 layer Co-patentee before: TIANJIN TIANXU FOREST SEEDS Co.,Ltd. Patentee before: HENAN HOFUNG SEED Co.,Ltd. |
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