CN105853472B - A kind of red shellfish essential oil and preparation method - Google Patents
A kind of red shellfish essential oil and preparation method Download PDFInfo
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- CN105853472B CN105853472B CN201610210975.6A CN201610210975A CN105853472B CN 105853472 B CN105853472 B CN 105853472B CN 201610210975 A CN201610210975 A CN 201610210975A CN 105853472 B CN105853472 B CN 105853472B
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- essential oil
- red shellfish
- organic solvent
- shellfish
- red
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- 235000015170 shellfish Nutrition 0.000 title claims abstract description 56
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- 238000001256 steam distillation Methods 0.000 claims abstract description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 39
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- 239000003921 oil Substances 0.000 claims description 15
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- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
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- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 6
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
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- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 3
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- KMPWYEUPVWOPIM-UHFFFAOYSA-N cinchonidine Natural products C1=CC=C2C(C(C3N4CCC(C(C4)C=C)C3)O)=CC=NC2=C1 KMPWYEUPVWOPIM-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a kind of red shellfish essential oil and preparation methods, the red shellfish essential oil derives from red shellfish E Shi pore fungi Earliella scabrosa (Pers.) Gilb.&Ryvarden of medicinal fungi, red shellfish E Shi pore fungi fructification passes through vacuum rotating steam distillation, the extraction of the organic solvents such as liquid ether is slipped out, ether is recycled after ether extraction liquid is dry up to red shellfish essential oil product.It is analyzed and identified through gas chromatography-mass spectrography, includes 35 kinds of ingredients in red shellfish essential oil, wherein the sum of relative mass degree of the highest 6 kinds of ingredients of content is 70-90%.The present invention specifies the main component in red shellfish E Shi pore fungi fructification essential oil for the first time, it was found that the essential oil is in that fragrant ingredient is unique, it is a kind of new flavors and fragrances, and preparation method of the present invention is simple and practical, it will not make raw material coking due to heating, and extraction time can be shortened, improve extraction of essential oil rate.
Description
Technical field
The present invention relates to a kind of essential oils, more particularly to a kind of red shellfish essential oil and preparation method.
Background technique
Essential oil in Chinese herbal medicine is an active component, has eliminating the phlegm, stomach invigorating, wind dispelling, antipyretic, sharp on clinical treatment
The effects of urine, analgesia, expelling parasite, antibacterial and disinfection.Such as Germacrone, piperitone etc. are the medicines for treating chronic bronchitis
Object, the former antitussive action is obvious, and the latter has anti-asthmatic action, has obvious curative effects to bronchial asthma.Cardamom oil, inulol and peppermint
Oil etc. can be used for dispelling-wind invigorating stomach.Birch Jiao oil, mustard oil, sassafras oil etc. can be used for anti-infective.Pinke needle oil can treat upper respiratory tract sense
Dye.Pine tar, turpentine oil, sandalwood oil etc. have diuresis.Angelica oil has sedation.The antibacterial anti-inflammatory such as eucalyptus oil, caryophyllus oil are made
With obvious, caryophyllus oil or local anesthetic.American wormseed oil can be with expelling parasite.In addition, essential oil is also widely used for food and fragrance
Industry.
In recent years, ganoderma lucidum spore oil is due to being widely used to medicine with antitumor and strengthen immunity and other effects and protecting
Strong product.But higher fungus essential oil does not obtain effective exploitation utilization also but.Red shellfish E Shi pore fungi Earliella scabrosa
(Pers.) Gilb.&Ryvarden fructification is the annual high medicinal fungi of basidiocarps, is distributed in Guangdong, Guangxi, Hainan, cloud
The ground such as south have promoting blood circulation and antipruritic and other effects (Dai Yucheng, scheme youngster Gu Li, Cui Baokai, and state of Qin husband writes " Chinese medicinal fungi figure
Will " Harbin: Northeast forestry publishing house, page 158), but there is presently no artificial domestication cultivations, also without Related product.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of red shellfish essential oils, unique in fragrant ingredient, are a kind of new perfume (or spice)
Smart fragrance can be applied to the fields such as health care product, cosmetics.
In order to solve the above technical problems, the technical scheme is that
A kind of red shellfish essential oil is made from red shellfish E Shi pore fungi fructification, highest 6 kinds of content in the red shellfish essential oil
Chemical component be (R)-(-) -3- methyl -2- butanol, 4- methyl -4- hydroxyl -2 pentanone, azulene, toluene, palmitinic acid and (Z,
Z) -9,12- octadecadienoic acid, the sum of relative mass degree are 70-90%.
Preferably, (R)-(-) -3- methyl -2- butanol in red shellfish essential oil of the present invention, 4- methyl -4- hydroxyl -2- penta
The sum of ketone, azulene, toluene, palmitinic acid and relative mass degree of (Z, Z) -9,12 octadecadienoic acid are
80.66%.
Another technical problem to be solved by the present invention is that providing the preparation method of above-mentioned red shellfish essential oil.
In order to solve the above technical problems, technical solution is:
A kind of preparation method of red shellfish essential oil, comprising the following steps:
(1) air-dried red shellfish E Shi pore fungi fructification is taken, obtains medicinal powder after crushing, medicinal powder is packed into 1000mL constant pressure addition
It is installed in funnel, after compacting in the 500mL round-bottomed flask for being placed with 1-2 zeolites, the suitable for reading of round-bottomed flask is equipped with bulb condensation
Pipe, from spherical condensation tube addition organic solvent suitable for reading, allows organic solvent to flow through medicinal powder and drips from constant pressure in the case where low-temperature circulating water is cooling
Liquid funnel instills in round-bottomed flask, until the volume of organic solvent is the 2/3 of round-bottomed flask volume, closes constant pressure funnel
Cock keeps the liquid level of organic solvent in constant pressure funnel to be more than medicinal powder and does not flow out from branch pipe, added with controllable temperature electric jacket
Heat makes the organic solvent boiling in round-bottomed flask, and the heating temperature of control controllable temperature electric jacket is 50 DEG C, organic solvent vapor from
The branch pipe of constant pressure funnel rises to spherical condensation tube, becomes organic solvent drop after low-temperature circulating water is cooling and instills perseverance
It presses in dropping funel, the cock for unscrewing constant pressure funnel makes the organic solvent drop instilled in constant pressure funnel and instills
Liquid drop speed in round-bottomed flask is consistent, and continuous backflow seepage pressure effects lead to until the drop instilled in round-bottomed flask is colourless
Coarse-fine oil is obtained after crossing distilling apparatus recycling organic solvent；
(2) distilled water is added into the coarse-fine oil that step (1) obtains, using vacuum rotary evaporator, in low-temperature circulating water
Under cooling, with heating water bath, vacuum rotating steam distillation collects distillate until no distillate；
(3) add solid sodium chloride into the distillate that step (2) are collected until saturation is closed with organic solvent extraction 3-5 times
And organic solvent extract liquor, then with filtering after desiccant dryness, filtrate obtains red shellfish essence after organic solvent is recovered by distillation
Oil.
Preferably, the matter of the red shellfish E Shi pore fungi fructification in step (1) of the present invention and the distilled water in step (2)
Amount is than being 1:3.
Preferably, the temperature of step (1) of the present invention and the low-temperature circulating water in (2) is 10-20 DEG C.
Preferably, the organic solvent in step (1) of the present invention and (3) is petroleum ether, ether, pentane, hexane, third
One of or several mixture in ketone, chloroform.
Preferably, in step (2) of the present invention, the temperature of heating water bath is 90-100 DEG C.
Preferably, in step (3) of the present invention, desiccant be anhydrous magnesium sulfate, anhydrous sodium sulfate, anhydrous calcium chloride,
One of which in silica gel, molecular sieve.
Preferably, in step (3) of the present invention, the volume ratio of distillate and organic solvent is 1:1.
Compared with prior art, the invention has the following advantages:
1. so far, there has been no about red shellfish E Shi pore fungi Earliella scabrosa (Pers.) Gilb.&
The report and Related product of Ryvarden essential oil.
2.GC/MS analysis shows, the highest 6 kinds of active chemical components of content are (R)-in red shellfish essential oil of the present invention
(-) -3- methyl -2- butanol, 4- methyl -4- hydroxyl -2 pentanone, azulene, 18 carbon of toluene, palmitinic acid and (Z, Z) -9,12-
Dienoic acid, total amount account for the 70-90% of essential oil, wherein and (R)-(-) -3- methyl -2- butanol is colourless liquid, has fruit aroma,
It is the main component of leaf of bamboo volatile oil and the main volatile flavor components of methods of soft-shell turtle skirt；4- methyl -4- hydroxyl -2 pentanone,
Also known as diacetone alcohol, it is the colourless liquid with aromatic odor, is present in Herba Ajugae volatile oil, in Cynanchum Komarrivii AI Iijiniski volatile oil
Content is up to 43.70%；Azulene also known as Azulene, azulenes etc. are present in the herb and flower of compositae plant german chamomile, lauraceae plant camphor tree
Deng it is the main component of tea aroma and the major volatile constituents of Siraitia grosvenorii；Toluene colourless transparent liquid has similar
The aromatic odor of benzene is widely used in medicine, pesticide, dyestuff, especially perfume synthesis；Therefore red shellfish essential oil is in that fragrant ingredient is only
Spy is a kind of new flavors and fragrances, can be applied to the fields such as health care product, cosmetics.
3. the preparation method of red shellfish essential oil of the present invention is simple and practical, organic solvent can be effectively saved, raw material will not be made
Coking due to heating, and can effectively shorten extraction time, improve extraction of essential oil rate.
Detailed description of the invention
Fig. 1 is that the GC/MS of red shellfish essential oil described in the embodiment of the present invention 1 analyzes total ion current figure.
Specific embodiment
Below in conjunction with specific embodiment, the present invention will be described in detail, herein illustrative examples and explanation of the invention
For explaining the present invention, but it is not as a limitation of the invention.
Embodiment 1
Red shellfish essential oil is prepared according to the following steps:
(1) the red shellfish E Shi pore fungi fructification for taking 100g air-dried, obtains medicinal powder after crushing, and medicinal powder is packed into 1000mL constant pressure
It is installed in dropping funel, after compacting in the 500mL round-bottomed flask for being placed with 1-2 zeolites, the suitable for reading of round-bottomed flask is equipped with spherical shape
Condenser pipe, from spherical condensation tube addition ether suitable for reading, allows ether to flow through medicinal powder under the low-temperature circulating water cooling that temperature is 10 DEG C
It is instilled in round-bottomed flask from constant pressure funnel, until the volume of ether is the 2/3 of round-bottomed flask volume, closes constant pressure addition leakage
The cock of bucket keeps the liquid level of ether in constant pressure funnel to be more than medicinal powder and does not flow out from branch pipe, added with controllable temperature electric jacket
Heat makes the ether in round-bottomed flask boil, and the heating temperature of control controllable temperature electric jacket is 50 DEG C, and ether steam is from constant pressure addition
The branch pipe of funnel rises to spherical condensation tube, becomes ether drop after low-temperature circulating water is cooling and instills constant pressure funnel
In, the cock for unscrewing constant pressure funnel to instill the ether drop in constant pressure funnel and instills the liquid in round-bottomed flask
Drop speed is consistent, and continuous backflow seepage pressure effects are recycled until the drop instilled in round-bottomed flask is colourless by distilling apparatus
Coarse-fine oil is obtained after organic solvent；
(2) distilled water is added into the coarse-fine oil that step (1) obtains, using vacuum rotary evaporator, in low-temperature circulating water
Under cooling, with 90 DEG C of heating water bath, vacuum rotating steam distillation collects distillate until no distillate；
(3) add solid sodium chloride into the distillate that step (2) are collected until saturation merges second with ether extraction 3-5 times
Ether extract liquor, then with filtering after anhydrous magnesium sulfate drying, filtrate obtains red shellfish essential oil after ether is recovered by distillation.
The chemical composition analysis of red shellfish essential oil:
The chemical composition analysis of red shellfish essential oil is using Agilent 7890A gas-chromatography series connection Agilent 5975C mass spectrometry
Instrument.
Chromatographic condition: chromatographic column uses J&W 122-0132DB-1ms quartz capillary column (0.25 μ of the μ m of 30m × 250
m)；With temperature programming: 60 DEG C of initial temperature, constant temperature 5min, 100 DEG C are warming up to 2 DEG C/min speed, then with 2 DEG C/min speed
Degree is warming up to 200 DEG C, then is warming up to 300 DEG C with 25 DEG C/min, constant temperature 5min；250 DEG C of injector temperature, 1 μ L of sample volume；It shunts
Than 16: 1；Carrier gas is helium.
Mass Spectrometry Conditions: EI ion source, 220 DEG C of ion source temperature, electron energy 70ev, scanning range 10-550m/z.
Qualitative-and-quantitative method: the determination of each group swarming relative amount uses peak area normalization method.The mass spectrometric data of acquisition makes
It is analyzed with U.S. NIST08.L spectrum library.
It the results are shown in Table 1 with GC/MS joint technology and the library analysis of NIST spectrum.
The red shellfish essential oil main chemical compositions of table 1 and relative amount
Go out red shellfish essential oil main chemical compositions by GC/MS joint technology and the total identification and analysis of NIST spectrum library analysis and have 35
Kind, GC/MS analysis total ion current figure see Fig. 1, wherein the highest 6 kinds of chemical components of content be (R)-(-) -3- methyl -2- butanol,
4- methyl -4- hydroxyl -2 pentanone, azulene, toluene, palmitinic acid and (Z, Z) -9,12- octadecadienoic acid, relative mass hundred
Dividing than the sum of content is 80.66%.(R)-(-) -3- methyl -2- butanol is colourless liquid, has fruit aroma, is leaf of bamboo volatilization
The main component of oil and the main volatile flavor components of methods of soft-shell turtle skirt.4- methyl -4- hydroxyl -2 pentanone also known as diacetone
Alcohol is the colourless liquid with aromatic odor, is present in Herba Ajugae volatile oil that content is up in Cynanchum Komarrivii AI Iijiniski volatile oil
43.70%.Azulene also known as Azulene, azulenes etc. are present in the herb and flower of compositae plant german chamomile, and lauraceae plant camphor tree etc., it is
The main component of tea aroma and the major volatile constituents of Siraitia grosvenorii.Toluene colourless transparent liquid has the fragrance of similar benzene
Smell is widely used in medicine, pesticide, dyestuff, especially perfume synthesis.
Embodiment 2
Red shellfish essential oil is prepared according to 1 the method for embodiment, wherein unlike the first embodiment in step (1) and (3)
Organic solvent is petroleum ether, and the temperature of heating water bath is 92 DEG C in step (2), and desiccant is anhydrous sodium sulfate, system in step (3)
Highest 6 kinds of chemical components (R)-(-) -3- methyl -2- butanol of content, 4- methyl -4- hydroxyl -2- penta in standby red shellfish essential oil out
The sum of ketone, azulene, toluene, palmitinic acid and relative mass degree of (Z, Z) -9,12 octadecadienoic acid are 70%.
Embodiment 3
Red shellfish essential oil is prepared according to 1 the method for embodiment, wherein unlike the first embodiment in step (1) and (3)
Organic solvent is pentane, and the temperature of heating water bath is 94 DEG C in step (2), and desiccant is anhydrous calcium chloride, preparation in step (3)
Highest 6 kinds of chemical components (R)-(-) -3- methyl -2- butanol of content, 4- methyl -4- hydroxyl -2- penta in red shellfish essential oil out
The sum of ketone, azulene, toluene, palmitinic acid and relative mass degree of (Z, Z) -9,12 octadecadienoic acid are 90%.
Embodiment 4
Red shellfish essential oil is prepared according to 1 the method for embodiment, wherein unlike the first embodiment in step (1) and (3)
Organic solvent is hexane, and the temperature of heating water bath is 96 DEG C in step (2), and desiccant is silica gel in step (3), and for preparing is red
Highest 6 kinds of chemical components (R)-(-) -3- methyl -2- butanol of content, 4- methyl -4- hydroxyl -2 pentanone, camomile in shellfish essential oil
The sum of indigo plant, toluene, palmitinic acid and relative mass degree of (Z, Z) -9,12 octadecadienoic acid are 75%.
Embodiment 5
Red shellfish essential oil is prepared according to 1 the method for embodiment, wherein unlike the first embodiment in step (1) and (3)
Organic solvent is acetone, and the temperature of heating water bath is 98 DEG C in step (2), and desiccant is molecular sieve in step (3), is prepared
It is highest 6 kinds of chemical components (R)-(-) -3- methyl -2- butanol of content in red shellfish essential oil, 4- methyl -4- hydroxyl -2 pentanone, sweet
The sum of chrysanthemum indigo plant, toluene, palmitinic acid and relative mass degree of (Z, Z) -9,12 octadecadienoic acid are 85%.
Embodiment 6
Red shellfish essential oil is prepared according to 1 the method for embodiment, wherein unlike the first embodiment in step (1) and (3)
Organic solvent is chloroform, and the temperature of heating water bath is 100 DEG C in step (2), and desiccant is anhydrous magnesium sulfate, system in step (3)
Highest 6 kinds of chemical components (R)-(-) -3- methyl -2- butanol of content, 4- methyl -4- hydroxyl -2- penta in standby red shellfish essential oil out
The sum of ketone, azulene, toluene, palmitinic acid and relative mass degree of (Z, Z) -9,12 octadecadienoic acid are 80%.
The principle of the present invention and its effect is only illustrated in above-described embodiment, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology all without departing from the spirit and scope of the present invention, carries out modifications and changes to above-described embodiment.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should be covered by the claims of the present invention.
Claims (7)
1. a kind of red shellfish essential oil, it is characterised in that: it is made from red shellfish E Shi pore fungi fructification, content in the red shellfish essential oil
Highest 6 kinds of chemical components are (R)-(-) -3- methyl -2- butanol, 4- methyl -4- hydroxyl -2 pentanone, azulene, toluene, palm fibre
Palmitic acid acid and (Z, Z) -9,12- octadecadienoic acid, the sum of relative mass degree are 70-90%.
2. a kind of red shellfish essential oil according to claim 1, it is characterised in that: (R)-(-) -3- in the red shellfish essential oil
Methyl -2- butanol, 4- methyl -4- hydroxyl -2 pentanone, azulene, toluene, palmitinic acid and (Z, Z) -9,12 octadecadienoic acid
The sum of relative mass degree be 80.66%.
3. a kind of preparation method of red shellfish essential oil according to claim 1 or 2, it is characterised in that: the following steps are included:
(1) air-dried red shellfish E Shi pore fungi fructification is taken, obtains medicinal powder after crushing, medicinal powder is packed into 1000mL constant pressure funnel
In, it being installed to after compacting in the 500mL round-bottomed flask for being placed with 1-2 zeolites, the suitable for reading of round-bottomed flask is equipped with spherical condensation tube,
Under low-temperature circulating water is cooling, from spherical condensation tube addition organic solvent suitable for reading, allows organic solvent to flow through medicinal powder and leaked from constant pressure addition
Bucket instills in round-bottomed flask, until the volume of organic solvent is the 2/3 of round-bottomed flask volume, closes the rotation of constant pressure funnel
Plug keeps the liquid level of organic solvent in constant pressure funnel to be more than medicinal powder and does not flow out from branch pipe, heated with controllable temperature electric jacket
Make the organic solvent boiling in round-bottomed flask, the heating temperature of control controllable temperature electric jacket is 50 DEG C, and organic solvent vapor is from perseverance
The branch pipe of pressure dropping funel rises to spherical condensation tube, becomes organic solvent drop after low-temperature circulating water is cooling and instills constant pressure
In dropping funel, the cock for unscrewing constant pressure funnel the organic solvent drop instilled in constant pressure funnel and instills to justify
Liquid drop speed in the flask of bottom is consistent, and continuous backflow seepage pressure effects pass through until the drop instilled in round-bottomed flask is colourless
Coarse-fine oil is obtained after distilling apparatus recycling organic solvent；
(2) 300mL distilled water is added into the coarse-fine oil that step (1) obtains, using vacuum rotary evaporator, in low-temperature circulating water
Under cooling, heating water bath, vacuum rotating steam distillation collects distillate until no distillate；
(3) add solid sodium chloride into the distillate that step (2) are collected until saturation, is extracted 3-5 times with organic solvent, be associated with
Solvent extract liquor, then with filtering after desiccant dryness, filtrate obtains red shellfish essential oil after organic solvent is recovered by distillation；
Organic solvent in the step (1) and (3) is petroleum ether, ether, pentane, hexane, acetone, wherein one in chloroform
Kind；
In the step (2), the temperature of heating water bath is 90-100 DEG C.
4. a kind of preparation method of red shellfish essential oil according to claim 3, it is characterised in that: red in the step (1)
The mass ratio of distilled water in shellfish E Shi pore fungi fructification and step (2) is 1:3.
5. a kind of preparation method of red shellfish essential oil according to claim 3, it is characterised in that: in the step (1) and (2)
Low-temperature circulating water temperature be 10 DEG C.
6. a kind of preparation method of red shellfish essential oil according to claim 3, it is characterised in that: dry in the step (3)
Agent is anhydrous magnesium sulfate, anhydrous sodium sulfate, anhydrous calcium chloride, silica gel, the one of which in molecular sieve.
7. a kind of preparation method of red shellfish essential oil according to claim 3, it is characterised in that: in the step (3), distillate
The volume ratio of liquid and organic solvent is 1:1.
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| CN101664422A (en) * | 2009-09-18 | 2010-03-10 | 长沙湘蕈生物科技有限公司 | Supercritical fluid extract technology of ganoderma volatile oil, ganodenic acid and ganoderma polysaccharide |
| CN101693853A (en) * | 2009-10-27 | 2010-04-14 | 北京林业大学 | Device for extracting plant essential oil and method for preparing bamboo leaf essential oil by using same |
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| CN101664422A (en) * | 2009-09-18 | 2010-03-10 | 长沙湘蕈生物科技有限公司 | Supercritical fluid extract technology of ganoderma volatile oil, ganodenic acid and ganoderma polysaccharide |
| CN101693853A (en) * | 2009-10-27 | 2010-04-14 | 北京林业大学 | Device for extracting plant essential oil and method for preparing bamboo leaf essential oil by using same |
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| Title |
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| "竹叶挥发油化学成分及其抗氧化特性";何跃君等;《林业科学》;20101231;第46卷(第7期);120-128 * |
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