CN114561246B - Preparation method of camphor tree essential oil and antibacterial application thereof - Google Patents
Preparation method of camphor tree essential oil and antibacterial application thereof Download PDFInfo
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- CN114561246B CN114561246B CN202210149087.3A CN202210149087A CN114561246B CN 114561246 B CN114561246 B CN 114561246B CN 202210149087 A CN202210149087 A CN 202210149087A CN 114561246 B CN114561246 B CN 114561246B
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- 241000723346 Cinnamomum camphora Species 0.000 title claims abstract description 97
- 239000000341 volatile oil Substances 0.000 title claims abstract description 59
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 230000000844 anti-bacterial effect Effects 0.000 title abstract description 26
- 238000000605 extraction Methods 0.000 claims abstract description 50
- 239000002904 solvent Substances 0.000 claims abstract description 28
- LVGUZGTVOIAKKC-UHFFFAOYSA-N 1,1,1,2-tetrafluoroethane Chemical compound FCC(F)(F)F LVGUZGTVOIAKKC-UHFFFAOYSA-N 0.000 claims abstract description 22
- 244000052616 bacterial pathogen Species 0.000 claims abstract description 14
- 230000001580 bacterial effect Effects 0.000 claims abstract description 11
- 241000233866 Fungi Species 0.000 claims abstract description 8
- 241000813090 Rhizoctonia solani Species 0.000 claims abstract description 7
- 241000233616 Phytophthora capsici Species 0.000 claims abstract description 6
- 241000196324 Embryophyta Species 0.000 claims abstract description 5
- 241000588701 Pectobacterium carotovorum Species 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 14
- 239000010779 crude oil Substances 0.000 claims description 12
- 239000000284 extract Substances 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 230000001276 controlling effect Effects 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 235000019441 ethanol Nutrition 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000012530 fluid Substances 0.000 claims description 3
- 239000003814 drug Substances 0.000 claims description 2
- 230000002401 inhibitory effect Effects 0.000 claims description 2
- 238000007670 refining Methods 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 239000000203 mixture Substances 0.000 abstract description 4
- 230000000443 biocontrol Effects 0.000 abstract description 2
- 230000005764 inhibitory process Effects 0.000 description 14
- 241000894006 Bacteria Species 0.000 description 13
- 238000000034 method Methods 0.000 description 11
- DSSYKIVIOFKYAU-XCBNKYQSSA-N (R)-camphor Chemical compound C1C[C@@]2(C)C(=O)C[C@@H]1C2(C)C DSSYKIVIOFKYAU-XCBNKYQSSA-N 0.000 description 8
- 229960000846 camphor Drugs 0.000 description 7
- 229930008380 camphor Natural products 0.000 description 7
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 7
- 239000003153 chemical reaction reagent Substances 0.000 description 6
- 244000000626 Daucus carota Species 0.000 description 4
- 235000002767 Daucus carota Nutrition 0.000 description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 description 4
- 240000007594 Oryza sativa Species 0.000 description 4
- 235000007164 Oryza sativa Nutrition 0.000 description 4
- 241000531155 Pectobacterium Species 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 235000009566 rice Nutrition 0.000 description 4
- 229920001817 Agar Polymers 0.000 description 3
- 239000008272 agar Substances 0.000 description 3
- 238000012258 culturing Methods 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 238000007873 sieving Methods 0.000 description 2
- 238000001256 steam distillation Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241001530056 Athelia rolfsii Species 0.000 description 1
- 244000063299 Bacillus subtilis Species 0.000 description 1
- 235000014469 Bacillus subtilis Nutrition 0.000 description 1
- 235000002566 Capsicum Nutrition 0.000 description 1
- 241000588724 Escherichia coli Species 0.000 description 1
- 239000006002 Pepper Substances 0.000 description 1
- 241000233614 Phytophthora Species 0.000 description 1
- 235000016761 Piper aduncum Nutrition 0.000 description 1
- 235000017804 Piper guineense Nutrition 0.000 description 1
- 244000203593 Piper nigrum Species 0.000 description 1
- 235000008184 Piper nigrum Nutrition 0.000 description 1
- 241000589517 Pseudomonas aeruginosa Species 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 244000082946 Tarchonanthus camphoratus Species 0.000 description 1
- 235000005701 Tarchonanthus camphoratus Nutrition 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000003385 bacteriostatic effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002538 fungal effect Effects 0.000 description 1
- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 238000003815 supercritical carbon dioxide extraction Methods 0.000 description 1
- 235000015112 vegetable and seed oil Nutrition 0.000 description 1
- 239000008158 vegetable oil Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/027—Recovery of volatiles by distillation or stripping
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a preparation method of camphor tree essential oil and antibacterial application thereof. According to the invention, the environmental-friendly solvent tetrafluoroethane is used as an extraction solvent, and the camphor tree essential oil prepared by extraction under subcritical conditions has obvious antibacterial activity on plant fungi and bacterial pathogenic bacteria such as Rhizoctonia solani, phytophthora capsici, rhizoctonia solani or pectobacterium carotovorum and the like due to the specific composition components, so that the camphor tree essential oil can be used in the field of crop biocontrol.
Description
Technical Field
The invention relates to a preparation method of camphor tree essential oil with antibacterial activity, belonging to the field of vegetable oil extraction, separation and application.
Background
Camphor tree Cinnamomum camphora, also called camphor, black camphor, camphor wood, camphor tree, etc. is a evergreen broad-leaf arbor of camphor genus of camphor family, and is planted in Guangdong, guangxi, jiangxi, fujian, taiwan area, hunan, hubei, sichuan, yunnan, etc. places in southeast and southwest of China. The camphor tree bark, root, stem and leaf can extract essential oil, has medicinal values of bacteriostasis, pain relieving, anticancer, antioxidation and the like, and is an important raw material in the industries of spice essence, medicine and health and the like.
The extraction method of camphor tree essential oil comprises a steam distillation method, an organic solvent extraction method, a supercritical carbon dioxide extraction method, an ultrasonic auxiliary extraction method, a simultaneous distillation extraction method, a microwave auxiliary water distillation method and the like, and the research on extracting camphor tree essential oil by subcritical fluid is very little at present. Zhou Haixu the extraction process is carried out by taking subcritical n-butane as solvent, extracting at 65deg.C and 45deg.C for 40min to obtain 3.54% of essential oil, and inhibiting Escherichia coli, staphylococcus aureus, pseudomonas aeruginosa, and Bacillus subtilis.
The kind of solvent is an important factor affecting the extraction effect. According to the principle of similar compatibility, the types of solvents can influence the chemical composition components in the extract, thereby influencing the application effect.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method and antibacterial application of camphor tree essential oil.
In order to achieve the above purpose, the following technical scheme is adopted:
according to the invention, the environmental-friendly solvent tetrafluoroethane is used as an extraction solvent, and the camphor tree essential oil prepared by extraction under subcritical conditions has obvious inhibition effect on plant fungi and bacterial pathogenic bacteria due to the specific composition components.
A preparation method of camphor tree essential oil comprises the following steps:
(1) Pretreatment of raw materials:
drying fresh camphor tree branches and leaves at 50-60 ℃ until the water content is 3-6%, and then crushing to obtain camphor tree branch and leaf powder;
(2) Subcritical fluid extraction:
placing camphor tree branch and leaf powder into an extraction tank of subcritical extraction equipment, regulating the system pressure to 0.01MPa by using a vacuum pump, then introducing a liquid solvent into the extraction tank from the solvent tank, controlling the feed liquid ratio of the camphor tree branch and leaf powder to the liquid solvent to be 1:4-1:7 (mass volume ratio kg/L), heating the extraction tank to 35-50 ℃ by using a hot water circulation system, controlling the extraction time to be 30-60 min, introducing an extract into a separation tank after extraction is finished, recovering the solvent by using a compressor, repeatedly extracting for 3-5 times, and merging extracts to obtain camphor tree crude oil;
(3) Refining camphor tree crude oil:
adding 20 times (mass volume ratio g/ml) of absolute ethyl alcohol into camphor tree crude oil, uniformly mixing, standing at-18 to-20 ℃, filtering, adding 1.5-3% (mass volume ratio g/ml) of active carbon into filtrate, stirring at 40 ℃, filtering, and distilling under reduced pressure at 45 ℃ and 0.01MPa to recover ethyl alcohol to obtain camphor tree essential oil.
Preferably, in the above preparation method of camphor tree essential oil, the liquid solvent is tetrafluoroethane (R134 a).
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention adopts subcritical extraction technology, has simple operation process and easy amplified production, and can greatly improve extraction efficiency compared with the traditional steam distillation technology.
(2) The invention adopts the environmental-friendly solvent tetrafluoroethane as the extraction solvent, is nonflammable and nontoxic, is safer than alkane solvents, and has not been reported in the research of extracting camphor tree essential oil by adopting subcritical tetrafluoroethane at present.
(3) According to the similar principle, the camphor tree essential oil extracted by subcritical tetrafluoroethane shows remarkable antibacterial activity to plant fungi and bacterial pathogenic bacteria such as banded sclerotial blight bacteria, phytophthora capsici, bacterial wilt bacteria or carrot soft rot pectobacterium due to the special chemical component composition mode, and can be used in the field of crop biocontrol. Wherein the colony diameter of the Rhizoctonia solani is 10.1+/-1.0 mm, the inhibition rate of the camphor tree essential oil is 88.65%, the colony diameter of the phytophthora capsici is 31.2+/-1.1 mm, and the inhibition rate of the camphor tree essential oil is 64.94%. The diameter of the antibacterial ring of camphor tree essential oil to bacterial wilt bacteria is 27.2 plus or minus 1.0mm, which belongs to high antibacterial intensity, and the diameter of the antibacterial ring to carrot soft rot pectobacterium is 23.3 plus or minus 1.2mm, which belongs to high antibacterial intensity.
Drawings
Fig. 1 is a graph showing the bacteriostatic effect of camphor tree essential oil on fungi and bacterial pathogens. Wherein A is Rhizoctonia solani, B is Phytophthora capsici, C is Rhizoctonia solani, and D is pectobacterium carotovorum; the left side of each figure is a blank control plate, and the right side is a plate treated with the essential oil added reagent.
Detailed Description
The following embodiments are some examples of the present invention and should not be construed as limiting the present invention.
EXAMPLE 1 preparation of camphor essential oil
Drying fresh camphor tree branches and leaves at 60 ℃ for 4 hours by adopting a heat pump dryer until the water content is 4%, and crushing the dry camphor tree branches and leaves by using a crusher and sieving the crushed dry camphor tree branches and leaves with a 20-mesh screen to obtain camphor tree branch and leaf powder.
Placing camphor tree branch and leaf powder into 300-mesh filter bags, placing the 300-mesh filter bags into an extraction tank of subcritical extraction equipment, using a vacuum pump to enable the system pressure to be 0.01MPa, then introducing tetrafluoroethane into the extraction tank from the solvent tank, controlling the feed-liquid ratio to be 1:7 (mass-volume ratio kg/L) by adopting a metering tank during the process, heating the extraction tank to 40 ℃ by adopting a hot water circulation system, controlling the extraction time to be 40min, introducing extract into a separation tank after extraction is finished, recovering tetrafluoroethane by using a compressor, repeatedly extracting for 4 times, and merging extracts to obtain camphor tree crude oil.
Adding 20 times (mass volume ratio g/ml) of absolute ethyl alcohol into camphor tree crude oil, uniformly mixing, standing at-18 ℃ for 24 hours, filtering, adding 2% (mass volume ratio g/ml) of active carbon into filtrate, stirring for 30 minutes at 40 ℃, filtering, and distilling under reduced pressure at 45 ℃ and 0.01MPa to recover the ethyl alcohol, thereby obtaining camphor tree essential oil, wherein the yield (mass ratio g/g) of the camphor tree essential oil relative to the raw material (camphor tree branch and leaf powder) is 2.62%.
EXAMPLE 2 preparation of camphor essential oil
Drying fresh camphor tree branches and leaves at 55 ℃ for 5 hours by adopting a heat pump dryer until the water content is 4%, and crushing the dry camphor tree branches and leaves by using a crusher and sieving the crushed dry camphor tree branches and leaves with a 20-mesh screen to obtain camphor tree branch and leaf powder.
Placing camphor tree branch and leaf powder into 300-mesh filter bags, placing the 300-mesh filter bags into an extraction tank of subcritical extraction equipment, using a vacuum pump to enable the system pressure to be 0.01MPa, then introducing tetrafluoroethane into the extraction tank from the solvent tank, controlling the feed-liquid ratio to be 1:5 (mass-volume ratio kg/L) by adopting a metering tank during the process, heating the extraction tank to 45 ℃ by adopting a hot water circulation system, controlling the extraction time to be 40min, introducing extract into a separation tank after extraction is finished, recovering tetrafluoroethane by using a compressor, repeatedly extracting for 4 times, and merging extracts to obtain camphor tree crude oil.
Adding 20 times (mass volume ratio g/ml) of absolute ethyl alcohol into camphor tree crude oil, uniformly mixing, standing at-20 ℃ for 24 hours, filtering, adding 2% (mass volume ratio g/ml) of active carbon into filtrate, stirring for 30 minutes at 40 ℃, filtering, and distilling under reduced pressure at 45 ℃ and 0.01MPa to recover the ethyl alcohol, thereby obtaining camphor tree essential oil, wherein the yield (mass ratio g/g) of the camphor tree essential oil relative to the raw material (camphor tree branch and leaf powder) is 2.84%.
EXAMPLE 3 preparation of camphor essential oil
Drying fresh camphor tree branches and leaves at 50 ℃ for 6 hours by adopting a heat pump dryer until the water content is 5%, and crushing the dry camphor tree branches and leaves to 40 meshes by using a crusher.
Placing camphor tree branch and leaf powder into 300-mesh filter bags, placing the 300-mesh filter bags into an extraction tank of subcritical extraction equipment, using a vacuum pump to enable the system pressure to be 0.01MPa, then introducing tetrafluoroethane into the extraction tank from the solvent tank, controlling the feed-liquid ratio to be 1:6 (mass-volume ratio kg/L) by adopting a metering tank during the process, heating the extraction tank to 45 ℃ by adopting a hot water circulation system, controlling the extraction time to be 50min, introducing extract into a separation tank after extraction is finished, recovering tetrafluoroethane by using a compressor, repeatedly extracting for 4 times, and merging extracts to obtain camphor tree crude oil.
Adding 20 times (mass volume ratio g/ml) of absolute ethyl alcohol into camphor tree crude oil, uniformly mixing, standing at-19 ℃ for 24 hours, filtering, adding 1.5% (mass volume ratio g/ml) of active carbon into filtrate, stirring for 30 minutes at 40 ℃, filtering, and distilling under reduced pressure at 45 ℃ and 0.01MPa to recover the ethyl alcohol, thereby obtaining camphor tree essential oil, wherein the yield (mass ratio g/g) of the camphor tree essential oil relative to the raw material (camphor tree branch and leaf powder) is 3.1%.
EXAMPLE 4 antibacterial Activity study of camphor tree essential oil
The antibacterial activity of camphor tree essential oil on pathogenic bacteria of fungi is researched by adopting a PDA flat plate counter method, and the antibacterial activity of camphor tree essential oil on the pathogenic bacteria is researched by adopting a filter paper agar diffusion method, wherein the pathogenic bacteria of the camphor tree are rice sheath blight bacteria and phytophthora capsici, and the pathogenic bacteria of the camphor tree are bacterial wilt bacteria and pectobacterium carotovorum.
The preparation method of camphor tree essential oil reagent for antibacterial activity research comprises the following steps: under aseptic condition, dissolving camphor tree essential oil with a certain amount of dimethyl sulfoxide (DMSO) to prepare 100mg/ml solution.
PDA plate counter method: a proper amount of fungus pathogenic bacteria cake is taken by a 6mm puncher and placed in the center of a PDA flat plate, and holes are punched at three points which are equidistant and in an equilateral triangle shape from the position about 2cm away from the bacteria cake, 100 μl of camphor tree essential oil reagent is added into each hole, and 3 repetitions of treatment are carried out, and the treatment without adding essential oil is used as a blank control. Culturing at 28 ℃ until the blank control plate is full of hypha, measuring the colony diameter of each treatment, and calculating the inhibition rate. The calculation formula is as follows:
antibacterial ratio = (diameter of control colony-diameter of treated colony)/diameter of control colony × 100%
Filter paper sheet agar diffusion method: about 20ml of a sterile agar medium was poured into a sterile petri dish, and after it had solidified, 100. Mu.l of a bacterial pathogen solution (concentration of the solution was adjusted to 10) 8 CFU/ml), and standing at a constant temperature of 30 ℃ for 1h after uniform coating. Placing a sterile circular filter paper sheet with the diameter of 6mm at the three points which are about 3cm away from the center point of the flat plate and form an equilateral triangle, sucking 20 μl of camphor tree essential oil reagent by a pipette, dispersing the camphor tree essential oil reagent on the filter paper, culturing at the constant temperature of 28 ℃ for 24 hours, observing the antibacterial effect of the essential oil reagent on pectobacterium carotovorum, observing the antibacterial effect of the essential oil on bacterial wilt after 48 hours, and measuring the diameter of a antibacterial circle by a crisscross method. The diameter of the inhibition zone is more than 15mm, the diameter of the inhibition zone is more than or equal to 10mm and less than or equal to 15mm, the diameter of the inhibition zone is more than 0mm and less than 10mm, the inhibition is performed moderately, and the inhibition is performed moderately.
According to the preparation method, tetrafluoroethane and n-butane are respectively used as extraction solvents for extracting camphor tree essential oil, the inhibition rate of the camphor tree essential oil prepared by using tetrafluoroethane as the extraction solvent for rice sheath blight bacteria is 88.65%, the inhibition rate of the camphor tree essential oil prepared by using n-butane as the extraction solvent for rice sheath blight bacteria is 64.94%, the inhibition rate of the camphor tree essential oil prepared by using n-butane for rice sheath blight bacteria is 78.09%, the inhibition rate of the camphor tree essential oil extracted by using tetrafluoroethane for pepper phytophthora bacteria is 56.97%, and the inhibition effect of the camphor tree essential oil extracted by using tetrafluoroethane for the two fungal pathogenic bacteria is more remarkable. The diameter of the antibacterial circle of the camphor tree essential oil prepared by using tetrafluoroethane as an extraction solvent for bacterial wilt bacteria is 27.2+/-1.0 mm, the diameter of the antibacterial circle of the camphor tree essential oil for carrot soft rot pectobacterium is 23.3+/-1.2 mm, the antibacterial circle of the camphor tree essential oil prepared by using n-butane as the extraction solvent for bacterial wilt bacteria is 12.3+/-1.2 mm, the diameter of the antibacterial circle for carrot soft rot pectobacterium is 13.3+/-1.1 mm, the antibacterial effect of the camphor tree essential oil extracted by using tetrafluoroethane for bacterial wilt bacteria is more remarkable. The antibacterial effect of tetrafluoroethane is shown in figure 1. The main components of the camphor tree essential oil extracted by tetrafluoroethane and n-butane are shown in table 1, and the main components and the proportion of the camphor tree essential oil are different, so that the essential oil has obvious difference in antibacterial activity on different pathogenic bacteria.
TABLE 1 GC/MS analysis results of essential oils of camphor tree leaf extracted with subcritical tetrafluoroethane and n-butane
Claims (2)
1. A preparation method of camphor tree essential oil is characterized by comprising the following steps:
(1) Pretreatment of raw materials:
drying fresh camphor tree branches and leaves at 50-60 ℃ until the water content is 3-6%, and then crushing to obtain camphor tree branch and leaf powder;
(2) Subcritical fluid extraction:
placing camphor tree branch and leaf powder into an extraction tank of subcritical extraction equipment, regulating the system pressure to 0.01MPa by using a vacuum pump, then introducing a liquid solvent into the extraction tank from the solvent tank, controlling the feed-liquid ratio of the camphor tree branch and leaf powder to the liquid solvent to be 1:4-1:7, heating the extraction tank to 35-50 ℃ by using a hot water circulation system, controlling the extraction time to be 30-60 min, introducing an extract into a separation tank after extraction is finished, recovering the solvent by using a compressor, repeatedly extracting for 3-5 times, and merging extracts to obtain camphor tree crude oil;
(3) Refining camphor tree crude oil:
adding 20 times of absolute ethyl alcohol into camphor tree crude oil, uniformly mixing, standing at-18 to-20 ℃, filtering, adding 1.5-3% of active carbon into filtrate, stirring at 40 ℃, filtering, and distilling under reduced pressure at 45 ℃ and 0.01MPa to recover ethyl alcohol to obtain camphor tree essential oil;
the liquid solvent is tetrafluoroethane.
2. Use of the camphor tree essential oil of claim 1 for preparing a medicament for inhibiting plant fungi or bacterial pathogens; the plant fungi or bacterial pathogenic bacteria are Rhizoctonia solani, phytophthora capsici, rhizoctonia solani or pectobacterium carotovorum.
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| NZ545146A (en) * | 2006-02-07 | 2009-03-31 | Ind Res Ltd | Near-critical fluid fractionation process for extracting plant or animal material |
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