CN114467985A - Method for extracting peony seed essential oil based on solvent method - Google Patents
Method for extracting peony seed essential oil based on solvent method Download PDFInfo
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- CN114467985A CN114467985A CN202210026052.0A CN202210026052A CN114467985A CN 114467985 A CN114467985 A CN 114467985A CN 202210026052 A CN202210026052 A CN 202210026052A CN 114467985 A CN114467985 A CN 114467985A
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- 241000736199 Paeonia Species 0.000 title claims abstract description 134
- 235000006484 Paeonia officinalis Nutrition 0.000 title claims abstract description 124
- 239000000341 volatile oil Substances 0.000 title claims abstract description 81
- 238000000034 method Methods 0.000 title claims abstract description 41
- 239000002904 solvent Substances 0.000 title claims description 34
- 238000000605 extraction Methods 0.000 claims abstract description 41
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims abstract description 30
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims abstract description 20
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000003208 petroleum Substances 0.000 claims abstract description 10
- 238000000944 Soxhlet extraction Methods 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims description 21
- 210000000582 semen Anatomy 0.000 claims description 14
- 239000012043 crude product Substances 0.000 claims description 11
- 238000010298 pulverizing process Methods 0.000 claims description 11
- 239000012528 membrane Substances 0.000 claims description 10
- 238000004321 preservation Methods 0.000 claims description 8
- 238000004821 distillation Methods 0.000 claims description 6
- 239000012535 impurity Substances 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- 239000000047 product Substances 0.000 claims description 3
- 235000015112 vegetable and seed oil Nutrition 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 2
- 238000000643 oven drying Methods 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 238000007670 refining Methods 0.000 claims description 2
- 238000011534 incubation Methods 0.000 claims 2
- 230000001680 brushing effect Effects 0.000 claims 1
- 239000012046 mixed solvent Substances 0.000 abstract description 2
- 238000000199 molecular distillation Methods 0.000 abstract description 2
- 239000003960 organic solvent Substances 0.000 abstract description 2
- 239000000419 plant extract Substances 0.000 abstract description 2
- 238000000926 separation method Methods 0.000 abstract description 2
- 238000003809 water extraction Methods 0.000 abstract 1
- 241001442207 Monochamus alternatus Species 0.000 description 30
- 235000011613 Pinus brutia Nutrition 0.000 description 23
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 22
- 241000018646 Pinus brutia Species 0.000 description 22
- 244000236658 Paeonia lactiflora Species 0.000 description 21
- 235000008598 Paeonia lactiflora Nutrition 0.000 description 20
- 201000010099 disease Diseases 0.000 description 11
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 11
- 239000010779 crude oil Substances 0.000 description 10
- 241000243771 Bursaphelenchus xylophilus Species 0.000 description 8
- 238000001035 drying Methods 0.000 description 8
- 238000007873 sieving Methods 0.000 description 8
- 241000196324 Embryophyta Species 0.000 description 7
- 238000011161 development Methods 0.000 description 6
- 230000018109 developmental process Effects 0.000 description 6
- 241000244206 Nematoda Species 0.000 description 4
- 238000009792 diffusion process Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 230000019617 pupation Effects 0.000 description 4
- 229920002379 silicone rubber Polymers 0.000 description 3
- 239000004945 silicone rubber Substances 0.000 description 3
- 241000243770 Bursaphelenchus Species 0.000 description 2
- 206010053759 Growth retardation Diseases 0.000 description 2
- 240000002853 Nelumbo nucifera Species 0.000 description 2
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 2
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 2
- 241000382353 Pupa Species 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000008280 blood Substances 0.000 description 2
- 210000004369 blood Anatomy 0.000 description 2
- 239000003086 colorant Substances 0.000 description 2
- 238000005553 drilling Methods 0.000 description 2
- 231100000001 growth retardation Toxicity 0.000 description 2
- 210000004185 liver Anatomy 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 235000019198 oils Nutrition 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241001237431 Anomala Species 0.000 description 1
- 235000007516 Chrysanthemum Nutrition 0.000 description 1
- 244000189548 Chrysanthemum x morifolium Species 0.000 description 1
- 244000223760 Cinnamomum zeylanicum Species 0.000 description 1
- 244000286779 Hansenula anomala Species 0.000 description 1
- 241000238631 Hexapoda Species 0.000 description 1
- OYHQOLUKZRVURQ-HZJYTTRNSA-N Linoleic acid Chemical compound CCCCC\C=C/C\C=C/CCCCCCCC(O)=O OYHQOLUKZRVURQ-HZJYTTRNSA-N 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 241000124446 Paeonia mairei Species 0.000 description 1
- 241000984759 Paeonia sinjiangensis Species 0.000 description 1
- 240000002390 Pandanus odoratissimus Species 0.000 description 1
- 241000218641 Pinaceae Species 0.000 description 1
- 235000011609 Pinus massoniana Nutrition 0.000 description 1
- 241000018650 Pinus massoniana Species 0.000 description 1
- 244000221860 Podophyllum emodi Species 0.000 description 1
- 244000169266 Pouteria obovata Species 0.000 description 1
- 241000218201 Ranunculaceae Species 0.000 description 1
- 241000220317 Rosa Species 0.000 description 1
- DTOSIQBPPRVQHS-PDBXOOCHSA-N alpha-linolenic acid Chemical compound CC\C=C/C\C=C/C\C=C/CCCCCCCC(O)=O DTOSIQBPPRVQHS-PDBXOOCHSA-N 0.000 description 1
- 235000020661 alpha-linolenic acid Nutrition 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000017531 blood circulation Effects 0.000 description 1
- 230000001914 calming effect Effects 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 235000017803 cinnamon Nutrition 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
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- 230000003111 delayed effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000005058 diapause Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000032669 eclosion Effects 0.000 description 1
- 235000013601 eggs Nutrition 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 235000019197 fats Nutrition 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 235000020778 linoleic acid Nutrition 0.000 description 1
- OYHQOLUKZRVURQ-IXWMQOLASA-N linoleic acid Natural products CCCCC\C=C/C\C=C\CCCCCCCC(O)=O OYHQOLUKZRVURQ-IXWMQOLASA-N 0.000 description 1
- 229960004488 linolenic acid Drugs 0.000 description 1
- KQQKGWQCNNTQJW-UHFFFAOYSA-N linolenic acid Natural products CC=CCCC=CCC=CCCCCCCCC(O)=O KQQKGWQCNNTQJW-UHFFFAOYSA-N 0.000 description 1
- VYQNWZOUAUKGHI-UHFFFAOYSA-N monobenzone Chemical compound C1=CC(O)=CC=C1OCC1=CC=CC=C1 VYQNWZOUAUKGHI-UHFFFAOYSA-N 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
- 238000012795 verification Methods 0.000 description 1
Classifications
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
- A01N65/08—Magnoliopsida [dicotyledons]
- A01N65/32—Ranunculaceae [Buttercup family], e.g. hepatica, hydrastis or goldenseal
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
-
- 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
-
- 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
- C11B9/022—Refining
-
- 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
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Wood Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Organic Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- Biotechnology (AREA)
- Agronomy & Crop Science (AREA)
- Natural Medicines & Medicinal Plants (AREA)
- Microbiology (AREA)
- Mycology (AREA)
- Plant Pathology (AREA)
- Dentistry (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Fats And Perfumes (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention belongs to the technical field of plant extracts, and particularly relates to a method for extracting peony seed essential oil by using a subcritical water extraction technology, and further discloses an application of the peony seed essential oil. The method for extracting the peony seed essential oil is used for extracting the peony seed essential oil based on an organic solvent method combined with a molecular distillation method, and the mixed solvent of ethyl acetate, ethanol and petroleum ether is selected for Soxhlet extraction by optimizing various operation parameters, so that the purposes of efficient extraction and separation of the peony seed essential oil and high purity of an extracted product are achieved, and the method has the advantages of simplicity in operation, short operation time and higher extraction efficiency.
Description
Technical Field
The invention belongs to the technical field of plant extracts, and particularly relates to a method for extracting peony seed essential oil based on a solvent method, and further discloses an application of the method.
Background
Paeonia (Paeonia L.) is shrub or herb of Ranunculaceae (Ranunculacea), and about 35 species are divided into 3 groups, i.e., Paeonia lactiflora and Paeonia lactiflora. The Paeonia lactiflora belongs to the largest group in China, the group is of herbaceous type and contains about 25 varieties, and the varieties are distributed in the continental Asia Europe, and about 8 varieties and 5 varieties exist in China. Currently, main varieties of paeonia plants in China include paeonia lactiflora (p.lactiflora), paeonia lactiflora (p.veitchii), paeonia lactiflora (p.obovata), paeonia lactiflora (p.anomala subsp.anomala), paeonia multiflora (p.emodi), paeonia alba (p.steriana), paeonia meili (p.mairei), paeonia sinkiangensis (p.sinjiangensis), paeonia tuberosa (p.internmedia) and the like. The peony medicinal plants mostly have bright flowers, wherein the flower phase of the peony (Paeonia lactiflora) flower is cultivated in most areas of China, and although the peony medicinal plants are mostly used as ornamental flowers, the root of the peony medicinal plants can be used as a medicine, and the peony medicinal plants have the effects of enriching and astringing yin, softening liver and relieving pain, nourishing yin and calming liver, clearing heat and cooling blood, promoting blood circulation and removing blood stasis and the like. In the chinese pharmacopoeia 2010 edition, white peony root is derived from roots of cultivated or its variant paeonia lactiflora var. trichocarpa, and red peony root is derived from roots of wild paeonia lactiflora and paeonia lactiflora (p.
Peony is the traditional famous flower of China, Song.Zheng firewoodGeneral will not be relievedCarrying out: paeonia herbaceous peony is written in the third generation, and also in the chant of elegant chant. In the later Tang Dynasty, people also refer to Paeonia lactiflora and Paeonia lactiflora as "two kings in flower", the term "Paeonia lactiflora is king of flower", and Paeonia lactiflora isFlower (A. B. A. B. A. B. A. B. A. B. A. B. A. B. A. B. A. B. A. B. A. B. A. B. A. B. A. B. A. B. A. B. A Phase(s)", which are enough to prove the chonghigh status and the unrivaled favor degree of the Chinese herbaceous peony in the traditional Chinese people's mind. After green peony has been bred from the lotus flower grower in recent years, the peony also realizes a complete system of 'red, yellow, white, pink, blue, black, purple, green and compound' nine major color systems like the king peony. Peony has various and peculiar flower colors and flower types, and the flower types are mostly single petal type, lotus type, rose type,Jin RuiThe flower bud is characterized by being shaped like a chrysanthemum, a cinnamon, a golden ring, an embroidery ball, a crown, a pavilion, and the like, and because the flower bud has the characteristics of needle-shaped colored petals, different colors of inner petals and outer petals, the peony is more magical and endless in charm.
The cultivation area of Chinese peony is large, and considerable amount of seeds can be harvested every year after proper cultivation. The peony seeds are the essence crystals of peony plants, and have unique medical and nutritional ingredients besides all the characteristics of the peony, and the peony seeds are nuts protected by shells and seed shells and have natural longevity genes. The peony seed is reported to have an oil content of more than 20%, contains a large amount of nutrient components such as linolenic acid and linoleic acid required by human body, wherein the content of unsaturated fatty acid is as high as about 90%, so the peony seed oil developed based on the peony seed has great development value.
Pine wood nematode disease, known as "cancer" in pine trees, is the most dangerous forest disease in the world and is a devastating epidemic disease of plants of the Pinaceae family. Although the pine wood nematode is seriously harmful, the pine wood nematode has the fatal weakness that the pine wood nematode can not spread and spread by itself and can only spread and spread by means of medium insects such as monochamus alternatus hope and the like. Studies have shown that the mass propagation of bursaphelenchus xylophilus is a direct cause of death in pine, while diffuse-type third instar larvae (L)III) And spread type four instar larva (L)IV) The matching of the formation time and the emergence time of the monochamus alternatus is the key point of the carrying and the transmission of the bursaphelenchus xylophilus. Therefore, if the emergence number of the monochamus alternatus hope can be effectively controlled, the approach of spreading the bursaphelenchus xylophilus disease is blocked. Therefore, by interfering and controlling the development of the monochamus alternatus larvae, the emergence time of the monochamus alternatus larvae can be delayed or the monochamus alternatus larvae cannot emerge, so that the diffused type fourth-instar larvae (L)IV) The method can not form and cut off the transmission and diffusion path, is the key for controlling the pine wilt disease, and has positive significance for the control of the pine wilt disease.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to provide a method for extracting peony seed essential oil based on a solvent method, the method realizes the efficient extraction of peony seeds, the obtained peony seed essential oil has the advantages of high purity and stable property, and the value of the peony seeds is improved to a higher level;
the second technical problem to be solved by the invention is to provide a new application of the peony seed essential oil in preparing a monochamus alternatus development retardant for preventing and treating pine wood nematodes.
In order to solve the technical problems, the method for extracting the peony seed essential oil based on the solvent method comprises the following steps:
(1) removing impurities from semen Paeoniae, removing shell, oven drying, and pulverizing;
(2) placing the obtained peony seed crushed material in a soxhlet extraction device, adding an organic extraction solvent for heat preservation extraction, collecting an extracting solution containing crude peony seed oil, carrying out reduced pressure concentration, and recovering the organic extraction solvent to obtain a crude peony seed essential oil product;
(3) and adding the obtained crude product of the peony seed essential oil into a molecular distiller for distillation treatment until the crude product of the peony seed essential oil is completely collected by a heavy phase collection tank and a light phase collection tank, and collecting the peony seed essential oil in the heavy phase collection tank to obtain the peony seed essential oil.
Specifically, in the step (2), the organic extraction solvent includes a mixture of ethyl acetate, ethanol and petroleum ether.
Specifically, in the step (2), the volume ratio of ethyl acetate, ethanol and petroleum ether is 1: 2: 5.
specifically, in the step (2), the mass ratio of the peony seed crushed aggregates to the organic extraction solvent is 1: 3-5.
Specifically, in the step (2), the temperature of the heat preservation extraction step is 70-90 ℃.
Specifically, in the step (2), before the step of heat preservation extraction, the method further comprises the step of soaking the peony seed crushed material for 1 hour.
Specifically, in the step (3), in the distillation treatment step, the vacuum degree in the molecular distiller is controlled to be 1.0-2.0Pa, the temperature is controlled to be 60-80 ℃, and the rotating speed of a rotary brush membrane in the molecular distiller is 150 r/min.
Specifically, in the step (3), the method further comprises a step of repeatedly refining the collected peony seed essential oil according to the distillation treatment manner of the step (3).
Specifically, in the step (1), the particle size of the peony seeds is controlled to be 50-100 meshes in the crushing step.
The invention also discloses the peony seed essential oil prepared by the method.
The invention also discloses application of the peony seed essential oil in preparing a monochamus alternatus development retardant.
The invention also discloses application of the peony seed essential oil in the field of biological control of the monochamus alternatus hope to effectively control the pine wilt disease.
Specifically, the method for biologically controlling monochamus alternatus hope and effectively controlling the bursaphelenchus xylophilus disease based on the paeonia lactiflora seed essential oil comprises the step of applying the paeonia lactiflora seed essential oil to pines containing monochamus alternatus hope larvae.
The method for extracting the peony seed essential oil is used for extracting the peony seed essential oil based on an organic solvent method combined with a molecular distillation method, and the mixed solvent of ethyl acetate, ethanol and petroleum ether is selected for Soxhlet extraction by optimizing various operation parameters, so that the purposes of efficient extraction and separation of the peony seed essential oil and high purity of an extracted product are achieved, and the method has the advantages of simplicity in operation, short operation time and higher extraction efficiency.
The extracted peony seed essential oil is further used for biologically controlling monochamus alternatus hope to effectively control the pine wilt disease, and by applying the peony seed essential oil to pine trees containing monochamus alternatus hope larvae before the beginning of pupation of annual monochamus alternatus hope, the pupation of the monochamus alternatus hope can be effectively blocked, so that the development of the monochamus alternatus hope larvae is stopped, the subsequent diffusion type fourth-instar nematodes formed by the pine nematodes along with the eclosion of the monochamus alternatus hope are effectively prevented, the diffusion and propagation of the pine nematodes are blocked, and the death rate and the diffusion and propagation speed of the pine in a pine nematode occurrence area are reduced. Although the effect of the monochamus alternatus hope growth retardation based on the peony seed essential oil is not ideal compared with the known chemical preparations, a new idea is provided for solving the problem of the control of the pine wilt disease.
Detailed Description
Example 1
The method for extracting peony seed essential oil based on the solvent method comprises the following steps:
(1) removing impurities from semen Paeoniae, placing into sieving equipment, drying the sieved semen Paeoniae in drying equipment at 66 deg.C for 18 hr, and pulverizing and sieving in pulverizing equipment to obtain 60 mesh semen Paeoniae crushed material;
(2) 100kg of the crushed material of the peony seeds is put into a soxhlet extraction device, and the weight ratio of the crushed material to the crushed material is 1: 4, adding an organic extraction solvent (the volume ratio of ethyl acetate to ethanol to petroleum ether is 1: 2: 5) in a mass ratio, dispersing and soaking for 1h, then heating to 80 ℃, performing heat preservation extraction for 3h, collecting an extracting solution containing crude oil of the peony seeds, performing reduced pressure concentration, and recovering the organic extraction solvent to obtain crude oil of the peony seeds;
(3) adding the prepared primary peony seed essential oil crude product into a molecular distiller, setting the vacuum degree in the molecular distiller to be 1.9Pa, the temperature to be 77 ℃ and the rotating speed of a rotary brush membrane in the molecular distiller to be 120r/min until the primary peony seed essential oil crude product is completely collected by a heavy phase collecting tank and a light phase collecting tank, and collecting in the heavy phase collecting tank to obtain peony seed essential oil;
(4) adding the collected peony seed essential oil into the molecular distiller again, resetting the vacuum degree in the molecular distiller to be 1.2Pa, the temperature to be 67 ℃, and the rotating speed of a rotary brush membrane in the molecular distiller to be 120r/min until the peony seed essential oil is completely collected by the heavy phase collection tank and the light phase collection tank, and collecting in the heavy phase collection tank to obtain the peony seed essential oil.
Example 2
The method for extracting peony seed essential oil based on the solvent method comprises the following steps:
(1) removing impurities from semen Paeoniae, placing into sieving equipment, drying the sieved semen Paeoniae in drying equipment at 60 deg.C for 18 hr, and pulverizing and sieving in pulverizing equipment to obtain 50-100 mesh semen Paeoniae crushed material;
(2) 100kg of the crushed material of the peony seeds is put into a soxhlet extraction device, and the weight ratio of the crushed material to the crushed material is 1: 4, adding an organic extraction solvent (the volume ratio of ethyl acetate to ethanol to petroleum ether is 1: 2: 5) in a mass ratio, dispersing and soaking for 1h, then heating to 85 ℃ for heat preservation and extraction for 3h, collecting an extracting solution containing crude oil of the peony seeds, performing reduced pressure concentration, and recovering the organic extraction solvent to obtain crude oil of the peony seeds;
(3) adding the prepared crude product of the primary peony seed essential oil into a molecular distiller, setting the vacuum degree in the molecular distiller to be 1.5Pa, the temperature to be 70 ℃, and the rotating speed of a rotary brush membrane in the molecular distiller to be 120r/min until the primary peony seed crude oil is completely collected by a heavy phase collection tank and a light phase collection tank, and collecting in the heavy phase collection tank to obtain the peony seed essential oil;
(4) adding the collected peony seed essential oil into the molecular distiller again, resetting the vacuum degree in the molecular distiller to be 1.5Pa, the temperature to be 70 ℃, and the rotating speed of a rotary brush membrane in the molecular distiller to be 120r/min until the peony seed essential oil is completely collected by the heavy phase collection tank and the light phase collection tank, and collecting in the heavy phase collection tank to obtain the peony seed essential oil.
Example 3
The method for extracting peony seed essential oil based on the solvent method comprises the following steps:
(1) removing impurities from semen Paeoniae, placing into sieving equipment, drying the sieved semen Paeoniae in drying equipment to 40 deg.C, pulverizing in pulverizing equipment, and sieving to obtain 80 mesh semen Paeoniae crushed material;
(2) 100kg of the crushed material of the peony seeds is put into a soxhlet extraction device, and the weight ratio of the crushed material to the crushed material is 1: 3, adding an organic extraction solvent (the volume ratio of ethyl acetate to ethanol to petroleum ether is 1: 2: 5) in the mass ratio of the raw oil to the crude oil, dispersing and soaking for 1h, then heating to 70 ℃ for heat preservation and extraction for 3h, collecting an extracting solution containing crude oil of the peony seeds, carrying out reduced pressure concentration, and recovering the organic extraction solvent to obtain crude oil of the peony seeds;
(3) adding the prepared primary peony seed essential oil crude product into a molecular distiller, setting the vacuum degree in the molecular distiller to be 1.0Pa, the temperature to be 60 ℃ and the rotating speed of a rotary brush membrane in the molecular distiller to be 100r/min until the primary peony seed essential oil crude product is completely collected by a heavy phase collecting tank and a light phase collecting tank, and collecting in the heavy phase collecting tank to obtain peony seed essential oil;
(4) adding the collected peony seed essential oil into the molecular distiller again, resetting the vacuum degree in the molecular distiller to be 1.0Pa, the temperature to be 60 ℃, and the rotating speed of a rotary brush membrane in the molecular distiller to be 100r/min until the peony seed essential oil is completely collected by the heavy phase collection tank and the light phase collection tank, and collecting in the heavy phase collection tank to obtain the peony seed essential oil.
Example 4
The method for extracting peony seed essential oil based on the solvent method comprises the following steps:
(1) removing impurities from semen Paeoniae, placing into sieving equipment, drying the sieved semen Paeoniae in drying equipment at 60 deg.C for 18 hr, and pulverizing and sieving in pulverizing equipment to obtain 50-80 mesh semen Paeoniae crushed material;
(2) 100kg of the crushed material of the peony seeds is put into a soxhlet extraction device, and the weight ratio of the crushed material to the crushed material is 1: 5, adding an organic extraction solvent (the volume ratio of ethyl acetate to ethanol to petroleum ether is 1: 2: 5) in a mass ratio, dispersing and soaking for 1h, then heating to 90 ℃, performing heat preservation extraction for 3h, collecting an extracting solution containing crude oil of the peony seeds, performing reduced pressure concentration, and recovering the organic extraction solvent to obtain crude oil of the peony seeds;
(3) adding the prepared primary peony seed essential oil crude product into a molecular distiller, setting the vacuum degree in the molecular distiller to be 2.0Pa, the temperature to be 80 ℃ and the rotating speed of a rotary brush membrane in the molecular distiller to be 100r/min until the primary peony seed essential oil crude product is completely collected by a heavy phase collecting tank and a light phase collecting tank, and collecting in the heavy phase collecting tank to obtain peony seed essential oil;
(4) adding the collected peony seed essential oil into the molecular distiller again, resetting the vacuum degree in the molecular distiller to be 2.0Pa, the temperature to be 80 ℃, and the rotating speed of a rotary brush membrane in the molecular distiller to be 120r/min until the peony seed essential oil is completely collected by the heavy phase collection tank and the light phase collection tank, and collecting in the heavy phase collection tank to obtain the peony seed essential oil.
Examples of the experiments
1. Extraction rate of peony seed essential oil
The extraction rate of the peony seed essential oil obtained in the above examples 1 to 4 was calculated according to the following formula:
the extraction rate is (the mass of the peony essential oil/the mass of the peony seed powder) multiplied by 100%;
the calculation results are recorded in table 1 below.
TABLE 1 results of extraction rate of essential oil from peony seeds in each example
2. Diapause of monochamus alternatus hope
In a pine planting test park in Shandong province, before pupation of monochamus alternatus hopes at the end of 4 months and 5 months, 60 pinus massoniana containing monochamus alternatus larvae through detection are selected for effect verification, and the specific identification method comprises the following steps: pine trees damaged by the pine wood nematodes do not flow fat after drilling, and have traces of carving grooves of monochamus alternatus eggs, and part of pine needles lose green and yellow.
Selecting 10 plants from pine trees as experimental groups and 10 plants as blank groups, drilling holes with the diameter of 2cm and the depth of 2cm at the positions of holes eaten by monochamus alternatus hope in the sunny side xylem of the tree body, and communicating the holes with a pupa chamber of the monochamus alternatus hope.
Taking the peony seed essential oil prepared in example 1, preparing a silicone rubber stopper adsorbing the peony seed essential oil in an adsorption amount of 1 ml/piece, inserting a plurality of silicone rubber stoppers adsorbing the peony seed essential oil into holes of experimental group pine trees, and inserting 30 silicone rubber stoppers into each pine tree;
the blank pine trees were not treated at all.
After 15 days, the monochamus alternatus larvae are dissected out for observation, and the contents of the pupae and the larvae in the monochamus alternatus are respectively calculated and recorded in the following table 1.
TABLE 1 treatment of monochamus alternatus in each group
| Numbering | Content of pupa/%) | Content of larvae/%) |
| Experimental group | 51％ | 49％ |
| Blank group | 80％ | 20％ |
Therefore, in the embodiment, the paeonia lactiflora seed essential oil is added into the pine tree, so that the pupation of the monochamus alternatus hope can be effectively blocked, and the development of the monochamus alternatus hope larvae can be stopped. Although the effect of the monochamus alternatus hope growth retardation based on the peony seed essential oil is not ideal compared with the known chemical preparations, a new idea is provided for solving the problem of the control of the pine wilt disease.
The foregoing descriptions of specific exemplary embodiments of the present invention have been presented for purposes of illustration and description. It is not intended to limit the invention to the precise form disclosed, and obviously many modifications and variations are possible in light of the above teaching. The exemplary embodiments were chosen and described in order to explain certain principles of the invention and its practical application to enable one skilled in the art to make and use various exemplary embodiments of the invention and various alternatives and modifications as are suited to the particular use contemplated. It is intended that the scope of the invention be defined by the claims and their equivalents.
Claims (10)
1. A method for extracting peony seed essential oil based on a solvent method is characterized by comprising the following steps:
(1) removing impurities from semen Paeoniae, removing shell, oven drying, and pulverizing;
(2) placing the obtained peony seed crushed material in a soxhlet extraction device, adding an organic extraction solvent for heat preservation extraction, collecting an extracting solution containing crude peony seed oil, carrying out reduced pressure concentration, and recovering the organic extraction solvent to obtain a crude peony seed essential oil product;
(3) and adding the obtained crude product of the peony seed essential oil into a molecular distiller for distillation treatment until the crude product of the peony seed essential oil is completely collected by a heavy phase collection tank and a light phase collection tank, and collecting the peony seed essential oil in the heavy phase collection tank to obtain the peony seed essential oil.
2. The solvent-based extraction method of peony seed essential oil as claimed in claim 1, wherein in the step (2), the organic extraction solvent comprises a mixture of ethyl acetate, ethanol and petroleum ether.
3. The solvent-based extraction method of peony seed essential oil according to claim 1 or 2, wherein in the step (2), the volume ratio of ethyl acetate, ethanol and petroleum ether is 1: 2: 5.
4. the solvent-based extraction method of peony seed essential oil according to any one of claims 1-3, wherein in the step (2), the mass ratio of the peony seed crushed material to the organic extraction solvent is 1: 3-5.
5. The solvent-based extraction method of peony seed essential oil according to any one of claims 1-4, wherein the temperature of the incubation extraction step in the step (2) is 70-90 ℃.
6. The solvent-based extraction method of peony seed essential oil as claimed in any one of claims 1-5, wherein said step (2) further comprises the step of soaking said peony seed crushed material for 1h before the step of extracting under incubation.
7. The method for extracting peony seed essential oil based on solvent method as claimed in any one of claims 1-6, wherein in the step (3), in the distillation treatment step, the vacuum degree in the molecular still is controlled to be 1.0-2.0Pa, the temperature is controlled to be 60-80 ℃, and the rotation speed of the rotary brushing membrane in the molecular still is controlled to be 100-150 r/min.
8. The solvent-based extraction method of peony seed essential oil according to any one of claims 1-7, wherein in step (3), said method further comprises the step of repeatedly refining the collected peony seed essential oil according to the distillation treatment of step (3).
9. The solvent-based extraction method of essential oil of peony seeds as claimed in any one of claims 1 to 8, wherein said pulverization step in step (1) controls the particle size of said peony seeds to 50-100 mesh.
10. Peony seed essential oil produced by the process of any one of claims 1-9.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2013180292A1 (en) * | 2012-05-31 | 2013-12-05 | 国立大学法人 琉球大学 | Control agent and control method for pine wilt |
| CN112011400A (en) * | 2020-09-03 | 2020-12-01 | 菏泽瑞璞牡丹产业科技发展有限公司 | New application of Chinese herbaceous peony |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013180292A1 (en) * | 2012-05-31 | 2013-12-05 | 国立大学法人 琉球大学 | Control agent and control method for pine wilt |
| CN112011400A (en) * | 2020-09-03 | 2020-12-01 | 菏泽瑞璞牡丹产业科技发展有限公司 | New application of Chinese herbaceous peony |
Non-Patent Citations (2)
| Title |
|---|
| 查素娥 等: "芍药籽油与牡丹籽油成分比较分析", 《种业导刊》, no. 11, pages 22 - 24 * |
| 郝德君 等: "松墨天牛化学生态学", 《生态学杂志》, vol. 27, no. 07, pages 1227 - 1233 * |
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