CN104673496B - A kind of snow deposit azalea oil and its application - Google Patents
A kind of snow deposit azalea oil and its application Download PDFInfo
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- CN104673496B CN104673496B CN201510075114.7A CN201510075114A CN104673496B CN 104673496 B CN104673496 B CN 104673496B CN 201510075114 A CN201510075114 A CN 201510075114A CN 104673496 B CN104673496 B CN 104673496B
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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
- C11B9/027—Recovery of volatiles by distillation or stripping
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/45—Ericaceae or Vacciniaceae (Heath or Blueberry family), e.g. blueberry, cranberry or bilberry
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- A61K2236/00—Isolation or extraction methods of medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicine
- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/331—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using water, e.g. cold water, infusion, tea, steam distillation, decoction
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Abstract
The present invention provides a kind of snow deposit azalea oil, and the snow deposit azalea oil is 15 20 times of distilled water of addition in dry snow deposit cuckoo, and after soaking 8 14h, distillation 10 14h of extraction, to volatilizing, oil volume no longer increases, and goes what upper strata obtained after standing.The present invention also provides it and is preparing the application in treating animal acariasis medicine.The yield of the snow deposit azalea oil of the present invention is up to 2.45%, and 76 kinds of compounds are obtained using the GC MS chromatographic processes analysis after improvement.The snow deposit azalea oil of the present invention has good therapeutic effect to animal acariasis, and has drug concentration dependence, available for treatment animal acariasis.
Description
Technical field
The present invention relates to a kind of snow deposit azalea oil.
Background technology
Snow deposit cuckoo（Rhododendron nivaleHook. f.）It is normal for one kind of Ericaceae rhododendron
Green undershrub, it is distributed in the Tibet, China southeast, south, east and northeast.Nepal, India, Bhutan, Sillim also have point
Cloth.It is born in alpine scrub, glacier valley floor, grassy marshland, height above sea level 3200-5800 rice.Spray, the leaf of snow deposit cuckoo are dispelled available for antibechic
Phlegm.But also no one conducts a research to its chemical composition and pharmacological activity at present.
Animal acariasis is a kind of animal chronic epizoonosis caused by acarid parasitic animal body surface, is taken place mostly in
Qiu Mo, winter and the early spring, be directly or indirectly infected by contact with healthy animal by infected animal, betide extensively ox, sheep, horse,
The animals such as dog, rabbit, chicken, it can also infect and give people, it is higher in pastoral area, farming and pastoral area and scale livestock farming infection rate and the incidence of disease.
Animal occur the disease be mainly shown as appetite reduce or it is useless absolutely, become thin, hair comes off, influence the production performance and economy of animal
Value is serious to restrict animal husbandry sound development and economic benefit.The medicine for being presently used for treating animal acariasis is mainly that chemistry closes
Into and antibiotics, such as ivermectin, mite it is net, such medicine is while effectively preventing and treating animal acariasis, due to medicine
Residual, the problems such as causing public health, food security and ecological environment again.
The content of the invention
The invention provides a kind of snow deposit azalea oil, and the snow deposit azalea oil is preparing treatment animal acariasis
Application in medicine.
The present invention provides a kind of snow deposit azalea oil, and the snow deposit azalea oil is added in dry snow deposit cuckoo
Enter 15-20 times of distilled water, after soaking 8-14h, distillation extraction 10-14h, oil volume no longer increases to volatilizing, and upper strata is gone to after standing
Obtain.
Second object of the present invention is to provide a kind of preparation method of snow deposit azalea oil, and step is as follows：In drying
Snow deposit cuckoo in add 15-20 times of distilled water, soak 8-14h after, distillation extraction 10-14h, to volatilize oil volume no longer increase
Add, upper strata is gone to after standing, obtain the snow deposit azalea oil of the present invention.
Third object of the present invention is to provide the analysis method of active ingredient in above-mentioned snow deposit azalea oil, specifically such as
Under：Snow deposit azalea oil is detected with gas chromatography-mass spectrometry, wherein, chromatographic condition：Chromatographic column is HP-5MS stones
English capillary column, column temperature：35 DEG C of holding 2min of temperature programming；80 DEG C are risen to 5 DEG C/min, keeps 3min；Again with 8 DEG C/min
130 DEG C are risen to, keeps 2min；140 DEG C are risen to 0.5 DEG C/min again, keeps 6min；150 DEG C are risen to 2 DEG C/min again, is kept
2min；260 DEG C of injector temperature, the μ L of sample size 10；Carrier gas He, flow velocity 1mL/min-1, split ratio 50:1；Mass Spectrometry Conditions：Electricity
It is EI from mode；Electron energy 70eV；150 DEG C of quadrupole rod temperature；230 DEG C of ion source temperature；Bulk delay 2min；Full scan
Drainage pattern；Quality of scanning number scope is 30~550m/z, and mass spectrometric data storehouse is NIST11.
Fourth object of the present invention is to provide above-mentioned snow deposit azalea oil in treatment animal acariasis medicine is prepared
Using.
The 5th purpose of the present invention is to provide a kind of medicine for treating animal acariasis, and the medicine includes claim 1
Described snow deposit azalea oil.
Preferably, in addition to medically acceptable pharmaceutic adjuvant, excipient.
Preferably, the formulation of the medicine is solution, injection, sustained release preparation and nanometer formulation.
Further, in the medicine, the concentration of snow deposit azalea oil is 8.33mg/ml-33.33mg/ml.
It is highly preferred that in the medicine, the concentration of snow deposit azalea oil is 16.67mg/ml-33.33mg/ml.
A variety of formulations can be made directly or after inclusion in the snow deposit azalea oil of the present invention：Solution（As aromatic waters,
Spray, emulsion etc.）, injection, the formulation such as sustained release preparation and nanometer formulation.Can be using snow deposit azalea oil as active matter
Matter, with the mixture such as medically acceptable pharmaceutic adjuvant, excipient, combine, be made according to method of the prior art above-mentioned each
Kind formulation；Can also with other treatment animal acariasis medicine collectively as active material, with medically acceptable pharmaceutic adjuvant,
The mixtures such as excipient, combination, are made above-mentioned various formulations.
The yield of snow deposit azalea oil of the present invention is up to 2.45%, and far above 2008 Liu Ying etc. use vapor
Distill the yield of extraction（0.68%）, and analyzed using the GC-MS chromatographic processes after improving and obtain 76 kinds of compounds, and 2008
Liu Ying etc. is extracted using steam distillation, only obtains 45 kinds of compounds using GC-MS analyses, its analysis method is:PyeUnicam
The gas chromatograph chromatographic columns of GC 304 are OV-101WCOT quartz capillary columns, caliber 0.26mm, column length 30m;Column temperature 80 ~ 200
DEG C, risen with 4 DEG C/min speed, carrier gas is helium, and split ratio is 25B1.Finnigan INCOS-50 GC/MS/DS combinations
Instrument, SE-54WCOT quartz capillary columns, the mm of caliber 0.24, the m of column length 30;90 ~ 180e of column temperature, risen with 5 DEG C/min speed,
EI-MS, 70eV, computer use INCOS data systems, and storehouse (NBS NBB is composed by NIH/EPA/MSDC
LIBRARY composes storehouse).
The snow deposit azalea oil of the present invention has good therapeutic effect to animal acariasis, and has drug concentration dependence
Property, high dose (33.33mg/ml) is cultivated in vitro all kills itch mite in 3 hours, 16.67mg/ml dosage is in 24 hours
Kill whole itch mites；8.33mg/ml dosage acaricidal rate in 24 hours is also up to 92.5%, available for treatment animal acariasis.
Embodiment
Following embodiment facilitates a better understanding of the present invention, but does not limit the present invention.Experiment in following embodiments
Method, it is conventional method unless otherwise specified.Test material used in following embodiments, it is certainly unless otherwise specified
What routine biochemistry reagent shop was commercially available.
Plant Ericaceae Rhododendron snow deposit cuckoo used in the present invention（Rhododendron nivale Hook. f.
）, pick up from Sehgyla Mountains, Tibet north slope height above sea level 4300m.
Embodiment 1
The preparation method of the snow deposit azalea oil of the present invention is as follows：
After fresh snow deposit cuckoo cauline leaf is dried in the shade, dry snow deposit cuckoo cauline leaf 100g is weighed, is put into volatile oil extracting
Device, add distilled water 1500mL, after soaking 8h, distillation extraction 8h, oil volume no longer increases to volatilizing, and upper strata is gone to after standing, must be waved
Hair oil.Yield is 2.01%.
Embodiment 2
The preparation method of the snow deposit azalea oil of the present invention is as follows：
After fresh snow deposit cuckoo cauline leaf is dried in the shade, dry snow deposit cuckoo cauline leaf 100g is weighed, is put into volatile oil extracting
Device, add distilled water 1700mL, after soaking 10h, distillation extraction 12h, oil volume no longer increases to volatilizing, and upper strata is gone to after standing, is obtained
Volatile oil.Yield is 2.23%.
Embodiment 3
The preparation method of the snow deposit azalea oil of the present invention is as follows：
After fresh snow deposit cuckoo cauline leaf is dried in the shade, dry snow deposit cuckoo cauline leaf 100g is weighed, is put into volatile oil extracting
Device, add distilled water 2000mL, after soaking 14h, distillation extraction 14h, oil volume no longer increases to volatilizing, and upper strata is gone to after standing, is obtained
Volatile oil.Yield is 2.43%.
Embodiment 4
The preparation method of the snow deposit azalea oil of the present invention is as follows：
After fresh snow deposit cuckoo cauline leaf is dried in the shade, dry snow deposit cuckoo cauline leaf 100g is weighed, is put into volatile oil extracting
Device, add distilled water 1800mL, after soaking 12h, distillation extraction 12h, oil volume no longer increases to volatilizing, and upper strata is gone to after standing, is obtained
Volatile oil.Yield is 2.45%.
By the snow deposit azalea oil that present invention extraction obtains through ether extraction and anhydrous sodium sulfate drying, take upper strata clear
Liquid, detected with gas chromatography-mass spectrometry, wherein, chromatographic condition：Chromatographic column be HP-5MS quartz capillary columns (30m ×
0.25mm, 0.25 μm).Column temperature：35 DEG C of holding 2min of temperature programming；80 DEG C are risen to 5 DEG C/min, keeps 3min；Again with 8 DEG C/
Min rises to 130 DEG C, keeps 2min；140 DEG C are risen to 0.5 DEG C/min again, keeps 6min；150 DEG C are risen to 2 DEG C/min again, is protected
Hold 2min.260 DEG C of injector temperature, the μ L of sample size 10.Carrier gas He, flow velocity 1mL/min-1, split ratio 50:1.Mass Spectrometry Conditions：
Ionization mode is EI；Electron energy 70eV；150 DEG C of quadrupole rod temperature；230 DEG C of ion source temperature；Bulk delay 2min；Sweep entirely
Retouch drainage pattern；Quality of scanning number scope is 30~550m/z, and mass spectrometric data storehouse is NIST11.From snow deposit cuckoo flowers volatile oil
76 kinds of chemical compositions are isolated and identified, account for the 84.28% of volatile oil total amount, its main component is δ-Cadinene (12.07%),
2-Isopropyl-5-methyl-9-methylene-bicyclo-1-decene (4.4.0) (6.96%) and β-Eudesmol
(6.63%) etc..76 kinds of compounds are obtained using GC-MS chromatographic processes analysis after above-mentioned improvement.
Embodiment 5
The snow deposit azalea oil of the present invention kills acarid experiment
1. experimental animal and itch mite
Psoroptes cuniculi (Psoroptes cuniculi) it is collected in the rabbit of artificial challenge's psoroptic acariasis, the rabbit of natural infection itch mite
Son, 1.8~2.2kg of body weight, Lanzhou Institute of Biological Products's Experimental Animal Center provide.Received from the external auditory meatus of rabbit severe infections
Collect crust, be placed in glass dish, plate is then placed into 0.5h at 35 DEG C, separation under the microscope identifies itch mite, and use is soft
It is soft to choose worm pin to collect energetic itch mite standby.
2. test drug
Snow deposit azalea oil before use, volatile oil is diluted into 33.33mg/ml with 10% glycerine, 16.67mg/ml and
8.33mg/ml。
3. test method
150 μ l snow deposit azalea oils extracts of Three doses are added in 24 orifice plates, filter paper is added and draws more extraction raffinates
Body.20 itch mites are chosen in each hole successively with worm pin is chosen, using the mixture of 10% glycerine as blank control, each concentration sets 3
Individual repetition.Then 24 orifice plates are put into test environment（25 DEG C, 75% relative humidity）Middle culture, every 3 h with micro- sem observation one
It is secondary, observe 24 hours, record the death condition of each period.When polypide podomere is motionless or reactionless with needle stimulus for a long time
It is determined as death.
4. result
As a result show, snow deposit azalea oil has very strong external insecticidal action.High dose (33.33mg/ml) is in body
Outer culture all kills itch mite in 3 hours, and 16.67mg/ml dosage killed whole itch mites in 24 hours.Refer to table 1.
The external of the snow deposit azalea oil of table 1 kills itch mite activity
。
Finally it should be noted that：The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention,
Although the present invention is described in detail with reference to the foregoing embodiments, for those skilled in the art, it still may be used
To be modified to the technical scheme described in foregoing embodiments, or equivalent substitution is carried out to which part technical characteristic.
Within the spirit and principles of the invention, any modification, equivalent substitution and improvements made etc., it should be included in the present invention's
Within protection domain.
Claims (1)
1. snow deposit azalea oil is preparing the application in treating animal acariasis medicine；Wherein, the snow deposit azalea oil
Preparation method is：15-20 times of distilled water is added in dry snow deposit cuckoo, after soaking 8-14h, distillation extraction 10-14h, extremely
Volatilization oil volume no longer increases, and upper strata is gone to after standing, obtains snow deposit azalea oil.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101716218A (en) * | 2009-12-02 | 2010-06-02 | 中国科学院西北高原生物研究所 | Process for extracting rhododendron oil |
| CN102428973A (en) * | 2011-10-18 | 2012-05-02 | 浙江农林大学 | Agricultural pesticide with essential oil and application thereof |
| CN102784350A (en) * | 2012-08-07 | 2012-11-21 | 孙雅儒 | Mite killing bactericide and preparation method of mite killing bactericide |
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2015
- 2015-02-12 CN CN201510075114.7A patent/CN104673496B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101716218A (en) * | 2009-12-02 | 2010-06-02 | 中国科学院西北高原生物研究所 | Process for extracting rhododendron oil |
| CN102428973A (en) * | 2011-10-18 | 2012-05-02 | 浙江农林大学 | Agricultural pesticide with essential oil and application thereof |
| CN102784350A (en) * | 2012-08-07 | 2012-11-21 | 孙雅儒 | Mite killing bactericide and preparation method of mite killing bactericide |
Non-Patent Citations (3)
| Title |
|---|
| 日本花柏树皮精油的活性成分;刘志明等;《经济林研究》;20110630;第29卷(第2期);摘要 * |
| 藏药樱草杜鹃挥发油的GC-MS分析;吴奶珠等;《药物分析杂志》;20101031;第30卷(第10期);全文 * |
| 西藏雪层杜鹃挥发油化学成分分析;刘灏等;《华南农业大学学报》;20081031;第29卷(第4期);第118页第2节第1段 * |
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