CN101612175B - Separation and identification of syringa amurensis rupr. bark volatile oil components and novel application - Google Patents
Separation and identification of syringa amurensis rupr. bark volatile oil components and novel application Download PDFInfo
- Publication number
- CN101612175B CN101612175B CN2009101457259A CN200910145725A CN101612175B CN 101612175 B CN101612175 B CN 101612175B CN 2009101457259 A CN2009101457259 A CN 2009101457259A CN 200910145725 A CN200910145725 A CN 200910145725A CN 101612175 B CN101612175 B CN 101612175B
- Authority
- CN
- China
- Prior art keywords
- volatile oil
- ether
- bark
- syringa
- reticulata var
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Classifications
-
- 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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Medicines Containing Plant Substances (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention belongs to the technical field of the research and development of medical products, and relates to the separation and identification of syringa amurensis rupr. bark volatile oil and a novel application. In the invention, syringa amurensis rupr. barks are taken, cut up after being dried, and processed by ultrasonic for one hour after being soaked by using distilled water for 6 to 8 hours, the temperature is 30 DEG C, and the power is 80W; medicinal materials and soaking liquid are poured into a volatile oil extractor together and are extracted for 4 to 5 hours by adopting a steam distillation method; a water layer is discharged, and the volatile oil extractor is repeatedly washed by ether to enable syringa amurensis rupr. volatile oil to be fully dissolved into the ether; and ether solution dissolved with the volatile oil is poured into a beaker, then anhydrous sodium sulfate is added into the beaker to suck up water, pure volatile oil is obtained after the ether is recovered, and the pure volatile oil is put into a refrigerator of 4 DEG C and preserved for standby. The syringa amurensis rupr. bark volatile oil is analyzed by using a 6890/5973N gas phase color spectrum and mass spectrum united instrument, and comprises the main chemical components of 27.46% of n-hexadecanoic acid, 28.52% of 9,12-octadecadienoic acid (Z,Z), 14.16% of 9,17-octadecadienal and 2.44% of tricosane. The syringa amurensis rupr. bark volatile oil has a suppressing function with different degrees for colibacillus, staphyiococcus aureus, pasteurella, streptococci and salmonella, can be developed into a natural antimicrobial agent applied to the industries of foods, medicines and the like, and can prepare various forms of products with a bacteriostatic function.
Description
Technical field
Medical product research and development technical field under the present invention.The present invention relates to the isolation identification and the purposes of syringa reticulata var mandshurica Syringa amurensis Rupr. bark volatile oil.
Background technology
Syringa reticulata var mandshurica Syringa amurensis Rupr. is one of common medicinal plants in Changbai Mountain, mainly is distributed in Jilin, Liaoning, North China, northwest and Central China, aboundresources in China.Bark, trunk and branch are all pharmaceutically acceptable, bitter in the mouth, cold nature, experimental results show that through modern pharmacology have lung heat clearing away, sputum eliminating, cough-relieving, relieving asthma, antiinflammatory, diuretic function.
At present, isolation identification and chemical constituent and the rarely seen report of pharmacological research about the syringa reticulata var mandshurica bark volatile oil only have several pieces of reports to separate from bark, branch and obtain several chemical compounds, the syringa reticulata var mandshurica bark volatile oil are not done antibacterial research.Therefore, the present invention adopts steam distillation that medicinal plants syringa reticulata var mandshurica bark volatile oil is extracted, and utilizes the 6890/5973N gas chromatogram to separate with the mass spectrometry instrument and identify, and the syringa reticulata var mandshurica bark volatile oil has been carried out bacteriostatic test.
Syringa reticulata var mandshurica bark volatile oil of the present invention is inhibited to gram positive bacteria, gram negative bacteria, and this bacteriostasis has positive using value.
Summary of the invention
The objective of the invention is syringa reticulata var mandshurica bark volatile oil composition is extracted, separates and identify and the syringa reticulata var mandshurica bark volatile oil is carried out bacteriostatic test, be beneficial to aspect antibacterial and develop and apply.
Syringa reticulata var mandshurica bark volatile oil composition of the present invention all has inhibitory action in various degree to escherichia coli, staphylococcus aureus, Pasteur bacterium, streptococcus, Salmonella, can be developed as natural antibacterial agent and be applied to industries such as food, medicine, prepare various forms of products with bacteriostasis.
1. the present invention relates to the isolation identification and the new purposes of syringa reticulata var mandshurica Syringa amurensis Rupr. bark volatile oil.Get the syringa reticulata var mandshurica bark, shred after the drying, with ultrasonic 1h behind the distilled water immersion 6-8h, temperature is that 30 ℃ of power are 80W.Medical material and soak are together poured in the volatile oil extractor, adopted steam distillation to extract 4-5h.Emit water layer, wash volatile oil extractor repeatedly, syringa reticulata var mandshurica volatile oil fully is dissolved in the ether with ether.The diethyl ether solution that is dissolved with volatile oil is poured in the beaker, added the anhydrous sodium sulfate suck dry moisture again in beaker, promptly obtain purified volatile oil after reclaiming ether, it is standby to put into 4 ℃ of preservations of refrigerator.
The syringa reticulata var mandshurica bark volatile oil is analyzed with 6890/5973N gas chromatogram and mass spectrometry instrument, syringa reticulata var mandshurica volatile oil main chemical compositions is n-Hexadecanoic acid (27.46%), 9,12-Octadecadienoic acid (Z, Z)-(28.52%), 9,17-Octadecadienal (14.16%) and Tricosane (2.44%).
2. the extraction of syringa reticulata var mandshurica bark volatile oil, separation and evaluation is characterized in that this technology comprises following process:
(1) get the syringa reticulata var mandshurica bark, choose the roguing thing, washing is dried or is dried, and pulverizes, and with ultrasonic 1h behind the distilled water immersion 6-8h, temperature is that 30 ℃ of power are 80W;
(2) (1) Chinese crude drug and soak are together poured in the volatile oil extractor, adopted steam distillation to extract 4-5h, edema over the face has the aqueous solution of volatile oil in the acquisition;
(3) there is the aqueous solution of volatile oil to emit water layer with going up edema over the face in (2), wash volatile oil extractor repeatedly with ether, make syringa reticulata var mandshurica volatile oil fully be dissolved in the ether, the diethyl ether solution that is dissolved with volatile oil is poured in the beaker, in beaker, add the anhydrous sodium sulfate suck dry moisture again, promptly obtain purified volatile oil after reclaiming ether, it is standby to put into 4 ℃ of preservations of refrigerator.
(4) syringa reticulata var mandshurica bark volatile oil in (3) is analyzed with 6890/5973N gas chromatogram and mass spectrometry instrument, syringa reticulata var mandshurica volatile oil main chemical compositions is n-Hexadecanoic acid (27.46%), 9,12-Octadecadienoic acid (Z, Z)-(28.52%), 9,17-Octadecadienal (14.16%) and Tricosane (2.44%).
3. the raw material of 1 to 2 described preparation syringa reticulata var mandshurica bark volatile oil is the bark of syringa reticulata var mandshurica Syringaamurensis Rupr. according to the present invention.
4. 1 to 2 described syringa reticulata var mandshurica bark volatile oil all has inhibitory action in various degree to escherichia coli, staphylococcus aureus, Pasteur bacterium, streptococcus, Salmonella according to the present invention.
5. 1 to the 2 described syringa reticulata var mandshurica bark volatile oil according to the present invention is characterized in that this bark volatile oil can be used as natural antibacterial agent and is used for industries such as food, medicine, replaces the synthetic antibacterial agents of toxic side effect.
According to the present invention, " % " among the present invention is percentage by weight.
The specific embodiment
Extraction, separation and the evaluation of syringa reticulata var mandshurica bark volatile oil composition of the present invention comprise following examples, and the following examples can further specify the present invention, but do not limit the present invention in any way.
Embodiment 1:
(1) get syringa reticulata var mandshurica bark 100g, choose the roguing thing, washing is dried or is dried, and pulverizes, and soaks ultrasonic 1h behind the 6h with distilled water 300mL, and temperature is that 30 ℃ of power are 80W;
(2) (1) Chinese crude drug and soak are together poured in the volatile oil extractor, adopted steam distillation to extract 4h, edema over the face has the aqueous solution of volatile oil in the acquisition;
(3) there is the aqueous solution of volatile oil to emit water layer with going up edema over the face in (2), wash volatile oil extractor repeatedly with ether, make syringa reticulata var mandshurica volatile oil fully be dissolved in the ether, the diethyl ether solution that is dissolved with volatile oil is poured in the beaker, in beaker, add the anhydrous sodium sulfate suck dry moisture again, promptly obtain purified volatile oil after reclaiming ether, it is standby to put into 4 ℃ of preservations of refrigerator.
(4) syringa reticulata var mandshurica bark volatile oil in (3) is analyzed with 6890/5973N gas chromatogram and mass spectrometry instrument, syringa reticulata var mandshurica volatile oil main chemical compositions is n-Hexadecanoic acid (27.46%), 9,12-Octadecadienoic acid (Z, Z)-(28.52%), 9,17-Octadecadienal (14.16%) and Tricosane (2.44%).
Embodiment 2:
(1) get syringa reticulata var mandshurica bark 200g, choose the roguing thing, washing is dried or is dried, and pulverizes, and soaks ultrasonic 1h behind the 8h with distilled water 600mL, and temperature is that 30 ℃ of power are 80W;
(2) (1) Chinese crude drug and soak are together poured in the volatile oil extractor, adopted steam distillation to extract 5h, edema over the face has the aqueous solution of volatile oil in the acquisition;
(3) there is the aqueous solution of volatile oil to emit water layer with going up edema over the face in (2), wash volatile oil extractor repeatedly with ether, make syringa reticulata var mandshurica volatile oil fully be dissolved in the ether, the diethyl ether solution that is dissolved with volatile oil is poured in the beaker, in beaker, add the anhydrous sodium sulfate suck dry moisture again, promptly obtain purified volatile oil after reclaiming ether, it is standby to put into 4 ℃ of preservations of refrigerator.
(4) syringa reticulata var mandshurica bark volatile oil in (3) is analyzed with 6890/5973N gas chromatogram and mass spectrometry instrument, syringa reticulata var mandshurica volatile oil main chemical compositions is n-Hexadecanoic acid (27.46%), 9,12-Octadecadienoic acid (Z, Z)-(28.52%), 9,17-Octadecadienal (14.16%) and Tricosane (2.44%), chemical constituent sees Table 2 in detail.
Pharmacological test example: the bacteriostasis of syringa reticulata var mandshurica bark volatile oil
1 experiment material
Escherichia coli, streptococcus, Salmonella, Pasteur bacterium and staphylococcus aureus all come from American Type Culture Collecti (ATCC), cultivate 12h for 37 ℃ in the peptone steamed beef soup.
Culture medium is a beef-protein medium.Use fluid medium when activation of bacterium and cultivation, consist of: Carnis Bovis seu Bubali cream: peptone: sodium chloride: distilled water (3: 10: 5: 1000).Use solid medium when preservation of bacterium and bacteriostatic experiment, consist of: Carnis Bovis seu Bubali cream: peptone: sodium chloride: agar: distilled water (3: 10: 5: 22: 1000).
2 experimental techniques
2.1 culture medium preparation
Get Carnis Bovis seu Bubali cream 0.6g, peptone 2g, sodium chloride 1g, distilled water 200ml, mix and stir that it is dissolved fully, be made into fluid medium.Measure fluid medium with graduated cylinder, its average mark is contained in the triangular flask of 10 50ml every bottle of 20ml.Get Carnis Bovis seu Bubali cream 3g, peptone 10g, sodium chloride 5g, agar 22g, distilled water 1000ml, be placed on the Electric stove after the mixing and heat, agar is dissolved fully, be made into solid medium.Measure solid medium with graduated cylinder, its average mark is contained in the triangular flask of 5 150ml every bottle of 100ml.The triangular flask bottleneck is all wrapped up with the tampon jam-pack and with kraft paper.
2.2 sterilization
The solid medium, the fluid medium that prepare are all put into high-pressure sterilizing pot and sterilized, and when temperature rose to 121 ℃, 20min picked up counting.Experiment equipments such as culture dish, graduated cylinder, tweezers, shears, 6mm filter paper (being placed in the small beaker), dropper, ammonia bottle are all put into 170 ℃ of sterilizations of baking oven 2h.Experiment is preceding with 75% ethanol wiping superclean bench and ultraviolet sterilization 20min.37 ℃ of constant incubators need be sterilized with 75% ethanol wiping before use.
2.3 the cultivation of bacterium with look into bacterium
5 strains are poured in the triangular flask that fluid medium is housed on superclean bench, under the alcohol burner environment, and every kind of bacterium is cultivated two parts.These 10 triangular flasks are put into shaking table shake bacterium 6h for 37 ℃.Microscope begins to look into bacterium after doing microscopy, and record data also calculate bacteria concentration, if 5 medium square total bacteria counts are A, bacterium liquid extension rate is B, then total bacteria count=A/5 * 25 * 10000 * 13=50000AB in the 1ml bacterium liquid
2.4 the preparation of sample liquid and filter paper
The syringa reticulata var mandshurica bark volatile oil is mixed with the solution (can add 0～4 μ L dimethyl sulfoxide and help appearance) of 5mg/ml, by 1: 2
nBe diluted to the solution of 2.5mg/ml, 1.25mg/ml, 0.625mg/ml, 0.3125mg/ml.Filter paper is broken into the disk that diameter is 6mm with card punch, at superclean bench filter paper is put in each gradient sample and soaked 2h.
2.5 the preparation of bacterio-agar flat board is arranged
The bacterium liquid that dilution is good mixes with solid medium and rocks evenly, and this moment, the concentration of bacterium should reach 3.6 * 10
8CFU/ml.To there be bacterium culture medium to pour into successively in each culture dish, and rock culture dish and make culture medium be layered on the culture dish bottom equably, and be cooled to and solidify.
2.6 bacteriostatic experiment method
, in that label on the bacterio-agar flat board is arranged soaked filter paper is pressed from both sides out with tweezers with marking pen, puts into the culture dish of writing corresponding contrast numbering, each sample do three parallel, put into 37 ℃ of constant incubators and cultivate.
3. experimental result
Fungistatic effect is represented (mm of unit) with antibacterial circle diameter DD.
12h, 24h after bacteriostatic experiment finishes, 36h, 48h observe the growing state of bacterium, measure antibacterial circle diameter and record.
The bacteriostatic activity of table 1 syringa reticulata var mandshurica bark volatile oil
The result shows: the syringa reticulata var mandshurica bark volatile oil all has inhibitory action in various degree to escherichia coli, staphylococcus aureus, Pasteur bacterium, streptococcus, Salmonella.
Can be used as natural antibacterial agent by concrete embodiment explanation syringa reticulata var mandshurica bark volatile oil and be used for industries such as food, medicine, replace the synthetic antibacterial agents of toxic side effect.
Table 2 syringa reticulata var mandshurica chemical composition of volatile oil
Claims (2)
1. the isolation and identification method of a syringa reticulata var mandshurica bark volatile oil is characterized in that may further comprise the steps:
(1), get the syringa reticulata var mandshurica bark, shred after the drying, with ultrasonic 1h behind the distilled water immersion 6-8h, temperature is 30 ℃, power is 80W;
(2), medical material and soak are together poured in the volatile oil extractor into employing steam distillation extraction 4-5h;
(3), emit water layer, wash volatile oil extractor repeatedly with ether, make syringa reticulata var mandshurica volatile oil fully be dissolved in the ether;
(4), the diethyl ether solution that will be dissolved with volatile oil pours in the beaker, adds the anhydrous sodium sulfate suck dry moisture again in beaker, promptly obtains purified volatile oil after reclaiming ether, it is standby to put into 4 ℃ of preservations of refrigerator;
(5), gained syringa reticulata var mandshurica bark volatile oil 6890/5973N gas chromatogram and GC-MS analysis in the step (four), its main chemical compositions is 27.46% n-hexadecylic acid, 28.52% Z, Z-9, the 12-octadecadienoic acid, 14.16%Z-9,17-18 carbon two olefine aldehydrs, 2.44% tricosane.
2. the purposes of a kind of syringa reticulata var mandshurica bark volatile oil as claimed in claim 1 in the inhibitor of preparation inhibition escherichia coli, streptococcus, Salmonella, Pasteur bacterium, staphylococcus aureus.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101457259A CN101612175B (en) | 2009-05-31 | 2009-05-31 | Separation and identification of syringa amurensis rupr. bark volatile oil components and novel application |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2009101457259A CN101612175B (en) | 2009-05-31 | 2009-05-31 | Separation and identification of syringa amurensis rupr. bark volatile oil components and novel application |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101612175A CN101612175A (en) | 2009-12-30 |
| CN101612175B true CN101612175B (en) | 2011-07-06 |
Family
ID=41492183
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2009101457259A Expired - Fee Related CN101612175B (en) | 2009-05-31 | 2009-05-31 | Separation and identification of syringa amurensis rupr. bark volatile oil components and novel application |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101612175B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106309516B (en) * | 2016-11-02 | 2020-02-21 | 南京中医药大学 | Annona squamosa pericarp volatile oil extract with anti-tumor activity and preparation method and application thereof |
| CN106867674B (en) * | 2017-02-14 | 2021-01-05 | 山东大学 | Extraction, purification and detection method of bean curd vegetable volatile oil and application thereof |
| CN106833904B (en) * | 2017-03-31 | 2020-10-09 | 山东大学 | Extraction, purification and detection method of chiseled volatile oil and application thereof |
| CN107164096B (en) * | 2017-05-27 | 2021-03-02 | 山东大学 | Method for extracting, purifying and detecting volatile oil of aidi grass and application thereof |
-
2009
- 2009-05-31 CN CN2009101457259A patent/CN101612175B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN101612175A (en) | 2009-12-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Wei et al. | Preparation, chemical constituents and antimicrobial activity of pyroligneous acids from walnut tree branches | |
| Hindi | In vitro antibacterial activity of aquatic garlic extract, apple vinegar and apple vinegar-garlic extract combination | |
| CN102028646A (en) | Thyme perfume | |
| CN103432047A (en) | Natural preservative composition and application thereof in cosmetics | |
| CN101612175B (en) | Separation and identification of syringa amurensis rupr. bark volatile oil components and novel application | |
| CN103340928A (en) | Antibacterial insecticidal essential oil composition and preparation method thereof | |
| Rani et al. | Evaluation of antibacterial activity of pongamia pinnata linn on pathogens of clinical isolates | |
| CN104327952A (en) | Pelargonium odoratissimum essential oil and extraction method and application of essential oil | |
| CN103584253B (en) | Natural preservative with leaf mustard leaves and camphor tree leaves used as raw materials, as well as preparation method and application of natural preservative | |
| CN101574093A (en) | New preparation technology and new applications of syringa amurensis rupr bar volatile oil | |
| CN109792990A (en) | Plants essential oil inhibits the application of mould in air in museum | |
| CN102585997B (en) | Isolation and identification as well as application of volatile oil elements of Parasenecio firmus leaf | |
| CN103484393A (en) | Klebsiella inoculum capable of biodegrading residual chlorpyrifos pesticide on surfaces of garden stuffs and soil | |
| CN105124716B (en) | The method for preparing food preservative using Chinese cassia tree oil extract waste liquid | |
| CN108208137A (en) | Antimicrobial antistaling agent for fresh-keeping of vegetables and its preparation method and application | |
| CN102520096A (en) | Separating identification and application of Farges meehania root volatile oil component | |
| CN101559087B (en) | New technique for preparing extract of Syringa amurensis Rupr bark and new applications thereof | |
| CN103122312A (en) | Microorganism composition for degrading acetochlor and/or butachlor and application of microorganism composition | |
| Ariffin et al. | Optimization of pyroligneous acid production from palm kernel shell and its potential antibacterial and antibiofilm activities | |
| CN109350570A (en) | A kind of cosmetics preservative and its application based on natural plant composition | |
| Nanthakumar et al. | IN VITRO ANTIMICROBIAL ACTIVITY OF AQUEOUS AND ETHANOL EXTRACTS OF RHINACANTHUS NASUTUS-A MEDICINAL PLANT. | |
| CN108938475A (en) | A kind of plant source antiseptic agent and its application in cosmetics | |
| Sujina et al. | Assessing the anticancer, anti-inflammatory, antimicrobial and antioxidant potential of bioactive compounds present in marine algae Ulva lactuca | |
| Shola et al. | The effect of fractionation of the essential oil from pinus syvestris on the synergistic and antagonistic medicinal activities | |
| CN101574094A (en) | New preparation technology and new applications of syringa amurensis rupr bar extract components |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20110706 Termination date: 20130531 |