CN106632517B - The extracting method of Jasmonate with analgesic activity - Google Patents
The extracting method of Jasmonate with analgesic activity Download PDFInfo
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- CN106632517B CN106632517B CN201610869546.XA CN201610869546A CN106632517B CN 106632517 B CN106632517 B CN 106632517B CN 201610869546 A CN201610869546 A CN 201610869546A CN 106632517 B CN106632517 B CN 106632517B
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- C07C51/42—Separation; Purification; Stabilisation; Use of additives
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/47—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
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- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/52—Separation; Purification; Stabilisation; Use of additives by change in the physical state, e.g. crystallisation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/48—Separation; Purification; Stabilisation; Use of additives
- C07C67/56—Separation; Purification; Stabilisation; Use of additives by solid-liquid treatment; by chemisorption
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- A—HUMAN NECESSITIES
- 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)
- A61K36/63—Oleaceae (Olive family), e.g. jasmine, lilac or ash tree
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Abstract
The invention discloses a kind of extracting method of Jasmonate with analgesic activity, which includes following operating procedure: 1) taking fresh arabian jasmine root cutting shoots, be added in the ethanol water of 0.8~2.0 times of weight and impregnate 3-24 hours, filter, take filtrate；2) filtrate is placed in and is contained in ware, being put into -10~-15 DEG C of icebox makes its icingization；3) freeze dryer is opened, after condenser temperature is down to-50 DEG C~-60 DEG C, the sample for being put into ice contains ware, and the vacuum degree for controlling freeze dryer is 160-170Pa, wait freeze dried completely；4) it takes out sample and contains ware, the film layer or cotton-shaped nitride layer for scraping upper layer are to get Jasmonate finished product.The present invention extracts Jasmonate using freezing and drying lyophilization, can prevent the oxidation deterioration of Jasmonate, and improve yield, and Jasmonate has the analgesic activity of highly significant.
Description
Technical field
The present invention relates to the extracting method of Phytochemistry composition, the extraction of specifically a kind of Jasmonate with analgesic activity
Method.
Background technique
Jasmine is root, stem, leaf, the flower of Oleaceae plants jasmine, is distributed mainly on the ground such as Guangxi, Guangdong, Yunnan, Sichuan,
Wild less, mostly family's kind is a kind of industrial crops.Make tea-drinking, referred to as jasmine tea with its flower, or mixes and stirs other tealeaves drink
With.The gained distillate after steam distillation is spent, arabian jasmine flower distillate is claimed, there is solution all aging gas in the heart, invigorating the spleen qi-regulating
The effect of.There is extensive plantation in the multiple small towns in Hengxian County, the industry to take on a certain scale, referred to as the township of jasmine.Jasmine answers
With only being spent at present with it, Jasmine section is held, all every year to promote the development of Jasmine industry.Jasmine only accounts for jasmine plant
Sub-fraction, and flower yield it is related with the old and new of plant, new strain spend it is more, old strain spend lacks.For the normal volume for keeping flower, kind
Old strain, the new strain of transplanting will be excavated every year by planting peasant household, or strike off the aerial part of old strain, and root is allowed to grow new talent, and be struck off
Rhizome usually abandon it.
Jasmine rhizome is not Chinese medicine, is also seldom seen as herbal medicine.Traditional popular prescription is all to take its fresh rhizome mill juice for oral administration,
Or fresh rhizome is smash into suede external application parched with wine, just there are analgesia, tranquilizing soporific, anesthesia and other effects.The analgesia anesthetic effect of jasmine exists
In the Chinese drug anesthesia research that eighties of last century the seventies are carried out, also without isolated this kind of monomer component.In recent years, Bu Shaoxue
Person also studies the chemical component of jasmine rhizome, but has jasmine extract to carry out treatment analgesia, town currently without discovery
The relevant report of quiet hypnosis.
The chemical property of the ingredients such as jasmine rhizome analgesia is quite active, light, air, temperature (especially heating), soda acid
Etc. its autoxidation can be promoted.Usual jasmine rhizome with solvent extraction does not go out active constituent after drying in the shade or drying, and illustrates them
It has aoxidized and has become other substances, can not do medicinal material.
Summary of the invention
It, can be with technical problem to be solved by the invention is to provide a kind of extracting method of Jasmonate with analgesic activity
Increase the type of analgesic, and waste agronomic crop can be made full use of, turns waste into wealth.
The present invention solves above-mentioned technical problem with following technical solution:
The present invention has the extracting method of the Jasmonate of analgesic activity, including following operating procedure:
1) fresh arabian jasmine root cutting shoots are taken, the ethyl alcohol that the volumetric concentration that 0.8~2.0 times of weight is added is 18-20% is water-soluble
It is impregnated 3-24 hours in liquid, filters, take filtrate；
2) filtrate is placed in and is contained in ware, being put into -10~-15 DEG C of icebox makes its icingization；
3) freeze dryer is opened, after condenser temperature is down to -50 DEG C~-60 DEG C, the sample for being put into ice contains ware,
And the vacuum degree for controlling freeze dryer is 160-170Pa, wait freeze dried completely；
4) it takes out sample and contains ware, the film layer or cotton-shaped nitride layer for scraping upper layer are to get Jasmonate finished product.
It in step 1), will be crushed after fresh arabian jasmine root cutting shoots, be then placed in immersion while progress in ethanol water
Suede is smash in stirring, then releases maceration extract, then by dregs of a decoction dislocation centrifuge, dries solution, and maceration extract and the solution thrown away are merged,
Obtain filtrate.
In step 1), the dissection, which refers to, is cut into 1-2cm.
In step 4), freeze dryer is run 48-55 hours after the sample for being put into ice contains ware, until freezing dried
Completely.
The method of the present invention can make the active constituent of jasmine extract separation under the conditions of low-temp low-pressure, and make active constituent not by
Oxidation deterioration keeps original bioactivity, and technical process is not required to thermal energy, does not pollute to environment.
The method of the present invention can increase the type of analgesic, and can make full use of waste agronomic crop, turn waste into wealth.
Specific embodiment
There is to the present invention extracting method work of the Jasmonate of analgesic activity further to retouch combined with specific embodiments below
It states；
Embodiment 1, extracting method is as follows:
1) it takes fresh arabian jasmine root cutting shoots (every segment length 1-2cm), sample weighs 400 grams, and the ethanol water that volumetric concentration is 18% is added
Solution 375ml impregnates 24 hours, is filtered using two layers of gauze, obtains filtrate；
2) filtrate is sub-packed in plastic ware, being placed in -10~-15 DEG C of icebox makes its icingization；
3) it opens freeze dryer and is put into the sample plastic ware of ice after condenser temperature is down to -55 DEG C, and control
The vacuum degree of freeze dryer is that 160Pa is freezed dried completely after operation 52 hours；
4) sample plastic ware is taken out, the film layer on upper layer is scraped, obtains Jasmonate finished product.
Jasmine cellulose content about 30% in the filtrate of step 1).Jasmonate yield is up to 0.1%.
Embodiment 2, extracting method is as follows:
1) it takes fresh arabian jasmine root cutting shoots (every segment length 1-2cm), sample weighs 500 grams, and the ethanol water that volumetric concentration is 20% is added
Solution 750ml impregnates 24 hours, is filtered using two layers of gauze, obtains filtrate 500ml；
2) filtrate is sub-packed in glass beaker, being placed in -10~-15 DEG C of icebox makes its icingization；
3) it opens freeze dryer and is put into the mother glass beaker of ice after condenser temperature is down to -50 DEG C, and control
The vacuum degree of freeze dryer processed is 165Pa, is run 48 hours, is freezed dried completely；
4) mother glass beaker is taken out, upper layer floccule is scraped, obtains Jasmonate finished product.
Jasmine cellulose content about 50% in the filtrate of step 1).Jasmonate yield is up to 0.35%.
Embodiment 3, extracting method is as follows:
1) fresh arabian jasmine root cutting shoots (every segment length 1-2cm), crushing are taken, take 1500 grams, it is 18% that volumetric concentration, which is added,
Ethanol water 2800ml impregnates, and stirs and smash suede extraction 3 hours, releasing maceration extract, in dregs of a decoction dislocation centrifuge, dries molten
Then maceration extract and the solution thrown away are merged to obtain filtrate by liquid；
2) filtrate is sub-packed in plastic ware, being placed in -10~-15 DEG C of icebox makes its icingization；
3) it opens freeze dryer and is put into the sample plastic ware of ice after condenser temperature is down to -60 DEG C, and control
The vacuum degree of freeze dryer is that 170Pa is freezed dried completely after operation 50 hours；
4) sample plastic ware is taken out, upper layer floccule is scraped, obtains Jasmonate finished product.
Jasmine cellulose content about 80% in the filtrate of step 1).Jasmonate yield is up to 1%.
It is the analgesic test carried out using the Jasmonate that the method for the present invention is extracted to animal below:
1 experimental material
1.1 animals: Kunming mouse, female, 18~22g of weight Guangxi Medical University's Experimental Animal Center provide, qualified
Card number: 2014-0002.
1.2 tested material
Jasmonate
2 experimental methods
2.1 Dichlorodiphenyl Acetates cause the influence of mouse writhing reaction
40 mouse are taken, male and female dual-purpose is randomly divided into 4 groups, i.e. Normal group, positive controls (aspirin 0.2g/
Kg), high low dosage administration group, every group of 10 mouse.The 30min after secondary administration, is tested, and every group of mouse is injected intraperitoneally
0.6% acetic acid 0.2mL records the writhing incubation period (i.e. from injection acetic acid to the time of writhing) of each group mouse and in 15min
The number of interior writhing, if non-writhing in 15min, incubation period is recorded by 15min.Inhibiting rate=(physiological saline group writhing mean-
Administration group writhing mean)/physiological saline group writhing mean × 100%.
2.2 statistical methods: SPSS16.0 software carries out statistical procedures to data.Testing result is with mean ± standard
Difference It indicates, multiple sample averages compare using one-way analysis of variance, are that difference is anticipated with statistics with P < 0.05
Justice.
3 results
3.1 Dichlorodiphenyl Acetates cause the influence of mouse writhing reaction
Compared with Normal group, the high low dose group of Jasmonate has significant difference (P < 0.01).The result shows that jasmine
Jasmine element can inhibit acetic acid induced mice writhing response, has apparent analgesic activity, is shown in Table 1.
1 Jasmonate Dichlorodiphenyl Acetate of table causes the influence of mouse writhing reaction
Compared with Normal group: * P < 0.05, * * P < 0.01
4 conclusions
The Jasmonate of two groups of dosage can significantly inhibit acetic acid induced mice writhing response, have apparent analgesic activity.
Claims (4)
1. the extracting method of the Jasmonate with analgesic activity, which is characterized in that including following operating procedure:
1) fresh arabian jasmine root cutting shoots are taken, are soaked in the ethanol water that the volumetric concentration that 0.8~2.0 times of weight is added is 18-20%
Bubble 3-48 hours, filtering, takes filtrate；
2) clear solution is placed in and is contained in ware, being put into -10~-15 DEG C of icebox makes its icingization；
3) freeze dryer is opened, after condenser temperature is down to -50 DEG C~-60 DEG C, the sample for being put into ice contains ware, and controls
The vacuum degree of freeze dryer processed is 160-170Pa, wait freeze dried completely；
4) it takes out sample and contains ware, the film layer or cotton-shaped nitride layer for scraping upper layer are to get Jasmonate finished product.
2. the extracting method of the Jasmonate with analgesic activity according to claim 1, which is characterized in that, will in step 1)
It is crushed after fresh arabian jasmine root cutting shoots, is then placed in be stirred while immersion in ethanol water and smashes suede, then release dipping
Liquid, then by dregs of a decoction dislocation centrifuge, solution is dried, maceration extract and the solution thrown away are merged, filtrate is obtained.
3. the extracting method of the Jasmonate with analgesic activity according to claim 2, which is characterized in that in step 1), institute
It states dissection and refers to and be cut into 1-2cm.
4. the extracting method of the Jasmonate with analgesic activity according to claim 1, which is characterized in that in step 3), ice
Freeze drier to run 48-55 hours after the sample for being put into ice contains ware, until freezing dried completely.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1524872A (en) * | 2003-02-25 | 2004-09-01 | 敏 洪 | Active ingredient of jasmine root, extracting method and uses thereof |
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- 2016-09-29 CN CN201610869546.XA patent/CN106632517B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1524872A (en) * | 2003-02-25 | 2004-09-01 | 敏 洪 | Active ingredient of jasmine root, extracting method and uses thereof |
Non-Patent Citations (2)
| Title |
|---|
| 茉莉根醇浸膏镇痛作用的实验研究;毛磊等;《中华中医药学刊》;20140331;第32卷(第3期);641-644 |
| 茉莉花根对小鼠的镇痛和镇静作用;宁天等;《中药药理与临床》;20141231;第30卷(第2期);99-101 |
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