CN109731132A - The liquid bandage of alleviation arthralgia containing Ginger P.E - Google Patents
The liquid bandage of alleviation arthralgia containing Ginger P.E Download PDFInfo
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Abstract
The liquid bandage for the alleviation arthralgia containing Ginger P.E that the invention discloses a kind of, the raw material including following parts by weight: 2 parts of Ginger P.E, 1 part of Chinese medical extract, 1 part of peach oil extract, 2 parts of elm bark extract, 10 parts of chitosan, 30 parts of cellulose acetate, 5 parts of polyvinylpyrrolidone and mass fraction are 100 parts of ethanol solution of 95%;Wherein, ethanol solution adjusts pH to 8~9 using the borate buffer solution that pH is 9.5.The liquid bandage of alleviation arthralgia of the present invention containing Ginger P.E not only has the function of that arthralgia is effectively relieved, but also can be in skin surface quick film-forming.
Description
Technical field
The present invention relates to the preparation fields of Ginger P.E.It is more particularly related to which a kind of contain Ginger P.E
Alleviation arthralgia liquid bandage.
Background technique
Arthralgia is a kind of systemic autoimmune disease characterized by arthritis, be seriously threaten health it is chronic
One of disease is mainly characterized by chronic, symmetry, progressive and invasion, and specific cash is pass caused by arthrosynovitis
Save swelling deformation and osteoclasia or even disability.
Currently, being mostly Chinese medicine ointment or patch for arthritic treatment, Chinese medicine ointment is applied to site of disease and is not only easy to
It being wiped free of, influences the function and effect of ointment, and be easy to keep clothes dirty, patch sticks the cutaneous gas permeability in position, and
And it coheres place and is easy to appear the symptoms such as skin allergy.
Summary of the invention
It is an object of the invention to solve at least the above problems, and provide the advantages of at least will be described later.
The liquid bandage for the alleviation arthralgia containing Ginger P.E that it is a still further object of the present invention to provide a kind of, no
Only have the function of that arthralgia is effectively relieved, and can quickly form film in skin surface.
In order to realize these purposes and other advantages according to the present invention, a kind of alleviation pass containing Ginger P.E is provided
Save the liquid bandage of pain, which is characterized in that the raw material including following parts by weight: 2 parts of Ginger P.E, Chinese medical extract 1
Part, 1 part of peach oil extract, 2 parts of elm bark extract, 10 parts of chitosan, 30 parts of cellulose acetate, polyvinylpyrrolidone 5
Part and mass fraction are 100 parts of ethanol solution of 95%;
Wherein, ethanol solution adjusts pH to 8~9 using the borate buffer solution that pH is 9.5;
Chinese medical extract the preparation method comprises the following steps: A1, mass ratio is taken to be the Dysosma versipellis, white of 1:1:1.3:1.8:2:2:2.5:3
The root of Dahurian angelica, bear gall, the root of Chinese clematis, monkshood, rhizoma arisaematis, sea otter and cape jasmine mix and crush, and sieving obtains crushed material;A2, crushing is taken
Material 10 times of gross mass amount mass fractions be 95% methanol solution, 5 times amount acetone, 1 times amount N,N-dimethylformamide,
0.01 times amount dimethyl sulfoxide mixing, and be added 0.1 times of crushed material gross mass amount mass fraction be 10% citric acid, 0.01
The acetic anhydride of amount again stirs 20min, obtains reserve liquid;A3, crushed material is added in reserve liquid, is placed under conditions of 50 DEG C
10h is heated, filters and is concentrated, obtain concentrate, concentrate is subjected to column chromatography, eluent system is acetate-methanol system,
It collects acetate-methanol volume ratio and is the eluent of 6~4:1, and be concentrated, obtain Chinese medical extract.
Preferably, the preparation method of Ginger P.E:
S1, it dries, and crushes under the conditions of ginger is placed in 60 DEG C, obtain ginger powder;
Then 5 times of ginger powder gross mass amounts are added in S2, the tetrahydrofuran for taking 10 times of ginger powder gross mass amounts into tetrahydrofuran
Gas-phase silica is placed in 50 DEG C, stirs 10min under conditions of 400r/min, then under conditions of 60 DEG C, 400r/min dropwise
The sulfuric acid solution of the 4M of 1 times of ginger powder gross mass amount is added, is added dropwise to sulfuric acid solution, continues to stir 20min, then in seven times etc.
The silane coupling agents of 6 times of ginger powder gross mass amounts are added in amount, are placed in 70 DEG C, stir 1h under conditions of 400r/min, filter, obtain
Solid finally rinses solid with the ethanol solution that mass fraction is 95%, and dries 6h under the conditions of solid is placed in 60 DEG C, obtains
Modified gas-phase silica, wherein silane coupling agent is (HO)3Si(CH2)3N(CH2PO3H2)2;
S3, the solvent for taking 20 times of ginger powder gross mass amounts, and acetic acid is added into solvent, the pH for adjusting solvent is 5~6, so
Modified gas-phase silica is added afterwards, is placed in 50 DEG C, stirs 20min under conditions of 400r/min, add ginger powder and flow back
It extracts, filtering obtains the first filtrate and filter residue, and the methanol that 4 times of filter residue gross mass amounts are added into filter residue impregnates 15h, filters
To the second filtrate, the first filtrate, the second filtrate are merged and is concentrated, medicinal extract is obtained, medicinal extract is separated using column chromatography, is washed
Lift-off system is petroleum ether-ethyl acetate system, petroleum ether-dichloromethane system, petroleum ether-methanol system, petroleum ether-acetone body
System, wherein collect the eluent that petroleum ether-ethyl acetate volume ratio is 6:1, petroleum ether-methylene chloride volume than washing for 8:1
The eluent that liquid, the eluent that petroleum ether-methanol volume ratio is 7:1, petroleum ether-acetone volume ratio are 2:1 is taken off, eluent is merged
And be concentrated, obtain Ginger P.E.
Preferably, peach oil extract the preparation method comprises the following steps: to peach oil in be added 10 times of its gross mass amount water, 5
The methanol of amount again, is placed in 60 DEG C of condition heating 5h, and filtering obtains third filtrate;Its gross mass is added into third filtrate
The active carbon of 0.5 times of amount carries out decolorization, and filtering obtains the 4th filtrate;0.08 times of its gross mass is added into the 4th filtrate
The white sugar of amount heats 1h under conditions of being placed in 80 DEG C, concentration, as peach oil extract.
Preferably, the preparation method of elm bark extract: shining dry doubling for elm bark and crush, and sieving obtains elm bark
Powder;The methanol of water, 10 times of amounts that 20 times of its gross mass amounts are added into elm bark powder mixes, and is added under the conditions of being placed in 70 DEG C
Hot 5h, filtering, obtains the 5th filtrate;The active carbon that 0.5 times of its gross mass amount is added into the 5th filtrate carries out decolorization, mistake
It filters and is concentrated, obtain elm bark extract.
Preferably, solvent is ethyl acetate.
Preferably, in S1, ginger is placed under the conditions of 60 DEG C and is dried, and also carry out sieving processing after crushing, obtain 200
Purpose ginger powder.
The present invention is include at least the following beneficial effects:
The first, the present invention not only has the function of that arthralgia is effectively relieved, but also can quickly be formed in skin surface
Film extends action time.
The second, Chinese medical extract, Dysosma versipellis, the root of Dahurain angelica, bear gall, the root of Chinese clematis, monkshood, rhizoma arisaematis, sea otter and cape jasmine are added
Help to alleviate arthralgia;In the preparation method of Chinese medical extract, by the way that methanol solution, acetone, N, N- dimethyl methyl is added
Amide mixed solvent, which extracts, can extract a greater variety of active ingredients, and enhancing liquid bandage alleviates the effect of arthralgia
Fruit;Addition dimethyl sulfoxide, sodium citrate, acetic anhydride can be improved the permeability of cell wall, make intracellular more kinds of effective ingredients
It releases, is extracted compared to technology using water, more kinds of effective ingredients are contained in preparation method of the invention, to alleviation
The effect of arthralgia is more preferable.
Third, addition Ginger P.E, Ginger P.E are used in combination with Chinese medical extract, and arthritis can be effectively relieved
Bitterly;Modified gas-phase silica is added into solvent, makes ginger powder ginger powder and gas-phase silica in cold soaking extraction or refluxing extraction
It rubs, improves cell-wall breaking ratio, promote the extraction of effective ingredient;Sulfuric acid is added and forms silicon hydroxyl convenient for gas-phase silica surface
Base promotes to form stable silicon oxygen silicon key between gas-phase silica and silane coupling agent, and silane coupling agent is added in equivalent several times
The probability that silane coupling agent itself is condensed can be reduced, the utilization rate of silane coupling agent is improved;It uses (HO)3Si(CH2)3N
(CH2PO3H2)2Gas-phase silica is modified, dispersibility of the gas-phase silica in solvent on the one hand can be improved, is increased
Contact of the ginger powder with gas-phase silica improves cell-wall breaking ratio, is on the other hand carried out using silane coupling agent to gas-phase silica
It is modified, absorption of the gas-phase silica to effective ingredient can be reduced, convenient for the separation of effective ingredient and gas-phase silica, improves and extracts
Rate;The silane coupling agent and gas for being convenient for the silane coupling agent, self-condensation that will not react are rinsed using ethanol solution
The separation of phase white carbon black avoids introducing new impurity in effective ingredient;It is eluted, can effectively be mentioned using a variety of eluent systems
Effective ingredient in high Ginger P.E.
4th, addition peach oil, can reduce the surface tension of liquid bandage, reduce liquid and flow on the skin, improve liquid
The bonding force of body bandage, and then effectively improve the effect for alleviating arthralgia;It is mixed using the methanol of 10 times of water measured, 5 times of amounts
Solvent extracts, convenient for extracting the effective ingredient in peach oil;White sugar and peach oil act on, and can be improved liquid bandage and skin
The sticking nature of skin.
5th, elm bark extract is added, elm bark extract is used in combination with Chinese medical extract, and pass can be effectively relieved
Save pain;Using 20 times of water measured, 10 times of methanol mixed solvents measured, convenient for the release of elm bark effective ingredient.
Further advantage, target and feature of the invention will be partially reflected by the following instructions, and part will also be by this
The research and practice of invention and be understood by the person skilled in the art.
Specific embodiment
The present invention will be further described in detail below with reference to the embodiments, to enable those skilled in the art referring to specification
Text can be implemented accordingly.
<embodiment 1>
The liquid bandage of alleviation arthralgia containing Ginger P.E, the raw material including following parts by weight: ginger extracts
2 parts of object, 1 part of Chinese medical extract, 1 part of peach oil extract, 2 parts of elm bark extract, 10 parts of chitosan, cellulose acetate 30
Part, 5 parts of polyvinylpyrrolidone and mass fraction are 100 parts of ethanol solution of 95%;
Wherein, ethanol solution adjusts pH to 8~9 using the borate buffer solution that pH is 9.5;
Chinese medical extract the preparation method comprises the following steps: A1, mass ratio is taken to be the Dysosma versipellis, white of 1:1:1.3:1.8:2:2:2.5:3
The root of Dahurian angelica, bear gall, the root of Chinese clematis, monkshood, rhizoma arisaematis, sea otter and cape jasmine mix and crush, and sieving obtains crushed material;A2, crushing is taken
Material 10 times of gross mass amount mass fractions be 95% methanol solution, 5 times amount acetone, 1 times amount N,N-dimethylformamide,
0.01 times amount dimethyl sulfoxide mixing, and be added 0.1 times of crushed material gross mass amount mass fraction be 10% citric acid, 0.01
The acetic anhydride of amount again stirs 20min, obtains reserve liquid;A3, crushed material is added in reserve liquid, is placed under conditions of 50 DEG C
10h is heated, filters and is concentrated, obtain concentrate, concentrate is subjected to column chromatography, eluent system is acetate-methanol system,
It collects acetate-methanol volume ratio and is the eluent of 6~4:1, and be concentrated, obtain Chinese medical extract.
The preparation method of Ginger P.E:
S1, it dries, and crushes under the conditions of ginger is placed in 60 DEG C, obtain ginger powder;
Then 5 times of ginger powder gross mass amounts are added in S2, the tetrahydrofuran for taking 10 times of ginger powder gross mass amounts into tetrahydrofuran
Gas-phase silica is placed in 50 DEG C, stirs 10min under conditions of 400r/min, then under conditions of 60 DEG C, 400r/min dropwise
The sulfuric acid solution of the 4M of 1 times of ginger powder gross mass amount is added, is added dropwise to sulfuric acid solution, continues to stir 20min, then in seven times etc.
The silane coupling agents of 6 times of ginger powder gross mass amounts are added in amount, are placed in 70 DEG C, stir 1h under conditions of 400r/min, filter, obtain
Solid finally rinses solid with the ethanol solution that mass fraction is 95%, and dries 6h under the conditions of solid is placed in 60 DEG C, obtains
Modified gas-phase silica, wherein silane coupling agent is (HO)3Si(CH2)3N(CH2PO3H2)2;
S3, the solvent for taking 20 times of ginger powder gross mass amounts, and acetic acid is added into solvent, the pH for adjusting solvent is 5~6, so
Modified gas-phase silica is added afterwards, is placed in 50 DEG C, stirs 20min under conditions of 400r/min, add ginger powder and flow back
It extracts, filtering obtains the first filtrate and filter residue, and the methanol that 4 times of filter residue gross mass amounts are added into filter residue impregnates 15h, filters
To the second filtrate, the first filtrate, the second filtrate are merged and is concentrated, medicinal extract is obtained, medicinal extract is separated using column chromatography, is washed
Lift-off system is petroleum ether-ethyl acetate system, petroleum ether-dichloromethane system, petroleum ether-methanol system, petroleum ether-acetone body
System, wherein collect the eluent that petroleum ether-ethyl acetate volume ratio is 6:1, petroleum ether-methylene chloride volume than washing for 8:1
The eluent that liquid, the eluent that petroleum ether-methanol volume ratio is 7:1, petroleum ether-acetone volume ratio are 2:1 is taken off, eluent is merged
And be concentrated, obtain Ginger P.E.
Peach oil extract the preparation method comprises the following steps: to peach oil in be added 10 times of its gross mass amount water, 5 times amount first
Alcohol, is placed in 60 DEG C of condition heating 5h, and filtering obtains third filtrate;0.5 times of its gross mass amount is added into third filtrate
Active carbon carries out decolorization, and filtering obtains the 4th filtrate;The white sugar of 0.08 times of its gross mass amount is added into the 4th filtrate,
1h is heated under conditions of being placed in 80 DEG C, is concentrated, as peach oil extract.
The preparation method of elm bark extract: shining dry doubling for elm bark and crush, and sieving obtains elm bark powder;To elm
The water of 20 times of its gross mass amounts is added in Pi Fenzhong, the methanol of 10 times of amounts mixes, and carries out heating 5h, mistake under the conditions of being placed in 70 DEG C
Filter, obtains the 5th filtrate;The active carbon that 0.5 times of its gross mass amount is added into the 5th filtrate carries out decolorization, filters and dense
Contracting, obtains elm bark extract.
Solvent is ethyl acetate.
In S1, ginger is placed under the conditions of 60 DEG C and is dried, and also carry out sieving processing after crushing, obtains the ginger powder of 200 mesh.
<comparative example 1>
Using the spray for being currently used for treatment of arthritis.
<comparative example 2>
The liquid bandage of the alleviation arthralgia containing Ginger P.E is prepared according to the method for embodiment 1, wherein different
It is the preparation method of Chinese medical extract, specifically: Dysosma versipellis, the root of Dahurain angelica, the bear for being 1:1:1.3:1.8:2:2:2.5:3 by mass ratio
Gallbladder, the root of Chinese clematis, monkshood, rhizoma arisaematis, sea otter and cape jasmine mix and crush, and sieving obtains crushed material, is added into crushed material
Its total mass ratio is the water of 20 times of amounts, heats 10h under conditions of being placed in 100 DEG C, filters and be concentrated, obtain concentrate, will be concentrated
Object carries out column chromatography, and eluent system is acetate-methanol system, and collecting acetate-methanol volume ratio is washing for 6~4:1
De- liquid, and be concentrated, obtain Chinese medical extract.
<comparative example 3>
The liquid bandage of the alleviation arthralgia containing Ginger P.E is prepared according to the method for embodiment 1, wherein different
It is the preparation method difference of Ginger P.E, specifically: ginger is placed under the conditions of 60 DEG C and is dried, and is crushed, ginger powder is obtained, to
The ethyl acetate that 20 times of ginger powder gross mass amounts are added in ginger powder carries out refluxing extraction, filters and is concentrated to get medicinal extract, medicinal extract is adopted
It is separated with column chromatography, eluent system is system, petroleum ether-dichloromethane system, petroleum ether-methanol system, petroleum ether-the third
Ketoboidies system, wherein collect the eluent that petroleum ether-ethyl acetate volume ratio is 6:1, petroleum ether-methylene chloride volume ratio is 8:1
Eluent, petroleum ether-methanol volume ratio be 7:1 eluent, petroleum ether-acetone volume ratio be 2:1 eluent, merging washes
De- liquid is simultaneously concentrated, and obtains Ginger P.E.
<comparative example 4>
The liquid bandage of the alleviation arthralgia containing Ginger P.E is prepared according to the method for embodiment 1, wherein different
It is that peach oil extract is not added.
<comparative example 5>
The liquid bandage of the alleviation arthralgia containing Ginger P.E is prepared according to the method for embodiment 1, wherein different
It is that elm bark extract is not added.
<comparative example 6>
The liquid bandage of the alleviation arthralgia containing Ginger P.E is prepared according to the method for embodiment 1, wherein different
It is gas-phase silica without using (HO)3Si(CH2)3N(CH2PO3H2)2It is modified.
<Experimental Characterization>prepares 7 groups of alleviation arthralgias containing Ginger P.E according to the method for implementing 1, comparative example 1~6
Liquid bandage, be respectively used to following research.
1, mouse experiment
The preparation of 1.1 arthritis mouse models
Taking 70 weight is the male mice of 80~100g, and is randomly divided into 7 groups, and every group has 10 mouse.Mouse is used
After 10% chloraldurate (0.3mL/100g) abdominal cavity holonarcosis (it is painless to pinch foot for no eye blink response), toes are used behind the right side
75% alcohol disinfecting, and inject carrageenan 0.2mL.
The assessment of 1.2 swellings
Using mouse toes volume measuring instrument measure every mouse it is right after foot swelling volume (by mL), after being accurate to decimal point
Two.It is measured behind 2,4,6,24,48 hours after carrageenin injection, foot swelling rate is sufficient percent by volume difference
And calculated by following formula: swelling rate (%)=(A-B)/B × 100, A indicates the sufficient volume of different time points after injection, B here
Indicating the sufficient volume before injection, the results are shown in Table 1, wherein in 7 groups of mouse, one group is model group (not using drug),
Remaining 6 groups of liquid bandages (even if with drug after injection carrageenan) for corresponding sprinkling embodiment 1, comparative example 1~5 respectively.
As a result it is expressed as average value, through statistical analysis p < 0.05, there is statistical significance.
Table 1, injection carrageenan after swelling and treatment after percentage variation
Group | 2h | 4h | 6h | 24h | 48h |
Model group | 17.20 | 54.1627 | 85.4531 | 73.656 | 62.775 |
Embodiment 1 | 7.71 | 19.2612 | 38.2319 | 23.3515 | 10.0113 |
Comparative example 1 | 9.29 | 28.4819 | 54.16226 | 46.248 | 39.797 |
Comparative example 2 | 14.39 | 30.6216 | 53.52323 | 39.8514 | 28.7311 |
Comparative example 3 | 13.68 | 22.4415 | 43.0921 | 32.6211 | 23.929 |
Comparative example 4 | 8.75 | 21.6814 | 43.0522 | 31.7712 | 19.4512 |
Comparative example 5 | 16.45 | 36.4918 | 60.7124 | 50.3510 | 42.568 |
Arthralgia can be effectively relieved in the present invention known to comparative analysis embodiment 1, comparative example 1;
Ginger P.E is added known to comparative analysis embodiment 1, comparative example 2, Ginger P.E is combined with Chinese medical extract
It uses, arthralgia can be effectively relieved, meanwhile, there are many preparation method that ginger of the present invention extracts can make to contain in Ginger P.E
Effective ingredient;
Comparative analysis embodiment 1, comparative example 3, comparative example 4 know that addition peach oil extract, elm extract can be into one
Step improves the effect for slowing down arthralgia.
2, film-formation result
Pig ear is taken, cold water is rinsed well, and rejects unhairing, and dermatotome takes the pig ear of about 600 μ m-thicks, is placed in -20 DEG C
Under the conditions of save backup;Example 1, comparative example 3 liquid bandage be sprayed on pig ear, observe liquid bandage in pig ear
On film formation time and liquid bandage surface tension, the results are shown in Table 2;
Table 2, film formation time and surface tension
Group | Film formation time | Surface tension (mN/m) |
Embodiment 1 | 8s | 20.619±0.027 |
Comparative example 4 | 13s | 26.785±0.018 |
The result shows that addition peach oil extract can reduce the surface tension of liquid bandage, reduces liquid and flow on the skin
It is dynamic, the bonding force of liquid bandage is improved, and then effectively improve the effect for alleviating arthralgia.
3, cell-wall breaking ratio
The breaking-wall cell situation of 200 mesh ginger powders is observed under the microscope, meanwhile, corresponding to observation embodiment 1, comparative example 3
The broken wall situation of medicinal extract, the results are shown in Table 3;
Table 3, cell-wall breaking ratio
Group | Cell-wall breaking ratio |
Embodiment 1 | 88% |
Ginger powder | 79% |
Comparative example 3 | 84% |
Comparative example 6 | 81% |
The result shows that modified gas-phase silica is added, to pass through gas-phase silica during the extraction process advantageous to the friction of ginger powder
In promotion breaking-wall cell.
4, gas-phase silica settles situation
Gas-phase silica is in the dispersion of ethyl acetate in observation extraction process, and the results are shown in Table 4;
Table 4, delamination
Group | Delamination |
Embodiment 1 | Gas-phase silica is evenly dispersed |
Comparative example 6 | Gas-phase silica sinks |
The result shows that using (HO)3Si(CH2)3N(CH2PO3H2)2Gas-phase silica is modified, gas phase can be improved
Dispersibility of the white carbon black in solvent increases contact of the ginger powder with gas-phase silica, improves sporoderm-broken rate.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited
In specific details and embodiment shown and described herein.
Claims (6)
1. the liquid bandage of the alleviation arthralgia containing Ginger P.E, which is characterized in that the raw material including following parts by weight:
2 parts of Ginger P.E, 1 part of Chinese medical extract, 1 part of peach oil extract, 2 parts of elm bark extract, 10 parts of chitosan, acetic acid are fine
30 parts of dimension element, 5 parts of polyvinylpyrrolidone and mass fraction are 100 parts of ethanol solution of 95%;
Wherein, ethanol solution adjusts pH to 8~9 using the borate buffer solution that pH is 9.5;
Chinese medical extract the preparation method comprises the following steps: A1, take mass ratio be 1:1:1.3:1.8:2:2:2.5:3 Dysosma versipellis, the root of Dahurain angelica, bear
Gallbladder, the root of Chinese clematis, monkshood, rhizoma arisaematis, sea otter and cape jasmine mix and crush, and sieving obtains crushed material;A2, the total matter of crushed material is taken
Measure the methanol solution, 5 times of acetone measured, 1 times of N,N-dimethylformamide measured, 0.01 times that the mass fraction of 10 times of amounts is 95%
The dimethyl sulfoxide of amount mixes, and the mass fraction that 0.1 times of crushed material gross mass amount is added be 10% citric acid, 0.01 times of amount
Acetic anhydride stirs 20min, obtains reserve liquid;A3, crushed material is added in reserve liquid, is heated under conditions of being placed in 50 DEG C
10h filters and is concentrated, obtains concentrate, and concentrate is carried out column chromatography, and eluent system is acetate-methanol system, is collected
Acetate-methanol volume ratio is the eluent of 6~4:1, and is concentrated, and obtains Chinese medical extract.
2. the liquid bandage of the alleviation arthralgia containing Ginger P.E as described in claim 1, which is characterized in that ginger mentions
Take the preparation method of object:
S1, it dries, and crushes under the conditions of ginger is placed in 60 DEG C, obtain ginger powder;
S2, the tetrahydrofuran for taking 10 times of ginger powder gross mass amounts, are then added the gas phase of 5 times of ginger powder gross mass amounts into tetrahydrofuran
White carbon black is placed in 50 DEG C, stirs 10min under conditions of 400r/min, is then added dropwise under conditions of 60 DEG C, 400r/min
The sulfuric acid solution of the 4M of 1 times of ginger powder gross mass amount, is added dropwise to sulfuric acid solution, continues to stir 20min, then equivalent adds in seven times
The silane coupling agents for entering 6 times of ginger powder gross mass amounts are placed in 70 DEG C, stir 1h under conditions of 400r/min, filter, consolidate
Body finally rinses solid with the ethanol solution that mass fraction is 95%, and dries 6h under the conditions of solid is placed in 60 DEG C, is changed
Property gas-phase silica, wherein silane coupling agent be (HO)3Si(CH2)3N(CH2PO3H2)2;
S3, the solvents for taking 20 times of ginger powder gross mass amounts, and acetic acid are added into solvent, and the pH for adjusting solvent is 5~6, then plus
Enter modified gas-phase silica, be placed in 50 DEG C, stir 20min under conditions of 400r/min, adds ginger powder and carry out refluxing extraction,
Filtering, obtains the first filtrate and filter residue, and the methanol that 4 times of filter residue gross mass amounts are added into filter residue impregnates 15h, is obtained by filtration second
First filtrate, the second filtrate are merged and are concentrated, obtains medicinal extract by filtrate, medicinal extract are separated using column chromatography, eluent system
For petroleum ether-ethyl acetate system, petroleum ether-dichloromethane system, petroleum ether-methanol system, petroleum ether-acetone system,
In, collect petroleum ether-ethyl acetate volume ratio be 6:1 eluent, petroleum ether-methylene chloride volume than for 8:1 eluent,
It is simultaneously dense to merge eluent for the eluent that eluent that petroleum ether-methanol volume ratio is 7:1, petroleum ether-acetone volume ratio are 2:1
Contracting, obtains Ginger P.E.
3. the liquid bandage of the alleviation arthralgia containing Ginger P.E as described in claim 1, which is characterized in that peach oil
Extract the preparation method comprises the following steps: to peach oil in be added 10 times of its gross mass amount water, 5 times amount methanol, be placed in 60 DEG C
Condition heats 5h, and filtering obtains third filtrate;The active carbon that 0.5 times of its gross mass amount is added into third filtrate decolourizes
Processing, filtering, obtains the 4th filtrate;The white sugar of 0.08 times of its gross mass amount is added into the 4th filtrate, is placed in 80 DEG C of item
1h is heated under part, is concentrated, as peach oil extract.
4. the liquid bandage of the alleviation arthralgia containing Ginger P.E as described in claim 1, which is characterized in that elm bark
The preparation method of extract: shining dry doubling for elm bark and crush, and sieving obtains elm bark powder;It is total that it is added into elm bark powder
The water of 20 times of quality amounts, 10 times of methanol mixing measured, carry out heating 5h, filter, obtain the 5th filtrate under the conditions of being placed in 70 DEG C;
The active carbon that 0.5 times of its gross mass amount is added into the 5th filtrate carries out decolorization, filters and is concentrated, and obtains elm bark extraction
Object.
5. the liquid bandage of the alleviation arthralgia containing Ginger P.E as described in claim 1, which is characterized in that solvent is
Ethyl acetate.
6. the liquid bandage of the alleviation arthralgia containing Ginger P.E as described in claim 1, which is characterized in that in S1,
Ginger is placed under the conditions of 60 DEG C and is dried, and also carries out sieving processing after crushing, obtains the ginger powder of 200 mesh.
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Citations (10)
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