CN105796892A - Traditional Chinese medicine extractive composition and preparation method thereof - Google Patents
Traditional Chinese medicine extractive composition and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a traditional Chinese medicine extractive composition and a preparation method thereof, wherein the extractive composition is prepared from the following components: by weight, 42-62 parts of hedera helix extractive, 5-10 parts of Marian thistle extractive, 3-5 parts of olive leaf extractive, 6-12 parts of fennel extractive, 10-15 parts of liquorice extractive, 10-15 parts of radix ophiopogonis extractive, 10-15 parts of dried tangerine peel extractive, and 8-10 parts of radix polygonati officinalis. By a special technology, the hedera helix extractive, Marian thistle extractive, olive leaf extractive, fennel extractive, liquorice extractive, radix ophiopogonis extractive, dried tangerine peel extractive and radix polygonati officinalis of higher purities are obtained and combined by an optimal proportion. The composition has a good curative effect on cough; it is safe and nontoxic with remarkable curative effect, and without generating resistance to drugs; it clinical effective rate is up to 97%, and its cure rate is up to 92%.
Description
Technical field
The present invention relates to a kind of Chinese medicine extraction mixture, be specifically related to a kind of traditional Chinese medicine extract composition and system thereof
Preparation Method.
Background technology
Cough is a kind of protectiveness respiratory reflex action of human body, can effectively remove respiratory tract by coughre flex
Interior secretions or the foreign body of entrance air flue.But it is under pathological state, as serious in cough long-term, frequent, violent
Affect the daily life of patient.
Under pathological state, cough may result in respiratory tract hemorrhage and even causes the symptoms such as laryngalgia, hoarseness and breathing myalgia.
In the traditional Chinese medical science, cough refers to because the factor such as diseases caused by exogenous pathogenic factor or internal injury, causes impaired depurative descending of lung QI, abnormal rising of lung-QI impact gas
A kind of disease into Clinical symptoms that sound is coughed in road and sending or companion coughs up phlegm.Ancient Chinese medicine doctor is referred to as coughing without expectorant by sound,
There is expectorant noiseless being referred to as to cough, have the cough of the sound meaning of expectorant.It mostly is expectorant sound clinically and sees, being difficult to well-separated,
Therefore to cough and to claim.Along with unsound lifes such as air pollution in recent years are day by day serious and people smoke, stay up late
The mode of living prevailing, cough sickness rate in crowd is more and more higher, causes people's physical and mental health greatly
Threat.
Cough medicine a multitude of names in the market, but mainly two big classes, one is cough medicine, and two is to eliminate the phlegm
Medicine.
Antitussive aspect includes central antitussive, such as dromethan, codeine, morphine, is mainly used in reflecting class
Dry cough.This kind of medicine cough-relieving dynamics is strong, but has the most additive.Next to that peripheral cough medicine, conventional has
Two big classes: one is demulcen, and conventional has syrup, Mel and loquat leaf extract etc.；Two is humidifying and steam suction,
Will sodium chloride, wade's balsam, eucalyptole etc. suck as a vapor.These medicines do not solve disease
, after drug withdrawal, easily there is the state of an illness repeatedly in the cause of disease of people's cough.
Eliminating the phlegm is most important one of the measure of suiting the medicine to the illness for the treatment of cough.Expectorant has two kinds: one to be nauseous eliminating the phlegm
Medicine, conventional has ammonium chloride, Radix Platycodonis, Radix Polygalae, guaifenesin.This kind of medicine can cause Nausea and vomiting
Deng the symptom that Severe gastrointestinal is uncomfortable.Two is mucolytic, and the sputum of stiff can be made to dissolve, after viscosity reduces
It is easy to bring up.Conventional medicine has bromhexine hydrochloride, Carbocysteine sheet, mucosolvan.This kind of medicine can only be alleviated for the moment
Symptom, without the therapeutical effect of essence.
As can be seen here, though the cough suppressing medicine of commercial type is many, but have that side effect is big, poor effect and stopping
The medicine state of an illness easily shortcoming such as the most repeatedly.These cough suppressing medicines can only play the effect alleviating the state of an illness for the moment, the trueest
It is right against the cause of disease to treat, therefore curative effect is not good enough.
Summary of the invention
For solving the problems referred to above, the invention provides a kind of traditional Chinese medicine extract composition and preparation method thereof, institute
Extract has a preferable therapeutical effect to cough, safety non-toxic, evident in efficacy, do not develop immunity to drugs,
Clinical effective rate is up to 97%, and cure rate reaches 92%.
For achieving the above object, the technical scheme that the present invention takes is:
A kind of traditional Chinese medicine extract composition, described extract is prepared from by the component of following weight portion:
Caulis Hederae Sinensis extract 42-62 part, Milk Thistle extract 5-10 part, Olive leaf P.E 3-5 part,
Fructus Foeniculi extract 6-12 part, Radix Glycyrrhizae extract 10-15 part, Radix Ophiopogonis extract 10-15 part, Exocarpium Citri Rubrum are extracted
Thing 10-15 part, Rhizoma Polygonati Odorati extract 8-10 part.
The preparation method of above-mentioned a kind of traditional Chinese medicine extract composition, comprises the steps:
S1, the preparation of Caulis Hederae Sinensis extract:
S11, dry Rhizoma Calystegiae Hederaceae is pulverized after aqueous solution carry out membrance separation by ultrafilter membrane after, collection
Permeate, is concentrated into the 10% of original volume, obtains concentrated solution；
S12, by the concentrated solution of gained with the flow velocity of 3-7BV/h by macroporous resin column, dynamic adsorption is saturated
After, colourless to effluent with the above-mentioned macroporous resin column of flow velocity drip washing of 5-8BV/h with deionized water, then use body
Fraction is that the organic solvent of 50%-70% carries out eluting with the flow velocity of 8-12BV/h, collects eluent, subtracts
Pressure concentrates, and obtains extractum；
S13, by after extractum water dissolution with the flow velocity of 3-5BV/h by polyamide column, dynamic adsorption is saturated
After, with 3-7BV deionized water with the above-mentioned polyamide column of flow velocity drip washing of 2-10BV/h, then use volume fraction
Aqueous solutions of organic solvent for 30%-50% carries out eluting with the flow velocity of 5-10BV/h, collects and has eluent,
It is spray-dried, obtains Caulis Hederae Sinensis extract；
S2, the preparation of Milk Thistle extract:
Being processed by dry Milk Thistle flash extracter, gained extracting solution first heats with high heat, uses after boiling
Slow fire heating 1-1.5h, hollow fiber ultrafiltration membrane filters；Medicinal residues add 15-25 times of soak by water twice, and hollow is fine
Dimension ultrafiltration membrance filter, merges three filtrates, is concentrated into 1.5g/ml；It is slowly added to 90-100% organic solvent,
Until organic solvent concentration is 55-65%, cold preservation 8-9 hour, after 2000-4000r/min is centrifuged 15-25min
Supernatant, precipitation is gone to dry, obtain Milk Thistle extract；
S3, the preparation of Olive leaf P.E:
S31, by after Folium olive saline soak 1-2 hour, dry and be placed in steam-explosion jar, be first passed through nitrogen
It is 0.7-1.3MPa to steam explosion pressure inside the tank, explosion treatment 8-25min；It is passed through the most rapidly steam to steam explosion
Pressure inside the tank is 1.3-1.7MPa, and after Steam explosion treatment 0.5-2.5min, room temperature is concentrated into relative density
1.10-1.20, it is spray-dried concentrated solution, obtains powder body；
S32, in powder body add 3-8 times of water, be by mass percentage 0.5-2% ratio add neutrality egg
White enzyme, enzymolysis 0.5-2h at 30-50 DEG C, filters, obtains enzymolysis solution；
S33, by enzymolysis solution directly by neutral alumina column, resin column blade diameter length ratio is 1: 6-1: 12, point
Not with 1-3 times of cylinder hydrops, the organic solution eluting remove impurity of 1-2 times of column volume 95%, with 6-10 times of cylinder
Organic solvent (1:1) eluant solution of long-pending 0.3-0.7% glacial acetic acid-50%, collects eluent；
S34, by eluent concentrate drying, obtain Olive leaf P.E；
S4, the preparation of Fructus Foeniculi extract:
S41, being placed in steam-explosion jar by dry Fructus Foeniculi, being first passed through nitrogen to steam explosion pressure inside the tank is
0.6-1.4MPa, explosion treatment 8-25min；Being passed through the most rapidly steam to steam explosion pressure inside the tank is
1.4-1.8MPa, after Steam explosion treatment 0.5-2.5min, room temperature is concentrated into relative density 1.10-1.20,
It is spray-dried concentrated solution, obtains powder body；
S42, powder body is carried out CO2Supercritical extraction, fluid extraction pressure is 30-40MPa, extraction temperature
30-40 DEG C, CO2Fluid flow is 700-800L/h, and extraction time is 3-5h, obtains Fructus Foeniculi extract；
S5, the preparation of Radix Glycyrrhizae extract:
After dry Milk Thistle flash extracter is processed, according to 1:(5-10) weight ratio, throwing
Enter alcohol organic solvent to carry out extracting, filtering, concentrate drying, obtain Radix Glycyrrhizae extract；
S6, the preparation of Radix Ophiopogonis extract:
Being placed in steam-explosion jar dry Radix Ophiopogonis, being first passed through nitrogen to steam explosion pressure inside the tank is 0.6-1.4MPa,
Explosion treatment 8-25min；Being passed through the most rapidly steam to steam explosion pressure inside the tank is 1.4-1.8MPa, and steam is quick-fried
After tear reason 0.5-2.5min, room temperature adds ethanol to alcohol content after being concentrated into relative density 1.10-1.20 be hundred
Proportion by subtraction 60-80%, collects precipitation after standing overnight, precipitation sephadex column carries out isolated and purified, vacuum
Lyophilization, obtains Radix Ophiopogonis extract；
S7, the preparation of Exocarpium Citri Rubrum extract:
By dry Exocarpium Citri Rubrum boiling, filtering, it is 1.05-1.30 that decocting liquid is concentrated into relative density, adds
Ethanol or (with) methanol carries out precipitate with ethanol, has precipitate to occur, filter, obtain precipitate, after drying, obtain Fructus Citri tangerinae
Sage extract；
S8, the preparation of Chinese medicine extraction mixture:
Weigh Caulis Hederae Sinensis extract 42-62 part, Milk Thistle extract 5-10 part, Olive leaf P.E 3-5
Part, Fructus Foeniculi extract 6-12 part, Radix Glycyrrhizae extract 10-15 part, Radix Ophiopogonis extract 10-15 part, Exocarpium Citri Rubrum
Extract 10-15 part, Rhizoma Polygonati Odorati extract 8-10 part are placed in mixing and blending machine and mix, and obtain mixed vaccine
Agent.
Wherein, described organic solvent is the turpentine derivatives of natural origin.
Wherein, described turpentine derivatives is the isomery of pinene, disproportionation products.
Wherein, the one during described alcohol organic solvent is methanol, ethanol and ethylene glycol.
The method have the advantages that
By special technique, obtain the higher Caulis Hederae Sinensis extract of purity, Milk Thistle extract, Fructus Canarii albi
Leaf extract, Fructus Foeniculi extract, Radix Glycyrrhizae extract, Radix Ophiopogonis extract, Exocarpium Citri Rubrum extract and Rhizoma Polygonati Odorati extract
And they are combined with optimum proportioning, cough is had preferable therapeutical effect, safety non-toxic,
Evident in efficacy, do not develop immunity to drugs, clinical effective rate is up to 97%, and cure rate reaches 92%.
Detailed description of the invention
In order to make objects and advantages of the present invention clearer, below in conjunction with embodiment, the present invention is carried out
Further describe.Should be appreciated that specific embodiment described herein only in order to explain the present invention,
It is not intended to limit the present invention.
In following example, the organic solvent used is the turpentine derivatives of natural origin；Oleum Terebinthinae spreads out
Biology is the isomery of pinene, disproportionation products；The alcohol organic solvent used is methanol, ethanol and ethylene glycol
In one
Embodiment 1
S1, the preparation of Caulis Hederae Sinensis extract:
S11, dry Rhizoma Calystegiae Hederaceae is pulverized after aqueous solution carry out membrance separation by ultrafilter membrane after, collection
Permeate, is concentrated into the 10% of original volume, obtains concentrated solution；
S12, by the concentrated solution of gained with the flow velocity of 3BV/h by macroporous resin column, after dynamic adsorption is saturated,
Colourless to effluent with the above-mentioned macroporous resin column of flow velocity drip washing of 5BV/h with deionized water, then use volume fraction
Be 50%% organic solvent carry out eluting with the flow velocity of 8BV/h, collect eluent, concentrating under reduced pressure, obtain leaching
Cream；
S13, by after extractum water dissolution with the flow velocity of 3BV/h by polyamide column, after dynamic adsorption is saturated,
With 3BV deionized water with the above-mentioned polyamide column of flow velocity drip washing of 2BV/h, then it is 30% have by volume fraction
Machine solvent aqueous solution carries out eluting with the flow velocity of 5BV/h, collects and has eluent, is spray-dried, obtains Caulis Hederae Sinensis
Extract；
S2, the preparation of Milk Thistle extract:
Being processed by dry Milk Thistle flash extracter, gained extracting solution first heats with high heat, uses after boiling
Slow fire heating 1h, hollow fiber ultrafiltration membrane filters；Medicinal residues add 15 times of soak by water twice, hollow fiber ultrafiltration membrane
Filter, merge three filtrates, be concentrated into 1.5g/ml；It is slowly added to 90% organic solvent, until organic molten
Agent concentration is 55%, cold preservation 8 hours, and 2000r/min goes supernatant, precipitation to dry after being centrifuged 15min,
Obtain Milk Thistle extract；
S3, the preparation of Olive leaf P.E:
S31, by after Folium olive saline soak 1 hour, dry and be placed in steam-explosion jar, be first passed through nitrogen extremely
Steam explosion pressure inside the tank is 0.7MPa, explosion treatment 25min；It is passed through the most rapidly steam to steam explosion pressure inside the tank
For 1.3MPa, after Steam explosion treatment 2.5min, room temperature is concentrated into relative density 1.10, is spray-dried dense
Contracting liquid, obtains powder body；
S32, in powder body add 3 times of water, be by mass percentage 0.5% ratio add neutral protease,
Enzymolysis 0.5h at 30 DEG C, filters, obtains enzymolysis solution；
S33, by enzymolysis solution directly by neutral alumina column, resin column blade diameter length ratio is 1: 6-1: 12, point
Not with 1-3 times of cylinder hydrops, the organic solution eluting remove impurity of 1-2 times of column volume 95%, with 6-10 times of cylinder
Organic solvent (1:1) eluant solution of long-pending 0.3-0.7% glacial acetic acid-50%, collects eluent；
S34, by eluent concentrate drying, obtain Olive leaf P.E；
S4, the preparation of Fructus Foeniculi extract:
S41, being placed in steam-explosion jar by dry Fructus Foeniculi, being first passed through nitrogen to steam explosion pressure inside the tank is 0.6MPa,
Explosion treatment 25min；Being passed through the most rapidly steam to steam explosion pressure inside the tank is 1.4MPa, Steam explosion treatment
After 2.5min, room temperature is concentrated into relative density 1.10, is spray-dried concentrated solution, obtains powder body；
S42, powder body is carried out CO2Supercritical extraction, fluid extraction pressure is 30MPa, extraction temperature 30 DEG C,
CO2Fluid flow is 700L/h, and extraction time is 3h, obtains Fructus Foeniculi extract；
S5, the preparation of Radix Glycyrrhizae extract:
After being processed by dry Milk Thistle flash extracter, according to 1:5 weight ratio, put into alcohols
Organic solvent carries out extracting, filtering, concentrate drying, obtains Radix Glycyrrhizae extract；
S6, the preparation of Radix Ophiopogonis extract:
Being placed in steam-explosion jar dry Radix Ophiopogonis, being first passed through nitrogen to steam explosion pressure inside the tank is 0.6MPa, explosion
Process 25min；Being passed through the most rapidly steam to steam explosion pressure inside the tank is 1.4MPa, Steam explosion treatment 2.5
After min, room temperature adds ethanol after being concentrated into relative density 1.10 be percentage ratio 60% to alcohol content, after standing overnight
Collecting precipitation, precipitation sephadex column carries out isolated and purified, and vacuum lyophilization obtains Radix Ophiopogonis extract；
S7, the preparation of Exocarpium Citri Rubrum extract:
By dry Exocarpium Citri Rubrum boiling, filtering, it is 1.05 that decocting liquid is concentrated into relative density, adds ethanol
Or (with) methanol carries out precipitate with ethanol, has precipitate to occur, filter, obtain precipitate, after drying, obtain Exocarpium Citri Rubrum and carry
Take thing；
S8, the preparation of Chinese medicine extraction mixture:
Weigh Caulis Hederae Sinensis extract 42 parts, Milk Thistle extract 5 parts, Olive leaf P.E 3 parts, Fructus Foeniculi
Extract 6 parts, Radix Glycyrrhizae extract 10 parts, Radix Ophiopogonis extract 10 parts, Exocarpium Citri Rubrum extract 10 parts, Rhizoma Polygonati Odorati
Extract 8 parts is placed in mixing and blending machine and mixes, and obtains mix bacterium agent.
Embodiment 2
S1, the preparation of Caulis Hederae Sinensis extract:
S11, dry Rhizoma Calystegiae Hederaceae is pulverized after aqueous solution carry out membrance separation by ultrafilter membrane after, collection
Permeate, is concentrated into the 10% of original volume, obtains concentrated solution；
S12, by the concentrated solution of gained with the flow velocity of 7BV/h by macroporous resin column, after dynamic adsorption is saturated,
Colourless to effluent with the above-mentioned macroporous resin column of flow velocity drip washing of 8BV/h with deionized water, then use volume fraction
Be 70% organic solvent carry out eluting with the flow velocity of 12BV/h, collect eluent, concentrating under reduced pressure, obtain leaching
Cream；
S13, by after extractum water dissolution with the flow velocity of 5BV/h by polyamide column, after dynamic adsorption is saturated,
With 7BV deionized water with the above-mentioned polyamide column of flow velocity drip washing of 10BV/h, then it is 50% by volume fraction
Aqueous solutions of organic solvent carries out eluting with the flow velocity of 10BV/h, collects and has eluent, is spray-dried, often obtains
Spring rattan extract；
S2, the preparation of Milk Thistle extract:
Being processed by dry Milk Thistle flash extracter, gained extracting solution first heats with high heat, uses after boiling
Slow fire heating 1.5h, hollow fiber ultrafiltration membrane filters；Medicinal residues add 25 times of soak by water twice, Hollow Fiber Ultrafiltration
Membrane filtration, merges three filtrates, is concentrated into 1.5g/ml；It is slowly added to 100% organic solvent, until having
Machine solvent strength is 65%, cold preservation 9 hours, and 4000r/min goes supernatant, precipitation to dry after being centrifuged 25min
Dry, obtain Milk Thistle extract；
S3, the preparation of Olive leaf P.E:
S31, by after Folium olive saline soak 2 hours, dry and be placed in steam-explosion jar, be first passed through nitrogen extremely
Steam explosion pressure inside the tank is 1.3MPa, explosion treatment 8min；Being passed through the most rapidly steam to steam explosion pressure inside the tank is
1.7MPa, after Steam explosion treatment 0.5min, room temperature is concentrated into relative density 1.20, is spray-dried and concentrates
Liquid, obtains powder body；
S32, in powder body add 8 times of water, be by mass percentage 0.5-2% ratio addition neutral protein
Enzyme, enzymolysis 2h at 50 DEG C, filters, obtains enzymolysis solution；
S33, by enzymolysis solution directly by neutral alumina column, resin column blade diameter length ratio is 1: 6-1: 12, point
Not with 1-3 times of cylinder hydrops, the organic solution eluting remove impurity of 1-2 times of column volume 95%, with 6-10 times of cylinder
Organic solvent (1:1) eluant solution of long-pending 0.3-0.7% glacial acetic acid-50%, collects eluent；
S34, by eluent concentrate drying, obtain Olive leaf P.E；
S4, the preparation of Fructus Foeniculi extract:
S41, being placed in steam-explosion jar by dry Fructus Foeniculi, being first passed through nitrogen to steam explosion pressure inside the tank is 1.4MPa,
Explosion treatment 8min；Being passed through the most rapidly steam to steam explosion pressure inside the tank is 1.8MPa, Steam explosion treatment
After 0.5min, room temperature is concentrated into relative density 1.20, is spray-dried concentrated solution, obtains powder body；
S42, powder body is carried out CO2Supercritical extraction, fluid extraction pressure is 40MPa, extraction temperature 40 DEG C,
CO2Fluid flow is 800L/h, and extraction time is 5h, obtains Fructus Foeniculi extract；
S5, the preparation of Radix Glycyrrhizae extract:
After being processed by dry Milk Thistle flash extracter, according to 1:10 weight ratio, put into alcohols
Organic solvent carries out extracting, filtering, concentrate drying, obtains Radix Glycyrrhizae extract；
S6, the preparation of Radix Ophiopogonis extract:
Being placed in steam-explosion jar dry Radix Ophiopogonis, being first passed through nitrogen to steam explosion pressure inside the tank is 1.4MPa, explosion
Process 8min；Being passed through the most rapidly steam to steam explosion pressure inside the tank is 1.8MPa, Steam explosion treatment 0.5min
After, room temperature adds ethanol after being concentrated into relative density 1.20 be percentage ratio 80% to alcohol content, receives after standing overnight
Collection precipitation, precipitation sephadex column carries out isolated and purified, and vacuum lyophilization obtains Radix Ophiopogonis extract；
S7, the preparation of Exocarpium Citri Rubrum extract:
By dry Exocarpium Citri Rubrum boiling, filtering, it is 1.30 that decocting liquid is concentrated into relative density, adds ethanol
Or (with) methanol carries out precipitate with ethanol, has precipitate to occur, filter, obtain precipitate, after drying, obtain Exocarpium Citri Rubrum and carry
Take thing；
S8, the preparation of Chinese medicine extraction mixture:
Weigh Caulis Hederae Sinensis extract 62 parts, Milk Thistle extract 10 parts, Olive leaf P.E 5 parts, Fructus Foeniculi
Extract 12 parts, Radix Glycyrrhizae extract 15 parts, Radix Ophiopogonis extract 15 parts, Exocarpium Citri Rubrum extract 15 parts, Rhizoma Polygonati Odorati
Extract 10 parts is placed in mixing and blending machine and mixes, and obtains mix bacterium agent.
Embodiment 3
S1, the preparation of Caulis Hederae Sinensis extract:
S11, dry Rhizoma Calystegiae Hederaceae is pulverized after aqueous solution carry out membrance separation by ultrafilter membrane after, collection
Permeate, is concentrated into the 10% of original volume, obtains concentrated solution；
S12, by the concentrated solution of gained with the flow velocity of 5BV/h by macroporous resin column, after dynamic adsorption is saturated,
Colourless to effluent with the above-mentioned macroporous resin column of flow velocity drip washing of 6.5BV/h with deionized water, then use volume integral
Number be 60% organic solvent carry out eluting with the flow velocity of 15BV/h, collect eluent, concentrating under reduced pressure,
Extractum；
S13, by after extractum water dissolution with the flow velocity of 4BV/h by polyamide column, after dynamic adsorption is saturated,
With 5BV deionized water with the above-mentioned polyamide column of flow velocity drip washing of 6BV/h, then it is 40% have by volume fraction
Machine solvent aqueous solution carries out eluting with the flow velocity of 7.5BV/h, collects and has eluent, is spray-dried, get Chang Chun
Rattan extract；
S2, the preparation of Milk Thistle extract:
Being processed by dry Milk Thistle flash extracter, gained extracting solution first heats with high heat, uses after boiling
Slow fire heating 1.25h, hollow fiber ultrafiltration membrane filters；Medicinal residues add 15-25 times of soak by water twice, doughnut
Ultrafiltration membrance filter, merges three filtrates, is concentrated into 1.5g/ml；It is slowly added to 95% organic solvent, until
Organic solvent concentration is 60%, cold preservation 8.5 hours, and 3000r/min removes supernatant after being centrifuged 20min, heavy
Form sediment and dry, obtain Milk Thistle extract；
S3, the preparation of Olive leaf P.E:
S31, by after Folium olive saline soak 1.5 hours, dry and be placed in steam-explosion jar, be first passed through nitrogen
It is 1MPa to steam explosion pressure inside the tank, explosion treatment 16.5min；It is passed through the most rapidly steam intrinsic pressure to steam-explosion jar
Power is 1.5MPa, and after Steam explosion treatment 1.5min, room temperature is concentrated into relative density 1.15, is spray-dried
Concentrated solution, obtains powder body；
S32, in powder body add 5.5 times of water, be by mass percentage 0.5-2% ratio add neutrality egg
White enzyme, enzymolysis 1.25h at 40 DEG C, filters, obtains enzymolysis solution；
S33, by enzymolysis solution directly by neutral alumina column, resin column blade diameter length ratio is 1: 9, uses 1-3 respectively
Times cylinder hydrops, the organic solution eluting remove impurity of 1-2 times of column volume 95%, with 6-10 times of column volume
Organic solvent (1:1) eluant solution of 0.3-0.7% glacial acetic acid-50%, collects eluent；
S34, by eluent concentrate drying, obtain Olive leaf P.E；
S4, the preparation of Fructus Foeniculi extract:
S41, being placed in steam-explosion jar by dry Fructus Foeniculi, being first passed through nitrogen to steam explosion pressure inside the tank is 1MPa,
Explosion treatment 16.5min；Being passed through the most rapidly steam to steam explosion pressure inside the tank is 1.6MPa, at steam explosion
After reason 1.5min, room temperature is concentrated into relative density 1.15, is spray-dried concentrated solution, obtains powder body；
S42, powder body is carried out CO2Supercritical extraction, fluid extraction pressure is 35MPa, extraction temperature 35 DEG C,
CO2Fluid flow is 750L/h, and extraction time is 4h, obtains Fructus Foeniculi extract；
S5, the preparation of Radix Glycyrrhizae extract:
After being processed by dry Milk Thistle flash extracter, according to 1:7.5 weight ratio, put into alcohol
Class organic solvent carries out extracting, filtering, concentrate drying, obtains Radix Glycyrrhizae extract；
S6, the preparation of Radix Ophiopogonis extract:
Being placed in steam-explosion jar dry Radix Ophiopogonis, being first passed through nitrogen to steam explosion pressure inside the tank is 1MPa, at explosion
Reason 16.5min；Being passed through the most rapidly steam to steam explosion pressure inside the tank is 1.6MPa, Steam explosion treatment 1.5min
After, room temperature adds ethanol after being concentrated into relative density 1.15 be percentage ratio 70% to alcohol content, receives after standing overnight
Collection precipitation, precipitation sephadex column carries out isolated and purified, and vacuum lyophilization obtains Radix Ophiopogonis extract；
S7, the preparation of Exocarpium Citri Rubrum extract:
By dry Exocarpium Citri Rubrum boiling, filtering, it is 1.175 that decocting liquid is concentrated into relative density, adds ethanol
Or (with) methanol carries out precipitate with ethanol, has precipitate to occur, filter, obtain precipitate, after drying, obtain Exocarpium Citri Rubrum and carry
Take thing；
S8, the preparation of Chinese medicine extraction mixture:
Weigh Caulis Hederae Sinensis extract 52 parts, Milk Thistle extract 7.5 parts, Olive leaf P.E 4 parts, fennel
Fragrant extract 9 parts, Radix Glycyrrhizae extract 12.5 parts, Radix Ophiopogonis extract 12.5 parts, Exocarpium Citri Rubrum extract 12.5
Part, Rhizoma Polygonati Odorati extract 9 parts are placed in mixing and blending machine and mix, and obtain mix bacterium agent.
The above is only the preferred embodiment of the present invention, it is noted that common for the art
For technical staff, under the premise without departing from the principles of the invention, it is also possible to make some improvements and modifications,
These improvements and modifications also should be regarded as protection scope of the present invention.
Claims (5)
1. a traditional Chinese medicine extract composition, it is characterised in that described extract is by the group of following weight portion
Divide and be prepared from:
Caulis Hederae Sinensis extract 42-62 part, Milk Thistle extract 5-10 part, Olive leaf P.E 3-5 part,
Fructus Foeniculi extract 6-12 part, Radix Glycyrrhizae extract 10-15 part, Radix Ophiopogonis extract 10-15 part, Exocarpium Citri Rubrum are extracted
Thing 10-15 part, Rhizoma Polygonati Odorati extract 8-10 part.
2. the preparation method of a traditional Chinese medicine extract composition, it is characterised in that comprise the steps:
S1, the preparation of Caulis Hederae Sinensis extract:
S11, dry Rhizoma Calystegiae Hederaceae is pulverized after aqueous solution carry out membrance separation by ultrafilter membrane after, collection
Permeate, is concentrated into the 10% of original volume, obtains concentrated solution；
S12, by the concentrated solution of gained with the flow velocity of 3-7BV/h by macroporous resin column, dynamic adsorption is saturated
After, colourless to effluent with the above-mentioned macroporous resin column of flow velocity drip washing of 5-8BV/h with deionized water, then use body
Fraction is that the organic solvent of 50%-70% carries out eluting with the flow velocity of 8-12BV/h, collects eluent, subtracts
Pressure concentrates, and obtains extractum；
S13, by after extractum water dissolution with the flow velocity of 3-5BV/h by polyamide column, dynamic adsorption is saturated
After, with 3-7BV deionized water with the above-mentioned polyamide column of flow velocity drip washing of 2-10BV/h, then use volume fraction
Aqueous solutions of organic solvent for 30%-50% carries out eluting with the flow velocity of 5-10BV/h, collects and has eluent,
It is spray-dried, obtains Caulis Hederae Sinensis extract；
S2, the preparation of Milk Thistle extract:
Being processed by dry Milk Thistle flash extracter, gained extracting solution first heats with high heat, uses after boiling
Slow fire heating 1-1.5h, hollow fiber ultrafiltration membrane filters；Medicinal residues add 15-25 times of soak by water twice, and hollow is fine
Dimension ultrafiltration membrance filter, merges three filtrates, is concentrated into 1.5g/ml；It is slowly added to 90-100% organic solvent,
Until organic solvent concentration is 55-65%, cold preservation 8-9 hour, after 2000-4000r/min is centrifuged 15-25min
Supernatant, precipitation is gone to dry, obtain Milk Thistle extract；
S3, the preparation of Olive leaf P.E:
S31, by after Folium olive saline soak 1-2 hour, dry and be placed in steam-explosion jar, be first passed through nitrogen
It is 0.7-1.3MPa to steam explosion pressure inside the tank, explosion treatment 8-25min；It is passed through the most rapidly steam to steam explosion
Pressure inside the tank is 1.3-1.7MPa, and after Steam explosion treatment 0.5-2.5min, room temperature is concentrated into relative density
1.10-1.20, it is spray-dried concentrated solution, obtains powder body；
S32, in powder body add 3-8 times of water, be by mass percentage 0.5-2% ratio add neutrality egg
White enzyme, enzymolysis 0.5-2h at 30-50 DEG C, filters, obtains enzymolysis solution；
S33, by enzymolysis solution directly by neutral alumina column, resin column blade diameter length ratio is 1: 6-1: 12, point
Not with 1-3 times of cylinder hydrops, the organic solution eluting remove impurity of 1-2 times of column volume 95%, with 6-10 times of cylinder
Organic solvent (1:1) eluant solution of long-pending 0.3-0.7% glacial acetic acid-50%, collects eluent；
S34, by eluent concentrate drying, obtain Olive leaf P.E；
S4, the preparation of Fructus Foeniculi extract:
S41, being placed in steam-explosion jar by dry Fructus Foeniculi, being first passed through nitrogen to steam explosion pressure inside the tank is
0.6-1.4MPa, explosion treatment 8-25min；Being passed through the most rapidly steam to steam explosion pressure inside the tank is
1.4-1.8MPa, after Steam explosion treatment 0.5-2.5min, room temperature is concentrated into relative density 1.10-1.20,
It is spray-dried concentrated solution, obtains powder body；
S42, powder body is carried out CO2Supercritical extraction, fluid extraction pressure is 30-40MPa, extraction temperature
30-40 DEG C, CO2Fluid flow is 700-800L/h, and extraction time is 3-5h, obtains Fructus Foeniculi extract；
S5, the preparation of Radix Glycyrrhizae extract:
After dry Milk Thistle flash extracter is processed, according to 1:(5-10) weight ratio, throwing
Enter alcohol organic solvent to carry out extracting, filtering, concentrate drying, obtain Radix Glycyrrhizae extract；
S6, the preparation of Radix Ophiopogonis extract:
Being placed in steam-explosion jar dry Radix Ophiopogonis, being first passed through nitrogen to steam explosion pressure inside the tank is 0.6-1.4MPa,
Explosion treatment 8-25min；Being passed through the most rapidly steam to steam explosion pressure inside the tank is 1.4-1.8MPa, and steam is quick-fried
After tear reason 0.5-2.5min, room temperature adds ethanol to alcohol content after being concentrated into relative density 1.10-1.20 be hundred
Proportion by subtraction 60-80%, collects precipitation after standing overnight, precipitation sephadex column carries out isolated and purified, vacuum
Lyophilization, obtains Radix Ophiopogonis extract；
S7, the preparation of Exocarpium Citri Rubrum extract:
By dry Exocarpium Citri Rubrum boiling, filtering, it is 1.05-1.30 that decocting liquid is concentrated into relative density, adds
Ethanol or (with) methanol carries out precipitate with ethanol, has precipitate to occur, filter, obtain precipitate, after drying, obtain Fructus Citri tangerinae
Sage extract；
S8, the preparation of Chinese medicine extraction mixture:
Weigh Caulis Hederae Sinensis extract 42-62 part, Milk Thistle extract 5-10 part, Olive leaf P.E 3-5
Part, Fructus Foeniculi extract 6-12 part, Radix Glycyrrhizae extract 10-15 part, Radix Ophiopogonis extract 10-15 part, Exocarpium Citri Rubrum
Extract 10-15 part, Rhizoma Polygonati Odorati extract 8-10 part are placed in mixing and blending machine and mix, and obtain mixed vaccine
Agent.
The preparation method of a kind of traditional Chinese medicine extract composition the most according to claim 2, it is characterised in that
Described organic solvent is the turpentine derivatives of natural origin.
The preparation method of a kind of traditional Chinese medicine extract composition the most according to claim 3, it is characterised in that
Described turpentine derivatives is the isomery of pinene, disproportionation products.
The preparation method of a kind of traditional Chinese medicine extract composition the most according to claim 2, it is characterised in that
Described alcohol organic solvent is the one in methanol, ethanol and ethylene glycol.
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| CN106490600A (en) * | 2016-10-09 | 2017-03-15 | 上海兰葹生物科技有限公司 | A kind of Herba Dendrobii compound tablet, injection, electuary |
| CN106490608A (en) * | 2016-10-09 | 2017-03-15 | 上海兰葹生物科技有限公司 | A kind of Herba Dendrobii enhancing immunity oral liquid, electuary, capsule, tablet |
| CN106560052A (en) * | 2016-11-04 | 2017-04-12 | 昔阳县大寨绿草湾牧业有限公司 | Feed additive capable of improving disease resistance of livestock and poultry |
| CN106665818A (en) * | 2017-03-17 | 2017-05-17 | 运城学院 | Preparation method and fresh keeping technology of sweet cherry fresh keeping agent |
| CN106721699A (en) * | 2016-11-30 | 2017-05-31 | 江苏食品药品职业技术学院 | A kind of sobering-up beverage and preparation method thereof |
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| CN110755649A (en) * | 2019-11-19 | 2020-02-07 | 华润三九（雅安）药业有限公司 | Sterilizing method of ginseng and aconite extract |
| CN112210269A (en) * | 2019-07-09 | 2021-01-12 | 常州市大使涂料有限公司 | Nontoxic antibacterial coating for drinking water tank |
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| CN106269143A (en) * | 2016-08-31 | 2017-01-04 | 华南农业大学 | A kind of Chinese crude drug preprocess method |
| CN106490600A (en) * | 2016-10-09 | 2017-03-15 | 上海兰葹生物科技有限公司 | A kind of Herba Dendrobii compound tablet, injection, electuary |
| CN106490608A (en) * | 2016-10-09 | 2017-03-15 | 上海兰葹生物科技有限公司 | A kind of Herba Dendrobii enhancing immunity oral liquid, electuary, capsule, tablet |
| CN106560052A (en) * | 2016-11-04 | 2017-04-12 | 昔阳县大寨绿草湾牧业有限公司 | Feed additive capable of improving disease resistance of livestock and poultry |
| CN106721699A (en) * | 2016-11-30 | 2017-05-31 | 江苏食品药品职业技术学院 | A kind of sobering-up beverage and preparation method thereof |
| CN106937747A (en) * | 2017-02-24 | 2017-07-11 | 江苏食品药品职业技术学院 | One kind is sobered up lozenge and preparation method thereof |
| CN106665818A (en) * | 2017-03-17 | 2017-05-17 | 运城学院 | Preparation method and fresh keeping technology of sweet cherry fresh keeping agent |
| CN106860768A (en) * | 2017-04-13 | 2017-06-20 | 河南中医药大学 | A kind of Chinese medicine compound prescription for treating the cancer of the esophagus |
| CN112210269A (en) * | 2019-07-09 | 2021-01-12 | 常州市大使涂料有限公司 | Nontoxic antibacterial coating for drinking water tank |
| CN110755649A (en) * | 2019-11-19 | 2020-02-07 | 华润三九（雅安）药业有限公司 | Sterilizing method of ginseng and aconite extract |
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