CN101306077A - Chinese traditional injection preparation for treating cancer and its preparation method - Google Patents
Chinese traditional injection preparation for treating cancer and its preparation method Download PDFInfo
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- CN101306077A CN101306077A CNA200810301949XA CN200810301949A CN101306077A CN 101306077 A CN101306077 A CN 101306077A CN A200810301949X A CNA200810301949X A CN A200810301949XA CN 200810301949 A CN200810301949 A CN 200810301949A CN 101306077 A CN101306077 A CN 101306077A
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Abstract
The invention discloses a Chinese traditional medicinal injection for curing cancers and a preparation method thereof. The Chinese traditional medicinal injection is prepared from 0.9 to 2.1 parts of cantharis, 30 to 70 parts of ginseng, 60 to 140 parts of milk veteh and 90 to 210 parts of acanthopanax. Ginseng, milk veteh and acanthopanax are aqueously extracted and ethanol extracted respectively. The extracted solution is condensed, and micro-filtered with an inorganic ceramic membrane before the extracted solution is refined with polyamide resin; then the refined solution is hyperfiltrated with an organic membrane, and is mixed with aqueous extract of cantharis. In this way, the Chinese traditional medicine injection is prepared. By comparing the invention with the prior art, in the method for preparing the Chinese traditional medicine injection, the medicinal materials are aqueously extracted and ethanol extracted; the extracted solution is purified, separated and condensed by combining the membrane separation technology and refining with resin; accordingly, the Chinese traditional medicine injection is rich in effective ingredients. By substituting the physical method for the traditional chemical process, macromolecular substance in the extracted solution of the Chinese traditional medicine can be effectively removed without introducing other inorganic ions, thus keeping the characteristics of the compound preparation of the Chinese traditional medicine, and effectively reducing the adverse effect of the medicaments, improving the curative effect, and improving and ensuring the product quality.
Description
Technical field:
The present invention relates to a kind of traditional medicine Injectio for the treatment of cancer and preparation method thereof, belong to technical field of traditional Chinese medicine pharmacy.
Background technology:
Traditional medicine Injectio is to be raw material with the Chinese crude drug, the sterilization preparation of making through steps such as extracting, separate, be refining.It has changed the traditional administering mode of Chinese medicine, and it is rapid to possess drug effect, the bioavailability height, dosage is more accurate, be applicable to the case of unsuitable oral or emergency and severe disease, and can make characteristics such as some drugs performance orientation or site-specific delivery of drugs, brought into play the effect of treatment by Chinese herbs acute disease serious symptom and difficult disease preferably.But, increasing along with clinical practice, Chinese medicine causes that the incident of adverse effect occurs repeatedly, and has caused vast medical worker's concern.The main cause of traditional medicine Injectio generation untoward reaction is: the chemical analysis of Chinese medicine raw material is very complicated, and the some of them macromolecular compound very easily causes allergic reaction as tannin, animal and vegetable protein; In addition, because the production technology of Chinese medicine owes maturation, cause indivedual lot number medicinal liquid purity not good enough, and then cause allergic reaction.
Ad pro injection is the herbal species that the applicant develops, make by Radix Ginseng, the Radix Astragali, Radix Et Caulis Acanthopanacis Senticosi and Mylabris 4 flavor Chinese medicines, effect with heat-clearing and toxic substances removing, repercussive eliminating stagnation, be mainly used in the treatment of primary hepatocarcinoma, pulmonary carcinoma, rectal cancer, malignant lymphoma, gynecologic malignant tumor etc. clinically, record in 20 of Ministry of Public Health ministry standards.The applicant discloses the preparation technology of ad pro injection in the patent No. is 03117114.1 " treatment tumor traditional medicine Injectio and preparation method thereof ": adopt panaxynol, moisture is carried, its excess-three flavor water is carried, the stone sulfur sedimentation method are handled, the method of precipitate with ethanol is obtained effective ingredient, this method constitutes simple, the loss of active drug composition is many, yield is low, has consumed a large amount of ethanol simultaneously, and energy consumption is big, the production process complexity, cycle is long, and efficient is low, the cost height, production security is poor, big to environmental effect, cause composition variation instability in the medicinal liquid easily, also make the polysaccharide component that has antitumor action in a large number not obtain utilizing.
Application number is that 200410004443.4 patent documentation discloses a kind of Chinese medicine lyophilized injectable powder preparation method that is used for the treatment of tumor, adopt alcohol extraction, macroporous adsorbent resin remove impurity and water is carried, the method for ultrafiltration combines, this technology has been introduced a large amount of polysaccharide that contained in the medical material, curative effect is increased, but it does not have effectively catching to polysaccharide, this is because the molecular weight ranges of polysaccharide is very big, the medicinal efficient of the polysaccharide of minimum molecule is low, and the polysaccharide of macromolecule causes untoward reaction again easily in drug administration by injection; In macroporous resin eluting purification step, the selection of resin choice, eluent, the control of elution speed have all greatly influenced obtaining effective ingredient simultaneously.
In addition, the conventional extracting method of medical material is that water is carried or alcohol extraction, but medical material is applicable to that water is carried actually, alcohol extraction still is pure water in conjunction with being to need the pharmacy worker to remove an emphasis of studying also, above-mentioned patent documentation is in the extraction process of medical material, extraction research to single medical material is not deep enough, cause the problem that single medical material extracts active ingredients efficient is low in the preparation, impurity content is high easily, so explore a kind of preparation method of feasible effective traditional medicine Injectio, to improve curative effect, the untoward reaction that reduces traditional medicine Injectio is the problem that medical worker will solve.
Summary of the invention:
The objective of the invention is to: a kind of traditional medicine Injectio for the treatment of cancer and preparation method thereof is provided.The present invention with medical material carry out alcohol respectively, moisture is carried, the method that adopts membrane separation technique binding resin refinement treatment such as inorganic ceramic membrane microfiltration, organic membrane ultrafiltration to combine is then carried out purification, separation to extracting solution and is concentrated, active constituent-enriched, filter out impurities, thereby reduced the untoward reaction of medicine, improved curative effect.
The present invention is achieved in that a kind of traditional medicine Injectio for the treatment of cancer, according to listed as parts by weight, it is made as follows with Mylabris 0.9-2.1 part, Radix Ginseng 30-70 part, Radix Astragali 60-140 part and Radix Et Caulis Acanthopanacis Senticosi 90-210 part: get the Radix Ginseng section, use alcohol reflux, extracting solution reclaims ethanol, and it is standby to get the Radix Ginseng extractive solution; Medicinal residues and Milkvetch Root be water extraction altogether, and extracting solution mixes with the Radix Ginseng extractive solution promptly to get joins the stilbene extracting solution, concentrates, and filters, and be refining, standby; Radix Et Caulis Acanthopanacis Senticosi is pulverized, and uses alcohol reflux, and extracting solution reclaims ethanol, concentrates, and filters, and is refining, standby; Mylabris is pulverized, and decocts with water, and decoction liquor filters, and is standby; The extracting solution of Radix Ginseng, the Radix Astragali and Radix Et Caulis Acanthopanacis Senticosi is carried out ultrafiltration, mix with the Mylabris extracting solution then, add adjuvant or do not add adjuvant, make different ejection preparations with diverse ways.
Say that exactly according to listed as parts by weight, it is made for 150 parts with 1.5 parts of Mylabris, 50 parts of Radix Ginsengs, 100 parts of the Radixs Astragali and Radix Et Caulis Acanthopanacis Senticosi.
Described ejection preparation is hydro-acupuncture preparation, infusion preparation, powder injection formulation or freeze-dried powder.
The preparation method of the traditional medicine Injectio of treatment cancer of the present invention is: get the Radix Ginseng section, use 55%-75% alcohol reflux 2-4 time, merge extractive liquid, reclaims ethanol, and it is standby to get the Radix Ginseng extractive solution; Medicinal residues and Milkvetch Root are total to water extraction 2-4 time, and extracting solution mixes with the Radix Ginseng extractive solution promptly to get joins the stilbene extracting solution, concentrate, and inorganic membrane filtration, resin purification, standby; Radix Et Caulis Acanthopanacis Senticosi is pulverized, the alcohol reflux of usefulness 60%-80% 2-4 time, and merge extractive liquid, reclaims ethanol, concentrates, inorganic membrane filtration, resin purification, standby; Mylabris is pulverized, and crosses the 40-60 mesh sieve, decocts with water 2-4 time, merges decoction liquor, filters, and is standby; The extracting solution of Radix Ginseng, the Radix Astragali and Radix Et Caulis Acanthopanacis Senticosi is carried out ultrafiltration with organic membrane, mix with the Mylabris extracting solution then, add adjuvant or do not add adjuvant, make different ejection preparations with diverse ways.
Preparation method is more specifically: get the Radix Ginseng section, use 55%-75% soak with ethanol 10-14 hour, reflux, extract, is 2-4 time then, adds ethanol 6-10 at every turn and doubly measures, extracts 0.5-2 hour, and merge extractive liquid, reclaims ethanol, and it is standby to get the Radix Ginseng extractive solution; Medicinal residues and Milkvetch Root add 4-6 times of water gaging and extract 2-4 time, and each 0.5-2 hour, merge extractive liquid, mixed with the Radix Ginseng extractive solution promptly to get and joins extracting solution at the beginning of the stilbene; First extracting solution is concentrated, inorganic ceramic film filters, filtered liquid medicine directly goes up polyamide column, 0.5-2ml crosses post with per second, with 1-5 times of column volume deionized water eluting, collect medicinal liquid, with 1-5 times of column volume 0.05-0.2%NaOH eluant solution, collect eluent and transfer PH to 4-6, get promptly that to join the stilbene extract standby; Radix Et Caulis Acanthopanacis Senticosi is pulverized, and uses 60%-80% alcohol reflux 2-4 time, adds ethanol 6-10 at every turn and doubly measures, extracts 0.5-2 hour, and merge extractive liquid, reclaims ethanol, promptly gets Radix Et Caulis Acanthopanacis Senticosi extracting solution just; First extracting solution is concentrated, inorganic ceramic film filters, filtered liquid medicine directly goes up polyamide column, 0.5-2ml crosses post with per second, with 1-5 times of column volume deionized water eluting, collect medicinal liquid, with 1-5 times of column volume 0.05-0.2%NaOH eluant solution, collect eluent and transfer PH to 4-6, it is standby promptly to get Radix Et Caulis Acanthopanacis Senticosi extract; Mylabris is pulverized, and crosses the 40-60 mesh sieve, decocts with water 2-4 time, adds water 6-10 at every turn and doubly measures, extracts 0.5-2 hour, merges decoction liquor, filters, and is standby; To join stilbene extract and Radix Et Caulis Acanthopanacis Senticosi extract and carry out ultrafiltration, mix with the Mylabris extracting solution then, and add adjuvant or do not add adjuvant, make different ejection preparations with diverse ways with organic membrane.
Preferred manufacturing procedure is: get Radix Ginseng section, with 65% soak with ethanol 12 hours, reflux, extract, was 3 times then, and add 8 times of amounts of ethanol at every turn, extracted 1 hour, merge extractive liquid,, recovery ethanol must the Radix Ginseng extractive solution; Medicinal residues and Milkvetch Root add 5 times of water gagings and extract 3 times, and each 1 hour, merge extractive liquid, mixed with the Radix Ginseng extractive solution promptly to get and joins extracting solution at the beginning of the stilbene; First extracting solution is concentrated, filter with inorganic ceramic film then, the water washing effective ingredient that adds 2-3 times of medicine liquid volume amount during filtration several times, filtered liquid medicine directly goes up polyamide column, and 1ml crosses post with per second, with 2 times of column volume deionized water eluting, collect medicinal liquid, with 2 times of column volume 0.1%NaOH eluant solutions, collect eluent and transfer pH to 5, get promptly that to join the stilbene extract standby; Radix Et Caulis Acanthopanacis Senticosi is pulverized, and the alcohol reflux with 70% 3 times adds 8 times of amounts of ethanol at every turn, extracted 1 hour, and merge extractive liquid, reclaims ethanol, promptly gets Radix Et Caulis Acanthopanacis Senticosi extracting solution just; First extracting solution is concentrated, filter with inorganic ceramic film then, the water washing effective ingredient that adds 2-3 times of medicine liquid volume amount during filtration several times, filtered liquid medicine directly goes up polyamide column, and 1ml crosses post with per second, with 2 times of column volume deionized water eluting, collect medicinal liquid, with 2 times of column volume 0.1%NaOH eluant solutions, collect eluent and transfer PH to 5, it is standby promptly to get Radix Et Caulis Acanthopanacis Senticosi extract; Mylabris is pulverized, and crosses 40 mesh sieves, decocts with water 3 times, adds 8 times of amounts of water at every turn, extracts 1 hour, merges decoction liquor, filters, and is standby; To join stilbene extract and Radix Et Caulis Acanthopanacis Senticosi extract and carry out ultrafiltration, mix with the Mylabris extracting solution then, and add adjuvant or do not add adjuvant, make different ejection preparations with diverse ways with the rolling organic membrane.
Wherein, hydro-acupuncture preparation is preparation like this: the extracting solution of the Radix Ginseng behind the ultra filtration, the Radix Astragali and Radix Et Caulis Acanthopanacis Senticosi is mixed with the Mylabris extracting solution,, regulate pH to 4.5-6.0 with the water for injection dissolving, and embedding, sterilization, promptly.
Infusion preparation is preparation like this: the extracting solution of the Radix Ginseng behind the ultra filtration, the Radix Astragali and Radix Et Caulis Acanthopanacis Senticosi is mixed with the Mylabris extracting solution, with the water for injection dissolving, add sodium chloride, calcium chloride, glucose or dextran adjusting etc. and ooze, regulate pH to 4.5-6.0, sterilization, promptly.
Powder injection formulation is preparation like this: the extracting solution of the Radix Ginseng behind the ultra filtration, the Radix Astragali and Radix Et Caulis Acanthopanacis Senticosi mixed with the Mylabris extracting solution,, adds mannitol or lactose or sorbitol, regulate pH to 4.5-6.0 with the water for injection dissolving, and drying, promptly.
Freeze-dried powder is preparation like this: the extracting solution of the Radix Ginseng behind the ultra filtration, the Radix Astragali and Radix Et Caulis Acanthopanacis Senticosi is mixed with the Mylabris extracting solution, dissolve with water for injection, add mannitol or lactose or sorbitol, regulate pH to 4.5-6.0, lyophilization, promptly get the component complexity of Chinese crude drug extracting solution, wherein except effective ingredient, also contain a large amount of impurity, the structure difference of each component, molecular size is also different, when medicinal liquid can be separated each component during by the different filter medium in aperture, therefore can adopt membrane separating method purification and refining.Membrane science and technology are one of state-of-the-art technology in modern separation technology field.Use membrane technology (comprising ultrafilter membrane, micro-filtration membrane, semipermeable membrane, reverse osmosis membrane etc.) can under protozoa system environment, realize separating substances, can efficiently concentrate rich long-pending product, effectively deviate from impurity.The ceramic membrane microfiltration is to serve as a kind of efficient, energy-conservation, the free of contamination new separation technology of filtration medium with the novel inorganic ceramic membrane, has the separation accuracy height, chemical property is stable, the enriched product or the efficient height that filters out impurities, need not that heating concentrates, active ingredient is not destroyed, shorten the production cycle, advantage such as enhance productivity; Resin purification is the treatment technology of new development both at home and abroad in recent years, and field of medicaments particularly natural drug refining in widely utilization, be a kind of effective ways that extract aqueous soluble active constituent in the refining Chinese herbal medicine.Therefore, the method purification refine traditional medicine Injectio that the present invention adopts inorganic ceramic film, polyamide and organic membrane to combine, its characteristics are: replaced traditional chemical method with physical method, can effectively remove the macromolecular substances in the Chinese medicine extraction liquid, do not introduce simultaneously other inorganic ions, the characteristics that kept compound Chinese medicinal preparation preferably can effectively reduce the untoward reaction of medicine.
Technical solutions according to the invention are that the applicant obtains through a large amount of experimental studies, and main content of the test is as follows:
Experimental example 1, extraction process analysis
With reference to the extraction process of ad pro injection, the combination of the Ai Di extraction process being carried out a plurality of schemes is preferred in experiment: to water carry, alcohol extraction, pure moisture carry respectively and studying, and investigates the extraction ratio of Radix Ginseng total saponins; Simultaneously Radix Ginseng, the Radix Astragali, Radix Et Caulis Acanthopanacis Senticosi are extracted respectively and handle, to obtain better extracting method.
1.1 Radix Et Caulis Acanthopanacis Senticosi extract technology
The technology of former ad pro injection is that the medicinal residues after Radix Et Caulis Acanthopanacis Senticosi and the Radix Astragali, Mylabris and the Radix Ginseng alcohol extraction are decocted jointly, and the inventor handles Radix Et Caulis Acanthopanacis Senticosi separately, compares with former method, found that the independent extraction of Radix Et Caulis Acanthopanacis Senticosi is more helped subsequent technique to be handled.
1.1.1 extracting method is selected
Get the Radix Et Caulis Acanthopanacis Senticosi medical material, employing decocts with water respectively, two kinds of methods of alcohol reflux are extracted, and are index with content, extracting solution color and luster, clarity, investigates the extraction ratio of medical material.
Water is carried, alcohol extraction Radix Et Caulis Acanthopanacis Senticosi effect assessment table
| Technology | Color and luster | Content (mg/L) | Clarity |
| Water is carried | Dark brown brown | 744 | Muddy |
| Alcohol extraction | Reddish brown | 1203 | Clear and bright |
The result shows, adopts alcohol extraction process, and clarity is better after treatment for extracting solution, color and luster is more shallow, light brown red; And the Radix Et Caulis Acanthopanacis Senticosi that water is carried is all relatively poor at aspects such as clarity, color and luster, content, and color and luster is darker, and is light brown.So select alcohol extraction.
1.1.2 Study on extraction
The addition of extraction solvent, extraction time and number of times are the key factors that influences extraction process, are index with syringoside content, above parameter are investigated, with preferred optimum process condition.
A. concentration of alcohol is investigated
Sample preparation: get Radix Et Caulis Acanthopanacis Senticosi medical material 50g, pulverize, according to the form below concentration adds alcoholic solution, reflux 3 times, and each 1 hour, merge backflow, filter.
The concentration of alcohol investigation table
| Concentration of alcohol | 50％ | 60％ | 70％ | 80％ | 90％ |
| Content (mg/L) | 853 | 1185 | 1206 | 1217 | 1225 |
Data show in the table, syringoside had almost extracted fully when concentration of alcohol was 60%-80%, and wherein 70% concentration is best, and is both economical reasonable.
B. extraction time is investigated
Get totally 6 parts of Radix Et Caulis Acanthopanacis Senticosi medical material 50g, section, equal amount of alcohol difference reflux 0.5,1,1.5,2,2.5,3 hour filters, and is settled to certain volume, sampling and measuring.The result is as follows:
Extraction time investigation table
| Extraction time | 0.5 | 1 | 1.5 | 2 | 2.5 | 3 |
| Content (mg/L) | 945 | 1048 | 1132 | 1174 | 1181 | 1183 |
Can find out that by data in the table extract after 2 hours, syringoside content does not have obvious change, Radix Et Caulis Acanthopanacis Senticosi extract is described after 2 hours, it is saturated that the stripping of material has been tending towards.Consider actual production efficient, preferred extraction time is 1 hour.
C. the investigation of ethanol consumption
Sample preparation: get totally 3 parts of Radix Et Caulis Acanthopanacis Senticosi medical material 50g, comply with not commensurability 70% ethanol of surface condition adding down, reflux 3 times, each 1 hour, filter, collect filtrate.The result is as follows:
Ethanol consumption investigation table
| Amount of alcohol is the multiple of medical material weight | 4 | 6 | 8 | 10 | 12 | 14 |
| Content (mg/L) | 814 | 1027 | 1156 | 1194 | 1210 | 1212 |
Syringoside content increases with the increasing of amount of alcohol, but to a certain degree not bigger variation of back, so selection ethanol consumption is 6-10 times of medical material weight, preferable amount is 8 times of amounts.
Comprehensive above-mentioned experimental result, the extraction process of decision Radix Et Caulis Acanthopanacis Senticosi medical material is: use 60%-80% alcohol reflux 2-4 time, add ethanol 6-10 at every turn and doubly measured, extract 0.5-2 hour.Be preferably:, add 8 times of amounts of ethanol at every turn, extracted 1 hour with 70% alcohol reflux 3 times.
1.2 extraction of panax ginseng
1.2.1 extracting method is selected
Get the ginseng crude drug, adopt respectively decoct with water, medicinal residues decoct with water three kinds of methods and extract behind the alcohol reflux, alcohol reflux, are index with Radix Ginseng total saponins, extracting solution color and luster, clarity, filtration complexity, investigate the extraction ratio of Radix Ginseng total saponins.
The extraction of panax ginseng table
| Method | Evaluation index | Total saponins | Extract liquid measure | Color and luster | Filter difficulty or ease | Clarity |
| 1 | Water is carried | 240mg/L | 150L | Pale brown (slightly muddy) | Easily | Clear and bright |
| 2 | Alcohol extraction | 320mg/L | 100L | Reddish brown | Difficult | Clear and bright |
| 3 | Alcohol, water combination | 275mg/L | 150L | Color and luster is between (slightly muddy) between the two | Easily | Clear and bright |
Experimental result shows, all can measure ginsenoside Rg1, Rb1, Re in water extract and the alcohol extract, and employing is pure, moisture is put forward the method that combines and extracted the ginseng crude drug, and extracting solution is all obtained good result at aspects such as color and luster, content, filtration difficulty or ease.Though the content that adopts alcohol extraction separately than higher, is considered the refining pure metallization processes of next stage, preferred alcohols, the bonded extracting method of water.
1.2.2 extracting method checking
Choose Radix Ginseng Rubra, Radix Ginseng respectively, Radix Ginseng extracting method of the present invention verified that the result is as follows:
Alcohol water is in conjunction with extracting Radix Ginseng Rubra, Radix Ginseng presentation quality evaluation table
| Radix Ginseng | Character | Color and luster |
| Radix Ginseng | After opalescence, the sterilization a large amount of pale precipitations are arranged | Pale brown |
| Radix Ginseng Rubra | After opalescence, the sterilization a large amount of gray precipitate are arranged | Dark brown red |
1.2.3 alcohol extraction process research
A. extraction time is investigated
Sample preparation: get ginseng crude drug 50g, section adds the 55%-75% alcohol heating reflux 5 times, and each 1 hour, collect each backflow respectively, filter.
Extraction time-Radix Ginseng total saponins table
| Extraction time | 1 | 2 | 3 | 4 | 5 |
| Content (mg/L) | 243 | 274 | 292 | 306 | 311 |
Data show in the table, when extracting 4 times, Radix Ginseng total saponins has almost extracted fully, determines that therefore the Radix Ginseng extraction time is 2-4 time, wherein extracts 3 times and is optimised process, and less expensive is reasonable.
B. the investigation of ethanol consumption
Sample preparation: get totally 3 parts of Radix Ginseng 50g, comply with the different 55%-75% ethanol of surface condition adding down, reflux 3 times, each 1 hour, filter, collect filtrate.The result is as follows:
Ethanol consumption amount Radix Ginseng total saponins table
| Amount of alcohol is the multiple of medical material weight | 4 | 6 | 8 | 10 | 12 | 14 |
| Content (mg/L) | 2536 | 291 | 307 | 314 | 318 | 321 |
The amount of Radix Ginseng total saponins increases with the increasing of amount of alcohol, but to a certain degree not bigger variation of back, so selection ethanol consumption is 6-10 times of medical material weight, preferable amount is 8 times of amounts.
In addition, the inventor finds under study for action, soaks 10-14 hour before the ginseng crude drug is extracted, and the extraction of its total saponins is more complete.So comprehensive The above results, decision ginseng crude drug's extraction process is: use 55%-75% soak with ethanol 10-14 hour, reflux, extract, is 2-4 time then, adds ethanol 6-10 at every turn and doubly measures, extracts 0.5-2 hour.Be preferably:, add 8 times of amounts of ethanol at every turn, extracted 1 hour with 65% soak with ethanol 12 hours, reflux, extract, 3 times.
1.3 Radix Astragali extraction process
Medicinal residues behind the Radix Ginseng alcohol reflux and Milkvetch Root are total to water extraction.The according to the form below amount of water extracts respectively 3 times, and each 1 hour is index with the total solid extraction ratio, investigates the influence of amount of water to the medical material effective component extraction rate.
Amount of water total solid extraction ratio evaluation table
| Amount of water is the multiple of medical material weight | 3 | 4 | 5 | 6 | 7 | 8 |
| Extraction ratio | 67％ | 79％ | 83％ | 85％ | 84％ | 85％ |
The result shows that extraction ratio increases with the increasing of amount of water, but to a certain degree not bigger variation of back, so the selection amount of water is 4-6 times of medical material weight, preferred addition is 5 times of amounts, comparatively economical rationality.
Experimental example 2, inorganic ceramic film separation purifying technique
The film that pore size is different can be removed float, colloid and macromole impurity (as protein, tannin etc.) in the extracting solution respectively, and the inorganic salts composition, keeps effective ingredient simultaneously, to obtain highly purified clear and bright medicinal liquid as far as possible.Advantage in view of the ceramic membrane filter technology, at first choose inorganic ceramic film the medicinal liquid after extracting is carried out microfiltration, to before filtering and filtered liquid medicine done contrast at aspects such as clarity, precipitation, color and luster, changes of contents, and the technological parameter of inorganic membrane filtration is investigated.
2.1 test method
Equipment: 2#, 3#, 4# ceramic membrane, operating parameter is: (P:0.35～0.4MP; T:35～42 ℃; V:12～16t/h), flux range is 60～100L.M-2.H-1.With the medicinal liquid after extracting cross 2#, 3# respectively, the 4# film carries out microfiltration, investigates the stability of film pipe flux, data see the following form.
Film pipe flux stability is investigated
2.2 the average flux of result of the test: 2#, 3#, 4# is 74L.M-2.H-1, because the flux of 4# film is unusual, so get rid of the interference of 4# film, the average flux of 2#, 3# film is 93L.M-2.H-1.But the flux that can estimate inoranic membrane in view of the above is 70～90L.M-2.H-1.
In experiment, find to use the inorganic ceramic membrane filtration, effective ingredient distributed density basically identical in permeate and the mother solution, mother solution is the dense medicinal liquid that does not see through remaining in the equipment, and can add pure water aborning and wash out effective ingredient, and the reuse nanofiltration concentrates can improve recovery rate.And the amount that at every turn adds entry is more little, and eluting rate is high more, and amount of water is that 2～3 times of eluting resultant effects are best, and loss of effective components generally is no more than 5%.This is considered as 0 with concentration difference before and after the membrane filtration, sets up mathematical model, make to add the water elution simulation drawing by quadrature conversion.
Experimental result shows: obviously improve with the medicinal liquid clarity behind the inorganic membrane filtration, more clear and bright and color and luster obviously shoals, and sterilization is placed and can be produced small amount of precipitate.With gel chromatography check feedback result be: just filter molecular weight through inoranic membrane and can not detect greater than 10000 macromolecular substances.When microfiltration, can add a spot of water washing effective ingredient several times,, extracting solution suitably can be concentrated with vacuum decompression in addition, can reduce filtration yield during microfiltration again, to save time, to raise the efficiency for improving the production efficiency of back workshop section.
Experimental example 3, resin purification technology
In experiment, inventor's original adoption inorganic ceramic film carries out purification refine with the ultrafiltration of rolling organic membrane, the spissated method of rolling NF membrane after handling, 8 parts in sample, and the result shows as has only a clarity to meet the requirements, and occurs precipitation after 1 month but place.Other several parts all precipitation just occurs at couple of days, still have precipitation to produce again after the ultrafiltration.Therefore, the inventor considers that the purified method of membrane separation technique binding resin reaches the effect of purifies and separates medicinal liquid.Concrete technical study is:
3.1 the selection of resin kind
Resin: D101, D201, AB-8 macroporous adsorbent resin, LSA-14 resin, ADS series plastics, polyamide, active carbon etc.With content, color and luster, clarity is that index is investigated relevant technological parameter: flow velocity, eluant strength, elution flow rate etc., and data and selection process conditions such as following table:
The resin kind is selected analytical table
| The resin title | Clarity behind the filtration sterilization | Color and luster before and after filtering | Contain heavily (in total glycosides) before crossing post | Cross content (in total glycosides) behind the post | Eluent content |
| D201 | - | Obviously shoal | 450 | Do not survey | Zhao |
| D101 | - | Obviously shoal | 450 | Do not survey | Zhao |
| AB-8 | - | Obviously shoal | 450 | Do not survey | Zhao |
| LSA-21 | - | Shoal | 450 | Do not survey | Zhao |
| Polyamide | + | Shoal | 450 | 300 | 140～180 |
| Activated carbon | - | Shoal | 450 | Do not survey | Zhao |
As seen from the above table, the medicinal liquid clarity of selecting polyamide to handle is best, after sterilization abortion give birth to muddy, so only measured polyamide handle the back medicinal liquid the content of content and eluent behind the post.And the medicinal liquid handled of polyamide can be respectively checked from wherein qualitative and measure ginsenoside Rg1, Rb1, Re quantitatively with thin layer check and high performance liquid chromatogram.
3.2 the selection of eluent research
The kind of eluent and concentration are the key factors that influences resin purification technology, 2 parts of the medicinal liquid of this test and Selection behind the ceramic membrane microfiltration, direct upper prop, earlier be eluted to colourless with 2 times of column volume deionized waters, use 2 times of column volume 0.5%NaOH solution and 50% ethanol elution then respectively, the result shows that the total saponin content that adopts the collection of NaOH solution is than ethanol liquid height, so the NaOH solution concentration is further studied.
Variable concentrations alkali cleaning synopsis
| Concentration | 0.05％ | 0.1％ | 0.2％ | 0.5％ | 1％ |
| Clarity | +++ | +++ | ++ | + | - |
| Color and luster | ++ | ++ | ++ | ++ | +++ |
According to above result, determine that resin purification technology is: the direct upper prop of medicinal liquid, 0.5-2ml crosses post with per second, with 1-5 times of column volume deionized water eluting, collect medicinal liquid, with 1-5 times of column volume 0.05-0.2%NaOH eluant solution, collect eluent and transfer PH to 4-6, standby.Selection process is: the direct upper prop of medicinal liquid, 1ml crosses post with per second, with 2 times of column volume deionized water eluting, collects medicinal liquid, with 2 times of column volume 0.1%NaOH eluant solutions, collects eluent and transfers PH to 5, and is standby.
Experimental example 4, organic membrane separation purifying technique
Organic membrane is handled and is divided into membrance concentration and two operating procedures of membrane ultrafiltration:
4.1 the membrance concentration condition is P:0.5～1MPa; T:30～40 ℃, V: 〉=2250L/h.Find that in experimentation the membrance concentration effective ingredient has loss, total glycosides content is at 13～19mg/L in the permeate water.
4.2 organic membrane ultrafiltration: ultrafilter membrane used in the experiment is the rolling ultrafilter membrane, is provided by Nanjing University of Technology, and molecular cut off is 10000.Operating condition is P:0.5～0.9MPa; T:30～40 ℃; V: 〉=2250L/h.Ultra-filtration process can add suitable quantity of water washing active ingredient, and its principle and eluting situation are similar to inoranic membrane, and ultrafiltration is held back effective ingredient, and loss rate is at 15%～20%.
Analyze: for reducing loss of effective components, should reduce ultrafiltration and nanofiltration number of times, and pressure should be the smaller the better when ultrafiltration and nanofiltration as far as possible, reclaiming ethanol and should make economic worth relatively when concentrated, the decompression heating recovery is better.
Experimental example 5, quality comparative study
5.1 check situation and yield
According to preparation method of the present invention, with Radix Ginseng 3kg, Radix Astragali 6kg, Radix Et Caulis Acanthopanacis Senticosi 9kg feed intake the experiment ten batches, in experiment, semi-finished product and finished product are carried out qualitative identification and quantitative identification respectively.
The qualitative identification item is: astragaloside, ginsenoside Rg1, Rb1, Re.In semi-finished product and finished product, all can detect.
The quantitative identification item is: ginsenoside Rg1, Rb1, Re.All can detect in semi-finished product and finished product, when semi-finished product total glycosides content was 330～400mg/L, Rg1, Rb1, RE three's summation were at 140～180mg/L.Total glycosides content is 310mg/L in the lab scale sample, and Rg1, Rb1, Re three's summation are 100.62mg/L.
The recovery rate situation: according to final test results, total saponins props up calculating with 3.0mg/, and average yield is 90%.
5.2 quality comparative study
The inventor has done comprehensive comparative study at the improvement of technology to the drug quality before and after improving.
5.2.1 test drug: same a collection of medical material Radix Ginseng 50g, Radix Astragali 100g, Radix Et Caulis Acanthopanacis Senticosi 150g, Mylabris 1.5g with commercially available, make medicine No. 1 according to the preparation method of commercially available ad pro injection; Make medicine No. 2, No. 3, No. 4, No. 5 by the preparation method of infusion preparation of the present invention, hydro-acupuncture preparation, powder injection formulation, freeze-dried powder again.
5.2.2 content of the test: finished product appearance character, pH value, undue toxicity, haemolysis and cohesion, content etc. are relatively investigated.
5.2.3 method and result: product of the present invention and commercially available prod are respectively got 2 parts, These parameters is detected according to existing quality standard.The result is as follows:
Technology of the present invention and commercially available prod technology comparative result
Annotate: " the data % " in last two row of form refers to contain in every 100mg solid preparation the mg number of ginsenoside Re or cantharidin, and " % " promptly is equivalent to " mg/100mg ".
By above data as can be known, infusion preparation of the present invention, hydro-acupuncture preparation, powder injection formulation, freeze-dried powder are all having greatly improved aspect finished product outward appearance and the content, other indexs all meet the requirement of quality standard simultaneously, illustrate that preparation were established of the present invention is reasonable in design, process conditions meet the plant produced requirement, and end product quality is controlled.
Experimental example 6, pharmacodynamic experiment
6.1 experiment material:
Medicine: commercially available ad pro injection, positive contrast medicine; Injection by preparation method of the present invention is made is medicine of the present invention.
Animal: Kunming mouse, body weight 18-22g.
6.2 experimental technique and result
6.2.1 to mice transplanted tumor S
180Influence:
Get the well-grown S in back that goes down to posterity
180Mice, aseptic condition extract ascites down, and by dilution in 1: 3, microscopically was counted with physiological saline solution, and transferring the oncocyte number is 1.0 * 10
7Individual/ml (putting in the ice bath); Get normal mouse then,, weigh after 24 hours in every mice armpit subcutaneous vaccination 0.2ml.Treating excess syndrome is tested medicine, and drug administration by injection dosage is 3.0g/kg, and every day, mouse tail vein was administered once, matched group tail intravenously administrable 0.2ml normal saline, and successive administration ten days, after the last administration 24 hours, get mice and put to death the dissection tumor according to a conventional method, weigh.The results are shown in following table.
To mice transplanted tumor S
180The growth inhibited effect
| Group | Tumor heavy (g) | Suppression ratio (%) |
| Matched group | 1.87 | - |
| Commercially available ad pro injection group | 1.33 | 28.9** |
| Injection group of the present invention | 1.18 | 36.9**# |
Annotate: compare with matched group: * * P＜0.01; With commercially available group relatively: #P＜0.05.
6.2.2 to transplanted hepatoma H
22Influence:
Get the well-grown H in back that goes down to posterity
22Mice, aseptic condition extract ascites down, add 4 times of amount normal saline mixings, every mouse peritoneal inoculation 0.2ml, random packet after 24 hours, female, hero half and half.The same 6.2.1 of dosage.Every day the tail intravenously administrable once, continuous ten days.Put to death mice in 24 hours after the last administration, dissect tumor, weigh.The results are shown in following table.
To transplanted hepatoma H
22Influence
| Group | Tumor heavy (g) | Suppression ratio (%) |
| Matched group | 2.56 | - |
| Commercially available ad pro injection group | 1.67 | 34.8** |
| Injection group of the present invention | 1.34 | 47.6**# |
Annotate: compare with matched group: * * P＜0.01; With commercially available group relatively: #P＜0.05.
According to above experimental result, ejection preparation of the present invention and existing ejection preparation relatively can obviously improve the inhibition effect to tumor, and the better efficacy of ejection preparation of the present invention is described, bioavailability is higher.
Compared with prior art, the present invention with medical material carry out alcohol respectively, moisture is carried, and adopt that membrane separation technique binding resin refinement treatment technology such as inorganic ceramic membrane microfiltration, organic membrane ultrafiltration replace stone sulfur methods, precipitate with ethanol, technology such as saltout, substitute traditional chemical method with physical method, improved the production technology of ad pro injection, can effectively remove the macromolecular substances in the Chinese medicine extraction liquid, do not introduce simultaneously other inorganic ions, fully enrichment effective ingredient, effectively reduce the untoward reaction of medicine, improve curative effect, thereby improved and guaranteed the quality of product; And the present invention has reduced processing step, has shortened flow process, and production cycle of ad pro injection was foreshortened to 5 ~ 7 days from 180 hours, can obtain good cost benefit.
The specific embodiment:
Embodiments of the invention 1: get Mylabris 1.5g, Radix Ginseng 50g, Radix Astragali 100g and Radix Et Caulis Acanthopanacis Senticosi 150g, according to the following steps preparation:
(1) Radix Ginseng section, with 65% soak with ethanol 12 hours, reflux, extract, was 3 times then, and add 8 times of amounts of ethanol at every turn, extracted 1 hour, merge extractive liquid,, recovery ethanol must the Radix Ginseng extractive solution; Medicinal residues and Milkvetch Root add 5 times of water gagings and extract 3 times, and each 1 hour, merge extractive liquid, mixed with the Radix Ginseng extractive solution promptly to get and joins extracting solution at the beginning of the stilbene; First extracting solution is concentrated, filter with inorganic ceramic film then, add the water washing effective ingredient of 2-3 times of medicine liquid volume amount during filtration several times, filtered liquid medicine directly goes up polyamide column, and 1ml crosses post with per second, with 2 times of column volume deionized water eluting, collect medicinal liquid,, collect eluent and transfer pH to 5 with 2 times of column volume 0.1%NaOH eluant solutions, promptly get and join the stilbene extract, standby.
(2) Radix Et Caulis Acanthopanacis Senticosi is pulverized, and the alcohol reflux with 70% 3 times adds 8 times of amounts of ethanol at every turn, extracted 1 hour, and merge extractive liquid, reclaims ethanol, promptly gets Radix Et Caulis Acanthopanacis Senticosi extracting solution just; First extracting solution is concentrated, filter with inorganic ceramic film then, add the water washing effective ingredient of 23 times of medicine liquid volume amounts during filtration several times, filtered liquid medicine directly goes up polyamide column, and 1ml crosses post with per second, with 2 times of column volume deionized water eluting, collect medicinal liquid,, collect eluent and transfer PH to 5 with 2 times of column volume 0.1%NaOH eluant solutions, promptly get Radix Et Caulis Acanthopanacis Senticosi extract, standby.
(3) Mylabris is pulverized, and crosses 40 mesh sieves, decocts with water 3 times, adds 8 times of amounts of water at every turn, extracts 1 hour, merges decoction liquor, filters, and is standby.
(4) will join stilbene extract and Radix Et Caulis Acanthopanacis Senticosi extract and carry out ultrafiltration with the rolling organic membrane, and mix with the Mylabris extracting solution then, and with the water for injection dissolving, add mannitol or lactose or sorbitol, and regulate pH to 4.5-6.0, lyophilization promptly gets freeze-dried powder.
Embodiments of the invention 2: get Mylabris 2.1g, Radix Ginseng 70g, Radix Astragali 140g and Radix Et Caulis Acanthopanacis Senticosi 210g, according to the following steps preparation:
(1) Radix Ginseng section, with 70% soak with ethanol 13 hours, reflux, extract, was 3 times then, and add 9 times of amounts of ethanol at every turn, extracted 1.5 hours, merge extractive liquid,, recovery ethanol, must the Radix Ginseng extractive solution standby; Medicinal residues and Milkvetch Root add 5 times of water gagings and extract 3 times, and each 1.5 hours, merge extractive liquid, mixed with the Radix Ginseng extractive solution promptly to get and joins extracting solution at the beginning of the stilbene; First extracting solution is concentrated, filter with inorganic ceramic film then, add the water washing effective ingredient of 23 times of medicine liquid volume amounts during filtration several times, filtered liquid medicine directly goes up polyamide column, and 1.5ml crosses post with per second, with 3 times of column volume deionized water eluting, collect medicinal liquid,, collect eluent and transfer PH to 5 with 3 times of column volume 0.15%NaOH eluant solutions, promptly get and join the stilbene extract, standby.
(2) Radix Et Caulis Acanthopanacis Senticosi is pulverized, and with 75% alcohol reflux 3 times, add 9 times of amounts of ethanol at every turn, extracted 1.5 hours, merge extractive liquid,, recovery ethanol promptly gets extracting solution at the beginning of the Radix Et Caulis Acanthopanacis Senticosi; First extracting solution is concentrated, filter with inorganic ceramic film then, add the water washing effective ingredient of 23 times of medicine liquid volume amounts during filtration several times, filtered liquid medicine directly goes up polyamide column, and 1.5ml crosses post with per second, with 3 times of column volume deionized water eluting, collect medicinal liquid,, collect eluent and transfer PH to 5 with 3 times of column volume 0.15%NaOH eluant solutions, promptly get Radix Et Caulis Acanthopanacis Senticosi extract, standby.
(3) Mylabris is pulverized, and crosses 50 mesh sieves, decocts with water 3 times, adds 9 times of amounts of water at every turn, extracts 1.5 hours, merges decoction liquor, filters, and is standby.
(4) will join stilbene extract and Radix Et Caulis Acanthopanacis Senticosi extract and carry out ultrafiltration with the rolling organic membrane, and mix with the Mylabris extracting solution then, and with the water for injection dissolving, add mannitol or lactose or sorbitol, and regulate pH to 4.5-6.0, drying promptly gets powder injection formulation.
Embodiments of the invention 3: get Mylabris 0.9g, Radix Ginseng 70g, Radix Astragali 60g and Radix Et Caulis Acanthopanacis Senticosi 210g, according to the following steps preparation:
(1) Radix Ginseng section, with 75% soak with ethanol 10 hours, reflux, extract, was 4 times then, and add 6 times of amounts of ethanol at every turn, extracted 2 hours, merge extractive liquid,, recovery ethanol, must the Radix Ginseng extractive solution standby; Medicinal residues and Milkvetch Root add 4 times of water gagings and extract 4 times, and each 0.5 hour, merge extractive liquid, mixed with the Radix Ginseng extractive solution promptly to get and joins extracting solution at the beginning of the stilbene; First extracting solution is concentrated, and inorganic ceramic film filters, and filtered liquid medicine directly goes up polyamide column, and 2ml crosses post with per second, with 1 times of column volume deionized water eluting, collect medicinal liquid, with 5 times of column volume 0.05%NaOH eluant solutions, collect eluent and transfer PH to 6, promptly get and join the stilbene extract, standby.
(2) Radix Et Caulis Acanthopanacis Senticosi is pulverized, and with 80% alcohol reflux 2 times, add 10 times of amounts of ethanol at every turn, extracted 0.5 hour, merge extractive liquid,, recovery ethanol promptly gets extracting solution at the beginning of the Radix Et Caulis Acanthopanacis Senticosi; First extracting solution is concentrated, and inorganic ceramic film filters, and filtered liquid medicine directly goes up polyamide column, and 2ml crosses post with per second, with 1 times of column volume deionized water eluting, collect medicinal liquid, with 5 times of column volume 0.05%NaOH eluant solutions, collect eluent and transfer PH to 6, promptly get Radix Et Caulis Acanthopanacis Senticosi extract, standby.
(3) Mylabris is pulverized, and crosses 60 mesh sieves, decocts with water 2 times, adds 10 times of amounts of water at every turn, extracts 0.5 hour, merges decoction liquor, filters, and is standby.
(4) will join stilbene extract and Radix Et Caulis Acanthopanacis Senticosi extract and carry out ultrafiltration, mix with the Mylabris extracting solution then,, regulate pH to 4.5-6.0 with the water for injection dissolving with organic membrane, embedding, sterilization promptly gets hydro-acupuncture preparation.
Embodiments of the invention 4: get Mylabris 2.1g, Radix Ginseng 30g, Radix Astragali 140g and Radix Et Caulis Acanthopanacis Senticosi 90g, according to the following steps preparation:
(1) Radix Ginseng section, with 55% soak with ethanol 14 hours, reflux, extract, was 2 times then, and add 10 times of amounts of ethanol at every turn, extracted 0.5 hour, merge extractive liquid,, recovery ethanol, must the Radix Ginseng extractive solution standby; Medicinal residues and Milkvetch Root add 6 times of water gagings and extract 2 times, and each 2 hours, merge extractive liquid, mixed with the Radix Ginseng extractive solution promptly to get and joins extracting solution at the beginning of the stilbene; First extracting solution is concentrated, and inorganic ceramic film filters, and filtered liquid medicine directly goes up polyamide column, and 0.5ml crosses post with per second, with 5 times of column volume deionized water eluting, collect medicinal liquid, with 1 times of column volume 0.2%NaOH eluant solution, collect eluent and transfer PH to 4, promptly get and join the stilbene extract, standby.
(2) Radix Et Caulis Acanthopanacis Senticosi is pulverized, and with 60% alcohol reflux 4 times, add 6 times of amounts of ethanol at every turn, extracted 2 hours, merge extractive liquid,, recovery ethanol promptly gets extracting solution at the beginning of the Radix Et Caulis Acanthopanacis Senticosi; First extracting solution is concentrated, inorganic ceramic film filters, filtered liquid medicine directly goes up polyamide column, 0.5ml crosses post with per second, with 5 times of column volume deionized water eluting, collects medicinal liquid, with 1 times of column volume 0.2%NaOH eluant solution, collect eluent and transfer PH to 4, promptly get Radix Et Caulis Acanthopanacis Senticosi extract, standby.
(3) Mylabris is pulverized, and crosses 40 mesh sieves, decocts with water 4 times, adds 6 times of amounts of water at every turn, extracts 2 hours, merges decoction liquor, filters, and is standby.
(4) will join stilbene extract and Radix Et Caulis Acanthopanacis Senticosi extract and carry out ultrafiltration, mix with the Mylabris extracting solution then, dissolve with water for injection with organic membrane, adding sodium chloride, calcium chloride, glucose or dextran adjusting etc. oozes, regulate pH to 4.5-6.0, sterilization promptly gets infusion preparation.
Embodiments of the invention 5: get Mylabris 0.9g, Radix Ginseng 30g, Radix Astragali 60g and Radix Et Caulis Acanthopanacis Senticosi 90g, according to the following steps preparation:
(1) Radix Ginseng section with 60% alcohol reflux 3 times, adds 7 times of amounts of ethanol at every turn, extracted 1.5 hours, merge extractive liquid,, and recovery ethanol, must the Radix Ginseng extractive solution standby; Medicinal residues and Milkvetch Root add 5 times of water gagings and extract 3 times, and each 1.5 hours, merge extractive liquid, mixed promptly to get with the Radix Ginseng extractive solution and joins the stilbene extracting solution, concentrate, and inorganic membrane filtration, polyamide column is made with extra care, and is standby
(2) Radix Et Caulis Acanthopanacis Senticosi is pulverized, and with 65% alcohol reflux 3 times, adds 7 times of amounts of ethanol at every turn, extracts 1.5 hours, and merge extractive liquid, reclaims ethanol, and is concentrated, inorganic membrane filtration, and polyamide column is made with extra care, and is standby.
(3) Mylabris is pulverized, and crosses 50 mesh sieves, decocts with water 3 times, adds 7 times of amounts of water at every turn, extracts 1.5 hours, merges decoction liquor, filters, and is standby.
(4) extracting solution with Radix Ginseng, the Radix Astragali and Radix Et Caulis Acanthopanacis Senticosi carries out ultrafiltration with organic membrane, mixes with the Mylabris extracting solution then, with the water for injection dissolving, adds mannitol or lactose or sorbitol, regulates pH to 4.5-6.0, and drying promptly gets powder injection formulation.
Claims (10)
1. traditional medicine Injectio for the treatment of cancer, it is characterized in that: according to listed as parts by weight, it is made as follows with Mylabris 0.9-2.1 part, Radix Ginseng 30-70 part, Radix Astragali 60-140 part and Radix Et Caulis Acanthopanacis Senticosi 90-210 part: get the Radix Ginseng section, use alcohol reflux, extracting solution reclaims ethanol, and it is standby to get the Radix Ginseng extractive solution; Medicinal residues and Milkvetch Root be water extraction altogether, and extracting solution mixes with the Radix Ginseng extractive solution promptly to get joins the stilbene extracting solution, concentrates, and filters, and be refining, standby; Radix Et Caulis Acanthopanacis Senticosi is pulverized, and uses alcohol reflux, and extracting solution reclaims ethanol, concentrates, and filters, and is refining, standby; Mylabris is pulverized, and decocts with water, and decoction liquor filters, and is standby; The extracting solution of Radix Ginseng, the Radix Astragali and Radix Et Caulis Acanthopanacis Senticosi is carried out ultrafiltration, mix with the Mylabris extracting solution then, add adjuvant or do not add adjuvant, make different ejection preparations with diverse ways.
2. according to the traditional medicine Injectio of the described treatment cancer of claim 1, it is characterized in that: according to listed as parts by weight, it is made for 150 parts with 1.5 parts of Mylabris, 50 parts of Radix Ginsengs, 100 parts of the Radixs Astragali and Radix Et Caulis Acanthopanacis Senticosi.
3. according to the traditional medicine Injectio of claim 1 or 2 described treatment cancers, it is characterized in that: described ejection preparation is hydro-acupuncture preparation, infusion preparation, powder injection formulation or freeze-dried powder.
4. as the preparation method of the traditional medicine Injectio of treatment cancer as described in each among the claim 1-3, it is characterized in that: get the Radix Ginseng section, with 55%-75% alcohol reflux 2-4 time, merge extractive liquid, reclaims ethanol, and is must the Radix Ginseng extractive solution standby; Medicinal residues and Milkvetch Root are total to water extraction 2-4 time, and extracting solution mixes with the Radix Ginseng extractive solution promptly to get joins the stilbene extracting solution, concentrate, and inorganic membrane filtration, resin purification, standby; Radix Et Caulis Acanthopanacis Senticosi is pulverized, the alcohol reflux of usefulness 60%-80% 2-4 time, and merge extractive liquid, reclaims ethanol, concentrates, inorganic membrane filtration, resin purification, standby; Mylabris is pulverized, and crosses the 40-60 mesh sieve, decocts with water 2-4 time, merges decoction liquor, filters, and is standby; The extracting solution of Radix Ginseng, the Radix Astragali and Radix Et Caulis Acanthopanacis Senticosi is carried out ultrafiltration with organic membrane, mix with the Mylabris extracting solution then, add adjuvant or do not add adjuvant, make different ejection preparations with diverse ways.
5. according to the preparation method of the traditional medicine Injectio of the described treatment cancer of claim 4, it is characterized in that: get the Radix Ginseng section, with 55%-75% soak with ethanol 10-14 hour, reflux, extract, is 2-4 time then, each ethanol 6-10 that adds doubly measured, extracts 0.5-2 hour, merge extractive liquid, reclaims ethanol, and it is standby to get the Radix Ginseng extractive solution; Medicinal residues and Milkvetch Root add 4-6 times of water gaging and extract 2-4 time, and each 0.5-2 hour, merge extractive liquid, mixed with the Radix Ginseng extractive solution promptly to get and joins extracting solution at the beginning of the stilbene; First extracting solution is concentrated, inorganic ceramic film filters, filtered liquid medicine directly goes up polyamide column, 0.5-2ml crosses post with per second, with 1-5 times of column volume deionized water eluting, collect medicinal liquid, with 1-5 times of column volume 0.05-0.2%NaOH eluant solution, collect eluent and transfer PH to 4-6, get promptly that to join the stilbene extract standby; Radix Et Caulis Acanthopanacis Senticosi is pulverized, and uses 60%-80% alcohol reflux 2-4 time, adds ethanol 6-10 at every turn and doubly measures, extracts 0.5-2 hour, and merge extractive liquid, reclaims ethanol, promptly gets Radix Et Caulis Acanthopanacis Senticosi extracting solution just; First extracting solution is concentrated, inorganic ceramic film filters, filtered liquid medicine directly goes up polyamide column, 0.5-2ml crosses post with per second, with 1-5 times of column volume deionized water eluting, collect medicinal liquid, with 1-5 times of column volume 0.05-0.2%NaOH eluant solution, collect eluent and transfer PH to 4-6, it is standby promptly to get Radix Et Caulis Acanthopanacis Senticosi extract; Mylabris is pulverized, and crosses the 40-60 mesh sieve, decocts with water 2-4 time, adds water 6-10 at every turn and doubly measures, extracts 0.5-2 hour, merges decoction liquor, filters, and is standby; To join stilbene extract and Radix Et Caulis Acanthopanacis Senticosi extract and carry out ultrafiltration, mix with the Mylabris extracting solution then, and add adjuvant or do not add adjuvant, make different ejection preparations with diverse ways with organic membrane.
6. according to the preparation method of the traditional medicine Injectio of the described treatment cancer of claim 5, it is characterized in that: get the Radix Ginseng section, with 65% soak with ethanol 12 hours, reflux, extract, is 3 times then, adds 8 times of amounts of ethanol at every turn, extracts merge extractive liquid, 1 hour, reclaim ethanol, get the Radix Ginseng extractive solution; Medicinal residues and Milkvetch Root add 5 times of water gagings and extract 3 times, and each 1 hour, merge extractive liquid, mixed with the Radix Ginseng extractive solution promptly to get and joins extracting solution at the beginning of the stilbene; First extracting solution is concentrated, filter with inorganic ceramic film then, the water washing effective ingredient that adds 2-3 times of medicine liquid volume amount during filtration several times, filtered liquid medicine directly goes up polyamide column, and 1ml crosses post with per second, with 2 times of column volume deionized water eluting, collect medicinal liquid, with 2 times of column volume 0.1%NaOH eluant solutions, collect eluent and transfer pH to 5, get promptly that to join the stilbene extract standby; Radix Et Caulis Acanthopanacis Senticosi is pulverized, and the alcohol reflux with 70% 3 times adds 8 times of amounts of ethanol at every turn, extracted 1 hour, and merge extractive liquid, reclaims ethanol, promptly gets Radix Et Caulis Acanthopanacis Senticosi extracting solution just; First extracting solution is concentrated, filter with inorganic ceramic film then, the water washing effective ingredient that adds 2-3 times of medicine liquid volume amount during filtration several times, filtered liquid medicine directly goes up polyamide column, and 1ml crosses post with per second, with 2 times of column volume deionized water eluting, collect medicinal liquid, with 2 times of column volume 0.1%NaOH eluant solutions, collect eluent and transfer PH to 5, it is standby promptly to get Radix Et Caulis Acanthopanacis Senticosi extract; Mylabris is pulverized, and crosses 40 mesh sieves, decocts with water 3 times, adds 8 times of amounts of water at every turn, extracts 1 hour, merges decoction liquor, filters, and is standby; To join stilbene extract and Radix Et Caulis Acanthopanacis Senticosi extract and carry out ultrafiltration, mix with the Mylabris extracting solution then, and add adjuvant or do not add adjuvant, make different ejection preparations with diverse ways with the rolling organic membrane.
7. according to the preparation method of the traditional medicine Injectio of claim 4,5 or 6 described treatment cancers, it is characterized in that: hydro-acupuncture preparation is preparation like this: the extracting solution of the Radix Ginseng behind the ultra filtration, the Radix Astragali and Radix Et Caulis Acanthopanacis Senticosi is mixed with the Mylabris extracting solution, dissolve with water for injection, regulate pH to 4.5-6.0, embedding, sterilization, promptly.
8. according to the preparation method of the traditional medicine Injectio of claim 4,5 or 6 described treatment cancers, it is characterized in that: infusion preparation is preparation like this: the extracting solution of the Radix Ginseng behind the ultra filtration, the Radix Astragali and Radix Et Caulis Acanthopanacis Senticosi is mixed with the Mylabris extracting solution, dissolve with water for injection, adding sodium chloride, calcium chloride, glucose or dextran adjusting etc. oozes, regulate pH to 4.5-6.0, sterilization, promptly.
9. according to the preparation method of the traditional medicine Injectio of claim 4,5 or 6 described treatment cancers, it is characterized in that: powder injection formulation is preparation like this: the extracting solution of the Radix Ginseng behind the ultra filtration, the Radix Astragali and Radix Et Caulis Acanthopanacis Senticosi is mixed with the Mylabris extracting solution, dissolve with water for injection, add mannitol or lactose or sorbitol, regulate pH to 4.5-6.0, drying, promptly
10. according to the preparation method of the traditional medicine Injectio of claim 4,5 or 6 described treatment cancers, it is characterized in that: freeze-dried powder is preparation like this: the extracting solution of the Radix Ginseng behind the ultra filtration, the Radix Astragali and Radix Et Caulis Acanthopanacis Senticosi is mixed with the Mylabris extracting solution, dissolve with water for injection, add mannitol or lactose or sorbitol, regulate pH to 4.5-6.0, lyophilization, promptly.
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| CN1248699C (en) * | 2004-02-23 | 2006-04-05 | 天津天士力之骄药业有限公司 | Method for preparing Chinese herb medicine freezing-drying power-injection for treating tumor |
| CN1709442A (en) * | 2005-07-06 | 2005-12-21 | 北京阜康仁生物制药科技有限公司 | Anti-cancer Chinese medicine lyophilized injection agent |
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| CN103202886A (en) * | 2013-03-29 | 2013-07-17 | 阚兆云 | Traditional chinese medicine composition and preparation method thereof |
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| CN108309998B (en) * | 2018-01-26 | 2020-11-03 | 北京大学 | Natural product composition and medical application thereof |
| CN115607587A (en) * | 2021-07-16 | 2023-01-17 | 贵州益佰制药股份有限公司 | Application of Aidi preparation in preparing medicine for treating herpes zoster |
| CN115607587B (en) * | 2021-07-16 | 2023-12-01 | 贵州益佰制药股份有限公司 | Application of Aidi preparation in preparation of medicament for treating herpes zoster |
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