CN101559084A - Anti-tumor pharmaceutical composition and preparation method thereof - Google Patents
Anti-tumor pharmaceutical composition and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an anti-tumor pharmaceutical composition and a preparation method thereof, and belongs to the technical field of bio-pharmaceuticals. The pharmaceutical composition comprises the following components: 20 to 60 percent of extract of brown heart rot of cinnamomum kanehirai, 5 to 30 percent of glossy ganoderma extract and 20 to 60 percent of grifola frondosa extract. The preparation method comprises the following steps: preparing the extract of the brown heart rot of the cinnamomum kanehirai; preparing the glossy ganoderma extract; preparing the grifola frondosa extract; and mixing the extract of the brown heart rot of the cinnamomum kanehira, the glossy ganoderma extract and the grifola frondosa extract. The anti-tumor pharmaceutical composition is an immunopotentiator, has no toxic and side effect, and mainly achieves the anti-tumor effect by reinforcing the immunological competence of the human body. The anti-tumor pharmaceutical composition has reasonable compatibility, and all the components are from natural products, so that the anti-tumor pharmaceutical composition is safe and has no toxic and side effect. The tumor inhibition rate of the anti-tumor pharmaceutical composition is 26.16 percent (P is less than 0.05) and is equivalent to that of the prior anti-cancer medicine cyclophosphamide, but the toxicity of the anti-tumor pharmaceutical composition is obviously lower than that of the cyclophosphamide. The preparation method for the anti-tumor pharmaceutical composition has reasonable design, simple and convenient operation and high extraction purity.
Description
Technical field
The invention belongs to biological pharmacy technical field, be specifically related to a kind of antitumor medicine composition and production method thereof.
Background technology
Antrodia Camphorata claims Antrodia camphorata or Antrodia camphorata again, and formal name used at school is Antrodia Camphorata, belongs to load army class guiding principle, Aphyllophorales, Polyporaceae, Polyporus.
Antrodia camphorata is the distinctive fungus in Taiwan, only grows on the distinctive Cinnamomum kanahirai hay tree in Taiwan.Antrodia Camphorata grows in the moist surface of rotten hollow inside of Cinnamomum kanahirai hay trunk or lodging trunk.Wild Antrodia camphorata length is in the Cinnamomum kanahirai hay of old-age group tree, and changeableization of sporophore shape has tabular, bell shape, horse-hof shape or tower shape; The nascent cerise, gradually long white, the light red brown, filbert or khaki of becoming.Antrodia Camphorata gas fragranced is arduous, flat.The circulation of qi promoting of dispeling the wind arranged, change that silt is invigorated blood circulation, warming middle-JIAO disappears knot, the effect of removing toxic substances and promoting subsidence of swelling, sedation-analgesia, antibiotic, antiviral, antitumor, lifting immunity of organisms; For treatment gastrointestinal distress, diarrhea and vomiting, alimentary toxicosis, mushroom poisoning, diabetes, alcoholic liver, fatty liver, liver cirrhosis, hepatocarcinoma etc. unique function is arranged especially.Antrodia Camphorata is that many physiologically active ingredients are arranged, as polysaccharide body, triterpenoid compound, sudismase, adenosine, protein (containing immune protein), vitamin, trace element, nucleic acid, agglutinin, aminoacid, solid liquor-saturated tired, cellulose, blood pressure stabilization material etc.In the effective ingredient of Antrodia Camphorata with triterpenoid compound for the most special, up to more than 200 kinds, be that other mushroom bacterium can't be compared, more than 200 in triterpenoid compound make Antrodia Camphorata have anticancer, effect such as protect the liver.Therefore the medicinal fungi of preciousness because Antrodia camphorata is regarded as uniqueness in Taiwan has high research and commercial value, also is the most expensive wild fungus in present Taiwan, is called as in Hongkong and Macro " Ganoderma ", and Taiwan is among the people to be referred to as " ruby in the forest ".
Grifola frondosa has another name called hen of the woods, and Japan claims dance fine and soft, belongs to Basidiomycetes, the macro fungi that is the subtropical zone to the temperate forests, and its polysaccharide has the good resistance tumor effect.
That Ganoderma just is considered to since ancient times is lucky, rich and honour, fine, the life-prolonging symbol, and the title of " Herba mesonae chinensis ", " Ganoderma " is arranged, and chinese tradition medical science is considered as strengthening by means of tonics for a long time always, consolidates the precious Chinese herbal medicine of setting upright.The folklore Ganoderma have come back to life, effect alive for evermore.Ganoderma is formally recorded by state-promulgated pharmacopoeia as medicine, and it is again the new resource food of state approval simultaneously, has no side effect, can medicine-food two-purpose.
Mainly be radiotherapy, chemotherapy for the treatment for cancer method at present,, can cause serious general toxic reaction no matter be that radiotherapy, chemotherapy all have very big toxic and side effects.As gastrointestinal dysfunction, hepatic and renal function is impaired, alopecia, feel sick, vomiting, xerostomia, anorexia, abdominal distention, diarrhoea, also oral ulcer, intestinal obstruction, constipation, gastrointestinal hemorrhage etc. can appear sometimes.If reaction seriously, can make patient bear and have to stop treatment.As seen, existingly put, traditional remedies such as chemotherapy only pays attention to killing cancer cell, and ignore the anti-cancer ability of body self, ignore the anticancer cell mass NK of body self cell, LAK.Some immunocompetences that strengthen human body selfs are also arranged on the market, but a lot of medicine is there is very big toxic and side effects, its effect neither be clearly.
Summary of the invention
The present invention is directed to the problem that prior art exists, design provides a kind of and has no side effect, and can strengthen the immunocompetence of human body self and the technical scheme of energy antitumor medicine composition and production method thereof.
Described a kind of antitumor medicine composition is characterized in that being made of following by weight percentage:
Antrodia Camphorata extract 20%-60% Ganoderma extract 5%-30% Grifola frondosa extract 20%-60%.
Described a kind of antitumor medicine composition is characterized in that being made of following by weight percentage:
Antrodia Camphorata extract 25%-55% Ganoderma extract 10%-25% Grifola frondosa extract 25%-55%.
Described a kind of antitumor medicine composition is characterized in that being made of following by weight percentage:
Antrodia Camphorata extract 30%-50% Ganoderma extract 15%-20% Grifola frondosa extract 30%-50%.
Described a kind of antitumor medicine composition is characterized in that being made of following by weight percentage:
Antrodia Camphorata extract 35%-45% Ganoderma extract 15%-20% Grifola frondosa extract 35%-45%.
The production method of described a kind of antitumor medicine composition is characterized in that comprising following processing step:
(1) preparation Antrodia Camphorata extract: get the Antrodia Camphorata coarse powder, the ethanol that 2-10 times of concentration of adding Antrodia Camphorata coarse powder weight is 60-80% under temperature 60-80 ℃, extracts after 1-3 hour, filters; Get filtered filtration residue, the ethanol that 1-5 times of concentration of adding filtering residue weight is 60-80% in filtering residue under temperature 60-80 ℃, extracts after 1-3 hour again, filters; Merge filtrate twice, reclaim ethanol, it is standby to obtain extractum; The filtering residue of getting after filter the above-mentioned second time adds filtering residue weight 15-25 water doubly, extracts after 1-3 hour, filters; Get filtered filtration residue, add filtering residue weight 5-15 water doubly in the filtering residue, extract after 1-3 hour, filter; After merging twice filtrate and above-mentioned extractum, carry out thin film evaporation and concentrate, being concentrated into density is 1.0-1.5g/cm
3, carry out spray drying then, collect spray powder, promptly obtain the Antrodia Camphorata extract;
(2) preparation Ganoderma extract: get the Ganoderma coarse powder, the ethanol that 2-10 times of concentration of adding Ganoderma coarse powder weight is 60-80% under temperature 60-80 ℃, extracts after 1-3 hour, filters; Get filtered filtration residue, the ethanol that 1-5 times of concentration of adding filtering residue weight is 60-80% in filtering residue under temperature 60-80 ℃, extracts after 1-3 hour again, filters; Merge filtrate twice, reclaim ethanol, it is standby to obtain extractum; The filtering residue of getting after filter the above-mentioned second time adds filtering residue weight 15-25 water doubly, and regulates PH to 7-9, extracts after 1-3 hour, filters; Get filtered filtration residue, add filtering residue weight 5-15 water doubly in the filtering residue, and regulate PH to 7-9, extract after 1-3 hour, filter; After merging twice filtrate and above-mentioned extractum, carry out thin film evaporation and concentrate, being concentrated into density is 1.0-1.2g/cm
3, carry out spray drying then, collect spray powder, promptly obtain Ganoderma extract;
(3) preparation Grifola frondosa extract: get the Grifola frondosa fine powder, add Grifola frondosa fine powder weight 25-35 water doubly, extract after 2-6 hour, carry out filter pressing; Get filtrate concentrating, being concentrated into relative density is 1.0-1.1g/cm
3In concentrated solution, add 1-3 times of concentration of concentrated solution volume and be 95% ethanol and carry out precipitate with ethanol, stirred 20-40 minute, place after 10-15 hour, filter; Filter rear filtrate and reclaim ethanol, precipitate adds entry, and heating for dissolving stirs simultaneously, regulates density to 1.0-1.05g/cm
3, spray drying is collected spray powder then, promptly obtains the Grifola frondosa extract;
(4) above-mentioned resulting Antrodia Camphorata extract, Ganoderma extract and Grifola frondosa extract are mixed by following percentage by weight:
Antrodia Camphorata extract 20%-60% Ganoderma extract 5%-30% Grifola frondosa extract 20%-60% promptly obtains antineoplastic pharmaceutical compositions.
The production method of described a kind of antitumor medicine composition is characterized in that adding the 4-8 times of ethanol that concentration is 65-75% in the step (1) in the Antrodia Camphorata coarse powder, under temperature 65-75 ℃, extracts 2-3 hour; Get filtered filtration residue, in filtering residue, add the 2-4 times of ethanol that concentration is 65-75% again, under temperature 65-75 ℃, extract after 2-3 hour; Merge filtrate twice, reflux condensation mode reclaims ethanol, until there not being the alcohol flavor, obtains extractum; Add 17-23 water doubly in the filtering residue after filtering for the second time, extracted 1.5-2.5 hour; Get filtered filtration residue, add 8-12 water doubly in the filtering residue, extracted 1.5-2.5 hour; Evaporation and concentration to density is 1.02-1.03g/cm
3, spray drying adopts 220-240 ℃ of inlet temperature, leaving air temp 80-100 ℃.
The production method of described a kind of antitumor medicine composition is characterized in that getting the Ganoderma coarse powder in the step (2), adds the 4-8 times of ethanol that concentration is 65-75%, under temperature 65-75 ℃, extracts 2-3 hour; Get filtered filtration residue, in filtering residue, add the 2-4 times of ethanol that concentration is 65%-75% again, under temperature 65-75 ℃, extract after 2-3 hour; Merge filtrate twice, reflux condensation mode reclaims ethanol, until there not being the alcohol flavor, obtains extractum; 17-23 water is doubly regulated PH to 7.5-8 with the food grade sodium hydroxide in the filtering residue after filtering for the second time, extracts 1.5-2.5 hour; Get filtered filtration residue, add 8-12 water doubly in the filtering residue, regulate PH to 7.5-8, extracted 1.5-2.5 hour with the food grade sodium hydroxide; Evaporation and concentration to density is 1.02-1.03g/cm
3, spray drying adopts 220-240 ℃ of inlet temperature, leaving air temp 80-100 ℃.
The production method of described a kind of antitumor medicine composition is characterized in that adding in the step (3) Grifola frondosa fine powder weight 27-33 water doubly, extracts 3-5 hour; Filtrate is carried out evaporation and concentration, and being concentrated into relative density is 1.07-1.09g/cm
3Add 1.5-2.5 times of concentration of concentrated solution volume in the concentrated solution and be 95% ethanol and carry out precipitate with ethanol, stirred 25-35 minute, placed 11-14 hour; Filter the rear filtrate reflux condensation mode and reclaim ethanol, precipitate adds entry, is 1.0-1.04g/cm until density
3, spray drying adopts 220-230 ℃ of inlet temperature, leaving air temp 80-90 ℃.
The production method of described a kind of antitumor medicine composition is characterized in that Antrodia Camphorata extract, Ganoderma extract and Grifola frondosa extract mix by following percentage by weight in the step (4):
Antrodia Camphorata extract 25%-55% Ganoderma extract 10%-25% Grifola frondosa extract 25%-55%.
The production method of described a kind of antitumor medicine composition is characterized in that Antrodia Camphorata extract, Ganoderma extract and Grifola frondosa extract mix by following percentage by weight in the step (4):
Antrodia Camphorata extract 30%-50% Ganoderma extract 15%-20% Grifola frondosa extract 30%-50.
A kind of antitumor medicine composition of the present invention is a kind of immunostimulant, have no side effect, thereby it mainly reaches the antineoplastic effect by the immunocompetence that strengthens human body self.The prescription compatibility that the present invention adopts is reasonable, and component all is from natural product, safe without toxic side effect.Its tumor control rate is 26.16% (P＜0.05), and suppression ratio is suitable with existing cancer therapy drug cyclophosphamide, but toxicity is starkly lower than cyclophosphamide.
The production method of a kind of antitumor medicine composition of the present invention, reasonable in design, simple to operation, the dna purity height.
The specific embodiment
Further specify the present invention with experimental example by the following examples.The Antrodia Camphorata that relates in the invention is bought by Taiwan, and Ganoderma, Grifola frondosa are produced by the Zhejiang Prov Fangge Pharmaceutical Co., Ltd base.
Embodiment 1:
(1) preparation Antrodia Camphorata extract: get the Antrodia Camphorata coarse powder, 6 times of concentration of adding Antrodia Camphorata coarse powder weight are 75% ethanol, under 75 ℃ of temperature, extract after 2 hours, filter; Get filtered filtration residue, in filtering residue, add 4 times of concentration of filtering residue weight again and be 75% ethanol, under 75 ℃ of temperature, extract after 1.5 hours, filter; Merge filtrate twice, reclaim ethanol,, obtain extractum until there not being the alcohol flavor with alcohol reflux tower reflux condensation mode; Get the water that filtering residue after above-mentioned second time filters adds 22 times of filtering residue weight, extract after 2 hours, filter; Get filtered filtration residue, add the water of 10 times of filtering residue weight in the filtering residue, extract after 1.5 hours, filter; After merging twice filtrate and above-mentioned extractum, carry out evaporation and concentration, being concentrated into density is 1.02g/cm
3, carry out spray drying then, 230 ℃ of spray drying inlet temperature, 90 ℃ of leaving air temps are collected spray powder, promptly obtain the Antrodia Camphorata extract;
(2) preparation Ganoderma extract: get the Ganoderma coarse powder, 6 times of concentration of adding Ganoderma coarse powder weight are 75% ethanol, under 75 ℃ of temperature, extract after 2 hours, filter; Get filtered filtration residue, in filtering residue, add 4 times of concentration of filtering residue weight again and be 75% ethanol, under 75 ℃ of temperature, extract after 1.5 hours, filter; Merge filtrate twice, reclaim ethanol,, obtain extractum until there not being the alcohol flavor with alcohol reflux tower reflux condensation mode; The filtering residue of getting after filter the above-mentioned second time adds the water of 22 times of filtering residue weight, and with food grade sodium hydroxide adjusting PH to 7.5, extracts after 2 hours, filters; Get filtered filtration residue, add the water of 10 times of filtering residue weight in the filtering residue, and regulate PH to 7.5, extract after 1.5 hours, filter with the food grade sodium hydroxide; After merging twice filtrate and above-mentioned extractum, carry out evaporation and concentration, being concentrated into density is 1.02g/cm
3, carry out spray drying then, 230 ℃ of spray drying inlet temperature, leaving air temp is collected spray powder for 90 ℃, promptly obtains Ganoderma extract;
(3) preparation Grifola frondosa extract: get the Grifola frondosa fine powder, add the water of 30 times of Grifola frondosa fine powder weight, extract after 4 hours, carry out filter pressing; Get filtrate concentrating, being concentrated into relative density is 1.08g/cm
3In concentrated solution, add 1.5 times of concentration of concentrated solution volume and be 95% ethanol and carry out precipitate with ethanol, stirred 30 minutes, place after 12 hours, filter; Filter rear filtrate and reclaim ethanol, precipitate adds entry, heats, stir simultaneously, and be 1.02g/cm until density
3, carry out spray drying then, 225 ℃ of spray drying inlet temperature, 85 ℃ of leaving air temps are collected spray powder, promptly obtain the Grifola frondosa extract;
(4) above-mentioned resulting Antrodia Camphorata extract, Ganoderma extract and Grifola frondosa extract are mixed by following percentage by weight: Antrodia Camphorata extract 40%, Ganoderma extract 20%, Grifola frondosa extract 40%.
Experimental example:
1. drug evaluation index: tumor control rate (%).
Observing time: 14 days.
2. experiment key step:
2.1 tumor strain and entity tumor implantation method: the strain of rat liver cancer (H22) tumor is preserved by central laboratory of Tumour Inst., Chinese Medical Academy is conventional.Tumor cell takes out in liquid nitrogen, after 37 ℃ of recoveries of thawing rapidly, is inoculated in the mouse peritoneal, and visible mouse web portion swells after 8 days, and tumor is recovered successfully.
2.2 tumor inoculation and grouping: put to death tumor-bearing mice and extract ascites cells under aseptic condition, dilution, counting, every Mus inoculate 0.2 ml cells suspension.Be divided into 6 groups at random, 10 every group.Be normal saline group, cyclophosphamide injection group, 1 group of Antrodia Camphorata, 2 groups of Antrodia Camphorata, 3 groups of Antrodia Camphorata, 4 groups of Antrodia Camphorata.(wherein Antrodia Camphorata is Antrodia Camphorata extract 40%, Grifola frondosa extract 60% mixture for 1 group, Antrodia Camphorata is Antrodia Camphorata extract 60%, Grifola frondosa extract 40% mixture for 2 groups, Antrodia Camphorata is an Antrodia Camphorata extract 100% for 3 groups, and Antrodia Camphorata is Antrodia Camphorata extract 40%, Ganoderma extract 20%, Grifola frondosa extract 40% mixture for embodiment 1 compositions for 4 groups)
2.3 tried the agent amount: the clinical human dosage of Antrodia Camphorata is 6 gram/skies (4 * of 0.5 gram/grain * 3 times/day), and people's standard body weight is pressed 70kg usually and calculated, and promptly people's dosage is 85.71mg/kg.
Convert (being people and mice) according to dose,equivalent between Drug And Statistics Ver 1.0 pharmacy software animals, the mice standard body weight is 0.02Kg, and conversion is the result get: individual used dosage 15.3557mg/, and 767.7848mg/Kg.
Put to death animal on the 14th day, the back of weighing is complete peels off tumor and claims tumor heavy.Calculate tumor control rate %, DAS.ver1.0 pharmacology software is done statistical procedures.
3. experimental result:
3.1 animals administer afterreaction: general states such as mice activity, feed are good during the oral drugs.
3.2 positive control cyclophosphamide and tried 1 to 4 group of thing and normal saline group relatively:
Cyclophosphamide and normal saline group comparison of tumor suppression ratio are 46.2% (P＜0.001).Antrodia Camphorata sample 4 tumour inhibiting rates are 26.16% (P＜0.001), and the tumor control rate of all the other Antrodia Camphorata samples 1,2,3 is respectively 17.38% (P＞0.05), 19.07% (P＞0.05), 14.74% (P＞0.05).
Table 1: oral Chinese medicine preparation Antrodia Camphorata is to the inhibitory action of mice lung cancer (Lewis)
Table 2: each experimental group body weight change (g)
4 experiment conclusion:
This experimental result: oral Antrodia Camphorata 4 sample sets tumor control rates are 26.16% (P＜0.001), be higher than other each experimental group, the tumor control rate of all the other Antrodia Camphorata samples 1,2,3 is respectively 17.38% (P＞0.05), 19.07% (P＞0.05), 14.74% (P＞0.05), and its toxic and side effects is less than cyclophosphamide.
Embodiment 2:
(1) preparation Antrodia Camphorata extract: get the Antrodia Camphorata coarse powder, 10 times of concentration of adding Antrodia Camphorata coarse powder weight are 60% ethanol, under 60 ℃ of temperature, extract after 3 hours, filter; Get filtered filtration residue, in filtering residue, add 5 times of concentration of filtering residue weight again and be 60% ethanol, under 65 ℃ of temperature, extract after 2 hours, filter; Merge filtrate twice, reclaim ethanol,, obtain extractum until there not being the alcohol flavor with alcohol reflux tower reflux condensation mode; Get the water that filtering residue after above-mentioned second time filters adds 15 times of filtering residue weight, extract after 3 hours, filter; Get filtered filtration residue, add the water of 15 times of filtering residue weight in the filtering residue, extract after 3 hours, filter; After merging twice filtrate and above-mentioned extractum, carry out evaporation and concentration, being concentrated into density is 1.05g/cm
3, carry out spray drying then, 220 ℃ of spray drying inlet temperature, leaving air temp is collected spray powder for 80 ℃, promptly obtains the Antrodia Camphorata extract;
(2) preparation Ganoderma extract: get the Ganoderma coarse powder, 8 times of concentration of adding Ganoderma coarse powder weight are 80% ethanol, under 80 ℃ of temperature, extract after 1 hour, filter; Get filtered filtration residue, in filtering residue, add 3 times of concentration of filtering residue weight again and be 80% ethanol, under 80 ℃ of temperature, extract after 1 hour, filter; Merge filtrate twice, reclaim ethanol,, obtain extractum until there not being the alcohol flavor with alcohol reflux tower reflux condensation mode; The filtering residue of getting after filter the above-mentioned second time adds the water of 15 times of filtering residue weight, and with food grade sodium hydroxide adjusting PH to 9, extracts after 3 hours, filters; Get filtered filtration residue, add the water of 8 times of filtering residue weight in the filtering residue, and regulate PH to 9, extract after 1 hour, filter with the food grade sodium hydroxide; After merging twice filtrate and above-mentioned extractum, carry out evaporation and concentration, being concentrated into density is 1.03g/cm
3, carry out spray drying then, 225 ℃ of spray drying inlet temperature, leaving air temp is collected spray powder for 85 ℃, promptly obtains Ganoderma extract;
(3) preparation Grifola frondosa extract: get the Grifola frondosa fine powder, add the water of 25 times of Grifola frondosa fine powder weight, extract after 2 hours, carry out filter pressing; Get filtrate concentrating, being concentrated into relative density is 1.0g/cm
3In concentrated solution, add 3 times of concentration of concentrated solution volume and be 95% ethanol and carry out precipitate with ethanol, stirred 20 minutes, place after 10 hours, filter; Filter rear filtrate and reclaim ethanol, precipitate adds entry, heats, stir simultaneously, and be 1.05g/cm until density
3, carry out spray drying then, 220 ℃ of spray drying inlet temperature, 80 ℃ of leaving air temps are collected spray powder, promptly obtain the Grifola frondosa extract;
(4) above-mentioned resulting Antrodia Camphorata extract, Ganoderma extract and Grifola frondosa extract are mixed by following percentage by weight: Antrodia Camphorata extract 60%, Ganoderma extract 20%, Grifola frondosa extract 20%.
The pharmaceutical composition that obtains at last is through test, and its tumor control rate is 23.5%.
Embodiment 3:
(1) preparation Antrodia Camphorata extract: get the Antrodia Camphorata coarse powder, 5 times of concentration of adding Antrodia Camphorata coarse powder weight are 80% ethanol, under 80 ℃ of temperature, extract after 1 hour, filter; Get filtered filtration residue, in filtering residue, add 1 times of concentration of filtering residue weight again and be 80% ethanol, under 60 ℃ of temperature, extract after 3 hours, filter; Merge filtrate twice, reclaim ethanol,, obtain extractum until there not being the alcohol flavor with alcohol reflux tower reflux condensation mode; Get the water that filtering residue after above-mentioned second time filters adds 25 times of filtering residue weight, extract after 1 hour, filter; Get filtered filtration residue, add the water of 5 times of filtering residue weight in the filtering residue, extract after 3 hours, filter; After merging twice filtrate and above-mentioned extractum, carry out evaporation and concentration, being concentrated into density is 1.5g/cm
3, carry out spray drying then, 240 ℃ of spray drying inlet temperature, leaving air temp is collected spray powder for 100 ℃, promptly obtains the Antrodia Camphorata extract;
(2) preparation Ganoderma extract: get the Ganoderma coarse powder, 10 times of concentration of adding Ganoderma coarse powder weight are 60% ethanol, under 60 ℃ of temperature, extract after 3 hours, filter; Get filtered filtration residue, in filtering residue, add 5 times of concentration of filtering residue weight again and be 60% ethanol, under 60 ℃ of temperature, extract after 3 hours, filter; Merge filtrate twice, reclaim ethanol,, obtain extractum until there not being the alcohol flavor with alcohol reflux tower reflux condensation mode; The filtering residue of getting after filter the above-mentioned second time adds the water of 25 times of filtering residue weight, and with food grade sodium hydroxide adjusting PH to 7, extracts after 1 hour, filters; Get filtered filtration residue, add the water of 15 times of filtering residue weight in the filtering residue, and regulate PH to 7, extract after 3 hours, filter with the food grade sodium hydroxide; After merging twice filtrate and above-mentioned extractum, carry out evaporation and concentration, being concentrated into density is 1.2g/cm
3, carry out spray drying then, 240 ℃ of spray drying inlet temperature, leaving air temp is collected spray powder for 100 ℃, promptly obtains Ganoderma extract;
(3) preparation Grifola frondosa extract: get the Grifola frondosa fine powder, add the water of 28 times of Grifola frondosa fine powder weight, extract after 6 hours, carry out filter pressing; Get filtrate concentrating, being concentrated into relative density is 1.1g/cm
3In concentrated solution, add 2.5 times of concentration of concentrated solution volume and be 95% ethanol and carry out precipitate with ethanol, stirred 40 minutes, place after 15 hours, filter; Filter rear filtrate and reclaim ethanol, precipitate adds entry, heats, stir simultaneously, and be 1.0g/cm until density
3, carry out spray drying then, 230 ℃ of spray drying inlet temperature, 90 ℃ of leaving air temps are collected spray powder, promptly obtain the Grifola frondosa extract;
(4) above-mentioned resulting Antrodia Camphorata extract, Ganoderma extract and Grifola frondosa extract are mixed by following percentage by weight: Antrodia Camphorata extract 55%, Ganoderma extract 15%, Grifola frondosa extract 30%.
The pharmaceutical composition that obtains at last is through test, and its tumor control rate is 24.5%.
Embodiment 4:
(1) preparation Antrodia Camphorata extract: get the Antrodia Camphorata coarse powder, 2 times of concentration of adding Antrodia Camphorata coarse powder weight are 78% ethanol, under 65 ℃ of temperature, extract after 2.5 hours, filter; Get filtered filtration residue, in filtering residue, add 3 times of concentration of filtering residue weight again and be 65% ethanol, under 80 ℃ of temperature, extract after 1 hour, filter; Merge filtrate twice, reclaim ethanol,, obtain extractum until there not being the alcohol flavor with alcohol reflux tower reflux condensation mode; Get the water that filtering residue after above-mentioned second time filters adds 20 times of filtering residue weight, extract after 2.5 hours, filter; Get filtered filtration residue, add the water of 8 times of filtering residue weight in the filtering residue, extract after 1 hour, filter; After merging twice filtrate and above-mentioned extractum, carry out evaporation and concentration, being concentrated into density is 1.0g/cm
3, carry out spray drying then, 230 ℃ of spray drying inlet temperature, leaving air temp is collected spray powder for 100 ℃, promptly obtains the Antrodia Camphorata extract;
(2) preparation Ganoderma extract: get the Ganoderma coarse powder, 2 times of concentration of adding Ganoderma coarse powder weight are 65% ethanol, under 60 ℃ of temperature, extract after 2.5 hours, filter; Get filtered filtration residue, in filtering residue, add 1 times of concentration of filtering residue weight again and be 65% ethanol, under 65 ℃ of temperature, extract after 3 hours, filter; Merge filtrate twice, reclaim ethanol,, obtain extractum until there not being the alcohol flavor with alcohol reflux tower reflux condensation mode; The filtering residue of getting after filter the above-mentioned second time adds the water of 20 times of filtering residue weight, and with food grade sodium hydroxide adjusting PH to 8, extracts after 2.5 hours, filters; Get filtered filtration residue, add the water of 5 times of filtering residue weight in the filtering residue, and regulate PH to 8, extract after 2.5 hours, filter with the food grade sodium hydroxide; After merging twice filtrate and above-mentioned extractum, carry out evaporation and concentration, being concentrated into density is 1.0g/cm
3, carry out spray drying then, 240 ℃ of spray drying inlet temperature, leaving air temp is collected spray powder for 100 ℃, promptly obtains Ganoderma extract;
(3) preparation Grifola frondosa extract: get the Grifola frondosa fine powder, add the water of 35 times of Grifola frondosa fine powder weight, extract after 5 hours, carry out filter pressing; Get filtrate concentrating, being concentrated into relative density is 1.05g/cm
3In concentrated solution, add 1 times of concentration of concentrated solution volume and be 95% ethanol and carry out precipitate with ethanol, stirred 35 minutes, place after 15 hours, filter; Filter rear filtrate and reclaim ethanol, precipitate adds entry, heats, stir simultaneously, and be 1.01g/cm until density
3, carry out spray drying then, 230 ℃ of spray drying inlet temperature, 90 ℃ of leaving air temps are collected spray powder, promptly obtain the Grifola frondosa extract;
(4) above-mentioned resulting Antrodia Camphorata extract, Ganoderma extract and Grifola frondosa extract are mixed by following percentage by weight: Antrodia Camphorata extract 55%, Ganoderma extract 15%, Grifola frondosa extract 30%.
The pharmaceutical composition that obtains at last is through test, and its tumor control rate is 26.05%.
Embodiment 5:
Press Antrodia Camphorata extract 35%, Ganoderma extract 25% and Grifola frondosa extract 40% and mix, other Step By Conditions are all identical with embodiment 1, and the pharmaceutical composition that obtains at last is through test, and its tumor control rate is 24.15%.
Embodiment 6:
Press Antrodia Camphorata extract 54%, Ganoderma extract 14% and Grifola frondosa extract 32% and mix, other Step By Conditions are all identical with embodiment 1, and the pharmaceutical composition that obtains at last is through test, and its tumor control rate is 25.18%.
Claims (10)
1. antitumor medicine composition is characterized in that being made of following by weight percentage:
Antrodia Camphorata extract 20%-60% Ganoderma extract 5%-30% Grifola frondosa extract 20%-60%.
2. a kind of antitumor medicine composition as claimed in claim 1 is characterized in that being made of following by weight percentage:
Antrodia Camphorata extract 25%-55% Ganoderma extract 10%-25% Grifola frondosa extract 25%-55%.
3. a kind of antitumor medicine composition as claimed in claim 1 is characterized in that being made of following by weight percentage:
Antrodia Camphorata extract 30%-50% Ganoderma extract 15%-20% Grifola frondosa extract 30%-50%.
4. a kind of antitumor medicine composition as claimed in claim 1 is characterized in that being made of following by weight percentage:
Antrodia Camphorata extract 35%-45% Ganoderma extract 15%-20% Grifola frondosa extract 35%-45%.
5. the production method of an antitumor medicine composition is characterized in that comprising following processing step:
(1) preparation Antrodia Camphorata extract: get the Antrodia Camphorata coarse powder, the ethanol that 2-10 times of concentration of adding Antrodia Camphorata coarse powder weight is 60-80% under temperature 60-80 ℃, extracts after 1-3 hour, filters; Get filtered filtration residue, the ethanol that 1-5 times of concentration of adding filtering residue weight is 60-80% in filtering residue under temperature 60-80 ℃, extracts after 1-3 hour again, filters; Merge filtrate twice, reclaim ethanol, it is standby to obtain extractum; The filtering residue of getting after filter the above-mentioned second time adds filtering residue weight 15-25 water doubly, extracts after 1-3 hour, filters; Get filtered filtration residue, add filtering residue weight 5-15 water doubly in the filtering residue, extract after 1-3 hour, filter; After merging twice filtrate and above-mentioned extractum, carry out thin film evaporation and concentrate, being concentrated into density is 1.0-1.5g/cm
3, carry out spray drying then, collect spray powder, promptly obtain the Antrodia Camphorata extract;
(2) preparation Ganoderma extract: get the Ganoderma coarse powder, the ethanol that 2-10 times of concentration of adding Ganoderma coarse powder weight is 60-80% under temperature 60-80 ℃, extracts after 1-3 hour, filters; Get filtered filtration residue, the ethanol that 1-5 times of concentration of adding filtering residue weight is 60-80% in filtering residue under temperature 60-80 ℃, extracts after 1-3 hour again, filters; Merge filtrate twice, reclaim ethanol, it is standby to obtain extractum; The filtering residue of getting after filter the above-mentioned second time adds filtering residue weight 15-25 water doubly, and regulates PH to 7-9, extracts after 1-3 hour, filters; Get filtered filtration residue, add filtering residue weight 5-15 water doubly in the filtering residue, and regulate PH to 7-9, extract after 1-3 hour, filter; After merging twice filtrate and above-mentioned extractum, carry out thin film evaporation and concentrate, being concentrated into density is 1.0-1.2g/cm
3, carry out spray drying then, collect spray powder, promptly obtain Ganoderma extract;
(3) preparation Grifola frondosa extract: get the Grifola frondosa fine powder, add Grifola frondosa fine powder weight 25-35 water doubly, extract after 2-6 hour, carry out filter pressing; Get filtrate concentrating, being concentrated into relative density is 1.0-1.1g/cm
3In concentrated solution, add 1-3 times of concentration of concentrated solution volume and be 95% ethanol and carry out precipitate with ethanol, stirred 20-40 minute, place after 10-15 hour, filter; Filter rear filtrate and reclaim ethanol, precipitate adds entry, and heating for dissolving stirs simultaneously, regulates density to 1.0-1.05g/cm
3, spray drying is collected spray powder then, promptly obtains the Grifola frondosa extract;
(4) above-mentioned resulting Antrodia Camphorata extract, Ganoderma extract and Grifola frondosa extract are mixed by following percentage by weight:
Antrodia Camphorata extract 20%-60% Ganoderma extract 5%-30% Grifola frondosa extract 20%-60% promptly obtains antineoplastic pharmaceutical compositions.
6. the production method of a kind of antitumor medicine composition as claimed in claim 5 is characterized in that adding the 4-8 times of ethanol that concentration is 65-75% in the step (1) in the Antrodia Camphorata coarse powder, under temperature 65-75 ℃, extracts 2-3 hour; Get filtered filtration residue, in filtering residue, add the 2-4 times of ethanol that concentration is 65-75% again, under temperature 65-75 ℃, extract after 2-3 hour; Merge filtrate twice, reflux condensation mode reclaims ethanol, until there not being the alcohol flavor, obtains extractum; Add 17-23 water doubly in the filtering residue after filtering for the second time, extracted 1.5-2.5 hour; Get filtered filtration residue, add 8-12 water doubly in the filtering residue, extracted 1.5-2.5 hour; Evaporation and concentration to density is 1.02-1.03g/cm
3, spray drying adopts 220-240 ℃ of inlet temperature, leaving air temp 80-100 ℃.
7. the production method of a kind of antitumor medicine composition as claimed in claim 5 is characterized in that getting the Ganoderma coarse powder in the step (2), adds the 4-8 times of ethanol that concentration is 65-75%, under temperature 65-75 ℃, extracts 2-3 hour; Get filtered filtration residue, in filtering residue, add the 2-4 times of ethanol that concentration is 65-75% again, under temperature 65-75 ℃, extract after 2-3 hour; Merge filtrate twice, reflux condensation mode reclaims ethanol, until there not being the alcohol flavor, obtains extractum; 17-23 water is doubly regulated PH to 7.5-8 with the food grade sodium hydroxide in the filtering residue after filtering for the second time, extracts 1.5-2.5 hour; Get filtered filtration residue, add 8-12 water doubly in the filtering residue, regulate PH to 7.5-8, extracted 1.5-2.5 hour with the food grade sodium hydroxide; Evaporation and concentration to density is 1.02-1.03g/cm
3, spray drying adopts 220-240 ℃ of inlet temperature, leaving air temp 80-100 ℃.
8. the production method of a kind of antitumor medicine composition as claimed in claim 5 is characterized in that adding in the step (3) Grifola frondosa fine powder weight 27-33 water doubly, extracts 3-5 hour; Filtrate is carried out evaporation and concentration, and being concentrated into relative density is 1.07-1.09g/cm
3Add 1.5-2.5 times of concentration of concentrated solution volume in the concentrated solution and be 95% ethanol and carry out precipitate with ethanol, stirred 25-35 minute, placed 11-14 hour; Filter the rear filtrate reflux condensation mode and reclaim ethanol, precipitate adds entry, is 1.0-1.04g/cm until density
3, spray drying adopts 220-230 ℃ of inlet temperature, leaving air temp 80-90 ℃.
9. the production method of a kind of antitumor medicine composition as claimed in claim 5 is characterized in that Antrodia Camphorata extract, Ganoderma extract and Grifola frondosa extract mix by following percentage by weight in the step (4):
Antrodia Camphorata extract 25%-55% Ganoderma extract 10%-25% Grifola frondosa extract 25%-55%.
10. the production method of a kind of antitumor medicine composition as claimed in claim 5 is characterized in that Antrodia Camphorata extract, Ganoderma extract and Grifola frondosa extract mix by following percentage by weight in the step (4):
Antrodia Camphorata extract 30%-50% Ganoderma extract 15%-20% Grifola frondosa extract 30%-50.
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