CN102641448B - Anti-lung-cancer traditional Chinese medicine composite, preparation method of composite, and application of composite in preparation of anti-lung-cancer medicament - Google Patents
Anti-lung-cancer traditional Chinese medicine composite, preparation method of composite, and application of composite in preparation of anti-lung-cancer medicament Download PDFInfo
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Abstract
The invention discloses an anti-lung-cancer traditional Chinese medicine composite, a preparation method of the composite, and an application of the composite in preparation of an anti-lung-cancer medicament. The composite comprises the following active pharmaceutical ingredients in parts by weight: 5 to 40 parts of ganoderma lucidum, 5 to 40 parts of semen coicis and 1 to 10 parts of lily; and as optimization, the composite comprises 20 parts of ganoderma lucidum, 20 parts of semen coicis and 3 parts of lily. The composite consists of six active ingredients including total triterpenoid of the ganoderma lucidum, coix seed oil, total alkaloids of the lily, ganoderma lucidum polysaccharides, semen coicis polysaccharides and lily polysaccharides. The composite disclosed by the invention has an obvious inhibition effect on the growth of Lewis tumors, the antitumor activity of the composite is superior to that of a single component after compatibility administration, and the tumor inhibition rate of the composite can reach 55.13%. Therefore, the active ingredients in the composite are extracted and separated to the greatest extent by virtue of a modern extraction and separation method, and the collaborative antitumor effect of the composite can better come into play by virtue of compatibility combination.
Description
Technical field
The present invention relates to technical field of Chinese medicines, be specifically related to a kind of anti-pulmonary carcinoma Chinese medicine composition, this anti-pulmonary carcinoma Chinese medicine composition preparation method, and the application of this Chinese medicine composition in preparing anti-lung-cancer medicament.
Background technology
At present, pulmonary carcinoma has become a large killer who threatens human health.According to domestic and foreign literature, the new cases of global pulmonary carcinoma, up to 205 020, account for 14% of global various tumor new cases, have the characteristics of rate occurred frequently and high mortality.Under the many-side impact of the factors such as environmental pollution, smoking, ionizing radiation, occupational exposure and viral infection, the sickness rate of pulmonary carcinoma and mortality rate are in propradation always, annual speed with 0.5% increases, and along with the increase of smoking in adolescents number, pulmonary carcinoma is rejuvenation increasingly.According to China Ministry of Public Health death survey result in 2008, show, pulmonary carcinoma has replaced hepatocarcinoma to become the first malignant tumor cause of the death of China (account for whole mortality of malignant tumors 22.7%).Therefore, the diagnosis of pulmonary carcinoma and treatment cause the enough attention of medical circle.
Pulmonary carcinoma is divided into small cell lung cancer (SCLC, 20%) and nonsmall-cell lung cancer (NSCLC, 80%), its pathogenic factor complexity.The at present both at home and abroad treatment of pulmonary carcinoma is take operation and radiotherapy, chemotherapy as main, but these methods easily cause larger side effect to patient's normal organ, and patient's prognosis and survival rate are poor.Chinese medicine take " eliminating pathogenic factor for supporting vital QI " as characteristic is being brought into play great function aspect treatment pulmonary carcinoma, and its curative effect is not only consolidated, and toxic and side effects is little, to body, can not cause large injury, with chemotherapy, also uses the effect that can play efficacy enhancing and toxicity reducing.Therefore from the anti-lung-cancer medicament of finding and develop high-efficiency low-toxicity Chinese medicine and natural drug, be focus and the difficult point of oncology studies.
Through retrieval, 200910266137.0), " a kind of Chinese medicine for the treatment of cancer " (patent No.: 200710166579.9) Chinese medicine composition that has multiple treatment cancer in existing patent, as " medicine-food dual-purpose composition of a kind of cancer patient of being applicable to and preparation method thereof the " (patent No.:; " a kind of herbal composite for the treatment of liver, stomach, lung, leukemia and preparation method thereof " (patent No.: 201110125724.5); " a kind of Chinese medicine composition for the treatment of cancer and preparation method thereof " (patent No.: 201110165923.9); 201110145442.1), " anticancer traditional Chinese medicinal composition and application thereof " (201110056786.5) etc. " a kind of Chinese medicine composition and application for the treatment of malignant tumor " (patent No.:, medicament categories used in these compositionss is more, and take mainly with decoction, or preparation technology is simpler, extract to such an extent that directly make oral formulations after extractum, the preparation dose is larger, although certain therapeutic effect is arranged clinically, but the extraction ratio of effective ingredient is lower, preparation is thicker, is unfavorable for the quality control of preparation.
Patent has been reported the antineoplastic related preparations of Ganoderma and Semen Coicis, and (200910031997.6 disclose a kind of self-mciro emulsifying nano composition and preparation method thereof of ganodenic acid extract of anti-tumor activity; 201110097796.3 disclose a kind of compound ganoderma lucidum spore soft capsule and preparation method thereof; 101010237432.6 disclose a kind of Coix seed anticancer Chinese medicament and preparation method thereof), these anti-tumor agents have just utilized Ganoderma total triterpenes, the single active component of Semen Coicis oil, and some component that plays assosting effect is abandoned, and [Lin Zhibin according to the literature, Wang Pengyun. the pharmacological research of Ganoderma spore and active component thereof [J]. Peking University's journal (medicine), 2006,38 (5): 541-547; Zhang Yumei, Yang Junshan, Zhao Yangjing, Deng. Semen Coicis chemical composition and pharmacology activity research progress [J]. Chinese Pharmaceutical Journal, 2002,37 (1): 8-11], ganoderan and coixan also have antitumor and immunoregulation effect, and therefore above-mentioned preparation can't embody the characteristics of Chinese medicine multicomponent, many target spots wholistic therapy.In addition, 201010187617.0 disclose the preparation of a kind of anticancer pharmaceutical composition and a kind of Chinese medicine composition, although being used in conjunction with of Chinese medicine composition (concentrated dry powder of the decoction liquor of medical material itself, medical material, the concentrated extract of decoction liquor or decoction liquor) and polysaccharide component paid attention in this invention, but the medical material kind that contains in this pharmaceutical composition is more, and the polysaccharide component not derives from the medical material in said composition, complicated component, be difficult to carry out quality control.
Summary of the invention
The purpose of this invention is to provide a kind of Chinese medicine composition with effect of anti-lung cancer and preparation method thereof, and this has the application of Chinese medicine composition in preparing anti-lung-cancer medicament of effect of anti-lung cancer, by selecting suitable medicine and suitable active component extracting method, optimize the proportion relation of active component, the final preparation method of determining Chinese medicine composition optimization prescription, optimizing component compatibility and compositions, make it bring into play antitumor action safely and effectively, be applicable to clinical practice.
First goal of the invention of the present invention is to realize by following technical scheme:
A kind of anti-pulmonary carcinoma Chinese medicine composition, is characterized in that, the weight portion of said composition crude drug is composed as follows: 5 ~ 40 parts of Ganodermas, 5 ~ 40 parts of Semen Coiciss, 1 ~ 10 part of Bulbus Lilii.
Wherein crude drug preferably consumption be: 10 ~ 30 parts of Ganodermas, 10 ~ 30 parts of Semen Coiciss, 1 ~ 6 part of Bulbus Lilii.
Wherein crude drug more preferably consumption be: 3 parts of 20 portions of Bulbus Liliies of 20 parts of Semen Coiciss of Ganoderma.
In recent years, Chinese medicine Ganoderma, Semen Coicis, the Bulbus Lilii as " integration of edible and medicinal herbs " receives the concern of research worker always in the exploitation of the research aspect anti-pulmonary carcinoma and new drug thereof.The present invention is comprised of this three flavors medical material, and the present Research of ingredients is as follows:
Ganoderma is the On Polyporaceae Ganoderma lucidum (Leyss. Ex Fr.) Karst.
Ganoderma lucidum(Leyss. ex Fr.) Karst. or Ganoderma
Ganoderma sinenseZhao. dry sporophore Xu et Zhang).GUIXIN, lung, liver, kidney channel.Has invigorating QI and tranquilization, the effect of relieving cough and asthma.For cough and asthma due to lung deficiency, asthenia is losed heart etc.Modern scientific research shows, Ganoderma has stronger antitumor action, and its antineoplastic active site is mainly Ganoderma triterpenoids and polysaccharide component.
Semen Coicis is the grass Semen Coicis
Coix lacryma-jobiL. var.
Ma-yuen(Roman.) dry mature kernal of Stapf.Return spleen, stomach, lung meridian.Has promoting diuresis to eliminate damp pathogen, invigorating the spleen to arrest diarrhea, eliminating impediment, evacuation of pus, the effect of detoxicating and resolving stagnation of pathogens.For lung abscess, acute appendicitis, wart, cancerous protuberance etc.Modern study shows, Semen Coicis has the antineoplastic pharmacological action, in core, contains numerous anti-tumor active ingredients, is mainly esters and fatty acid compound and polysaccharide component.
Bulbus Lilii is the liliaceous plant tiger lily
Lilium lancifoliumThunb., Bulbus Lilii
Lilium browniiF. E. Brown var.
ViridulumBaker) or Lilium tenuifolium
Lilium pumilumDC. dry meat scale leaf.GUIXIN, lung meridian.Has nourishing YIN and moistening the lung, the effect of clearing away heart-fire for tranquillization.For deficiency of YIN cough caused by dryness, chronic cough hemoptysis etc.Modern study shows, Bulbus Lilii has anti-tumor activity preferably, and its antineoplastic main active is biological alkali components and polysaccharide component.
This Chinese medicine composition is clinical anti-pulmonary carcinoma proved recipe, and the Ganoderma invigorating QI and tranquilization, be monarch drug, the Semen Coicis invigorating spleen to remove dampness, and the Bulbus Lilii yin nourishing is calmed the nerves, and is all ministerial drug.Full side has boosting qi and nourishing yin, promoting diuresis to eliminate damp pathogen, and the effect of dispersing tumor softening the hard mass, be applicable to malignant tumor deficiency of qi and yin, retention of water-damp person.
Further optimization of the present invention can obtain following technical scheme:
Described anti-pulmonary carcinoma Chinese medicine composition, be comprised of Ganoderma total triterpenes, Semen Coicis oil, Bulbus Lilii total alkaloids, ganoderan, coixan and 6 active components of Bulbus Lilii polysaccharide.Wherein, the weight portion of Ganoderma total triterpenes, Semen Coicis oil, Bulbus Lilii total alkaloids consists of: Ganoderma total triterpenes 1 ~ 20, Semen Coicis oil 1 ~ 35, Bulbus Lilii total alkaloids 1 ~ 10; Ganoderan wherein, coixan and Bulbus Lilii polysaccharide are to add by its crude drug and Ganoderma total triterpenes, Semen Coicis oil, crude drug amount 1:1 weight ratio that the Bulbus Lilii total alkaloids is identical.
The weight ratio of described Ganoderma total triterpenes, Semen Coicis oil, Bulbus Lilii total alkaloids, ganoderan, coixan and Bulbus Lilii polysaccharide is 18-22:33-37:1:33-37:43-47:3-5.
Optimal proportion is that the weight ratio of described Ganoderma total triterpenes, Semen Coicis oil, Bulbus Lilii total alkaloids, ganoderan, coixan and Bulbus Lilii polysaccharide is 20:35:1:35:45:4.
Wherein, the Ganoderma total triterpenes extraction ratio is 3.75%, and purity is 61.50%; The Semen Coicis oil extraction ratio is 6.62%, and purity is 74.35%; Bulbus Lilii total alkaloids extraction ratio is 1.25%, and purity is 59.92%; The ganoderan extraction ratio is 6.56%, and purity is 57.70%; The coixan extraction ratio is 8.40%, and purity is 64.42%; The Bulbus Lilii polysaccharide extraction ratio is 4.84%, and purity is 62.53%.
More particularly, anti-pulmonary carcinoma Chinese medicine composition of the present invention refers to the compositions that obtains according to following preparation method:
Step ⑴: Ganoderma sporophore is pulverized and sieved, adopt supercritical CO
2Extraction extracts Ganoderma total triterpenes class component;
Step ⑵: Ganoderma coarse powder residue decocts with water, and filtrate is concentrated, the ethanol precipitation, and collecting precipitation, the precipitation water dissolves again, and except insoluble impuritiess such as deproteinizes, concentrate drying, finally obtain ganoderan class component;
Step ⑶: Semen Coicis is pulverized and sieved, adopt supercritical CO
2Extraction extracts Semen Coicis oil;
Step ⑷: Semen Coicis coarse powder residue decocts with water, and filtrate is concentrated, the ethanol precipitation, and collecting precipitation, the precipitation water dissolves again, and except insoluble impuritiess such as deproteinizes, concentrate drying, finally obtain coixan class component;
Step ⑸: Bulbus Lilii is pulverized and sieved, with acid ethanol solution, extract, reclaim ethanol, reclaim liquid and alkalize with strong aqua ammonia, then use chloroform extraction, reclaim chloroform, drying, obtain Bulbus Lilii total alkaloids class component;
Step ⑹: Bulbus Lilii coarse powder residue decocts with water, and filtrate is concentrated, the ethanol precipitation, and collecting precipitation, the precipitation water dissolves again, and except insoluble impuritiess such as deproteinizes, concentrate drying, finally obtain Bulbus Lilii polysaccharide class component;
Step ⑺: by the component mix homogeneously that above each step obtains, obtain described anti-pulmonary carcinoma Chinese medicine composition.
The technical scheme that completes second invention task of the present invention is: the preparation method of above-mentioned anti-pulmonary carcinoma Chinese medicine composition: it is characterized in that, step is as follows,
Step ⑴: Ganoderma sporophore is pulverized and sieved, adopt supercritical CO
2Extraction extracts Ganoderma total triterpenes class component;
Step ⑵: Ganoderma coarse powder residue decocts with water, and filtrate is concentrated, the ethanol precipitation, and collecting precipitation, the precipitation water dissolves again, and except insoluble impuritiess such as deproteinizes, concentrate drying, finally obtain ganoderan class component;
Step ⑶: Semen Coicis is pulverized and sieved, adopt supercritical CO
2Extraction extracts Semen Coicis oil;
Step ⑷: Semen Coicis coarse powder residue decocts with water, and filtrate is concentrated, the ethanol precipitation, and collecting precipitation, the precipitation water dissolves again, and except insoluble impuritiess such as deproteinizes, concentrate drying, finally obtain coixan class component;
Step ⑸: Bulbus Lilii is pulverized and sieved, with acid ethanol solution, extract, reclaim ethanol, reclaim liquid and alkalize with strong aqua ammonia, then use chloroform extraction, reclaim chloroform, drying, obtain Bulbus Lilii total alkaloids class component;
Step ⑹: Bulbus Lilii coarse powder residue decocts with water, and filtrate is concentrated, the ethanol precipitation, and collecting precipitation, the precipitation water dissolves again, and except insoluble impuritiess such as deproteinizes, concentrate drying, finally obtain Bulbus Lilii polysaccharide class component;
Step ⑺: by the component mix homogeneously that above each step obtains, obtain described anti-pulmonary carcinoma Chinese medicine composition.
The further optimization of above preparation method, concrete operation step is:
Step ⑴: Ganoderma sporophore is pulverized and sieved, adopt supercritical CO
2Extraction extracts Ganoderma total triterpenes class component, and extracting pressure is 20 ~ 40MPa, and extraction temperature is 40 ~ 50 ℃, and extraction time is 1 ~ 3 h, and entrainer (percent by volume 95% ethanol) consumption is 1 ~ 4 mLg
-1Crude drug.
Step ⑵: Ganoderma coarse powder residue, add the decocting of 8 ~ 14 times of amounts to boil, decocting number of times is 1 ~ 3 time, each 1 ~ 3h, and filtrate is concentrated, it is 60 ~ 90% that concentrated solution alcohol is sink to concentration of alcohol (percent by volume), collecting precipitation, precipitation is dissolved with the water of 4 ~ 10 times of amounts again, except insoluble impuritiess such as deproteinizes, concentrate drying, finally obtain ganoderan class component.
Step ⑶: Semen Coicis is pulverized and sieved, adopt supercritical CO
2Extraction extracts Semen Coicis oil, and extracting pressure is 15 ~ 25MPa, and extraction temperature is 30 ~ 40 ℃, and extraction time is 1 ~ 3 h, and entrainer (percent by volume 95% ethanol) consumption is 1 ~ 4 mLg
-1Crude drug.
Step ⑷: Semen Coicis coarse powder residue, add the decocting of 8 ~ 14 times of amounts to boil, decocting number of times is 1 ~ 3 time, each 1 ~ 3 h, and filtrate is concentrated, it is 60 ~ 90% that concentrated solution alcohol is sink to concentration of alcohol (percent by volume), collecting precipitation, precipitation is dissolved with the water of 4 ~ 10 times of amounts again, except insoluble impuritiess such as deproteinizes, concentrate drying, finally obtain coixan class component.
Step ⑸: Bulbus Lilii is pulverized and sieved, the volume fraction that adds 5 ~ 10 times of amounts is that the alcoholic solution (containing 1% acetic acid) of 70%-90% extracts, extraction time is 1 ~ 3 time, each 1 ~ 3 h, reclaim ethanol, reclaims liquid and alkalize to pH8 ~ 11 with strong aqua ammonia, again with equal amounts of chloroform extraction 2 ~ 8 times, reclaim chloroform, drying, obtain Bulbus Lilii total alkaloids class component.
Step ⑹: Bulbus Lilii coarse powder residue, add the decocting of 8 ~ 14 times of amounts to boil, decocting number of times is 1 ~ 3 time, each 1 ~ 3 h, and filtrate is concentrated, it is 60 ~ 90% that concentrated solution alcohol is sink to concentration of alcohol (percent by volume), collecting precipitation, precipitation is dissolved with the water of 4 ~ 10 times of amounts again, except insoluble impuritiess such as deproteinizes, concentrate drying, finally obtain Bulbus Lilii polysaccharide class component.
Step ⑺: by the component mix homogeneously that above each step obtains, obtain described anti-pulmonary carcinoma Chinese medicine composition.
In the prioritization scheme of Chinese medicine composition preparation method of the present invention,
The described extraction conditions of step ⑴ is: extracting pressure 25 ~ 35MPa, and extraction temperature is 43 ~ 48 ℃; Extraction time is 1 ~ 2 h, and entrainer (95% ethanol) consumption is 2 ~ 3 mLg
-1Crude drug;
Step ⑵ is described to be decocted with water, and is the water that adds 9 ~ 11 times of amounts, and decocting number of times is 1 ~ 2 time, each 1 ~ 2h;
Described concentrated solution precipitate with ethanol condition is that to be sink to concentration of alcohol (percent by volume) be 75 ~ 85% to concentrated solution alcohol;
Described precipitation is to dissolve with the water of 5 ~ 7 times of amounts again;
The described extraction conditions of step ⑶ is: extracting pressure is 20 ~ 25MPa, and extraction temperature is 35 ~ 40 ℃, and extraction time is 2 ~ 3 h, and entrainer (95% ethanol) consumption is 2 ~ 3 mLg
-1Crude drug;
Step ⑷ is described to be decocted with water, and is the water that adds 9 ~ 11 times of amounts, and decocting number of times is 1 ~ 2 time, each 1 ~ 2 h;
Described concentrated solution precipitate with ethanol condition is that to be sink to concentration of alcohol (percent by volume) be 75 ~ 85% to concentrated solution alcohol;
Described precipitation is to dissolve with the water of 5 ~ 7 times of amounts again;
Step ⑸ is described to be added ethanol acetate and extracts, and is that to add the volume fraction of 6 ~ 8 times of amounts be that 75% ~ 85% alcoholic solution (containing percent by volume 1% acetic acid) extracts, and extraction time is 1 ~ 2 time, each 1 ~ 2 h;
Described filtrate is to alkalize to pH9 ~ 10 with strong aqua ammonia;
With the equal amounts of chloroform extraction, it is 3 ~ 7 times again;
Step ⑹ is described to be decocted with water, and is the water that adds 9 ~ 11 times of amounts, and decocting number of times is 1 ~ 2 time, each 1 ~ 2 h;
Described concentrated solution precipitate with ethanol condition is that to be sink to concentration of alcohol (percent by volume) be 75 ~ 85% to concentrated solution alcohol;
Described precipitation is to dissolve with the water of 5 ~ 7 times of amounts again.
In the prioritization scheme of Chinese medicine composition preparation method, the condition that the present invention recommends is:
The described extraction conditions of step ⑴ is: extracting pressure is 30 MPa, and extraction temperature is 45 ℃; Extraction time is 1.5 h, and entrainer (percent by volume 95% ethanol) consumption is 3 mLg
-1Crude drug;
Step ⑵ is described to be decocted with water, and is the water that adds 10 times of amounts, and decocting number of times is 2 times, each 1 h;
Described concentrated solution precipitate with ethanol condition is that to be sink to concentration of alcohol (percent by volume) be 80% to concentrated solution alcohol;
Described precipitation is to dissolve with the water of 6 times of amounts again;
The described extraction conditions of step ⑶ is: extracting pressure is 22MPa, and extraction temperature is 38 ℃; Extraction time is 2.5 h, and entrainer (95% ethanol) consumption is 3 mLg
-1Crude drug;
Step ⑷ is described to be decocted with water, and is the water that adds 10 times of amounts, and decocting number of times is 2 times, each 1 h;
Described concentrated solution precipitate with ethanol condition is that to be sink to concentration of alcohol (percent by volume) be 80% to concentrated solution alcohol;
Described precipitation is to dissolve with the water of 6 times of amounts again;
Step ⑸ is described to be added ethanol acetate and extracts, and is that to add the volume fraction of 7 times of amounts be that 80% alcoholic solution (containing 1% acetic acid) extracts, and extraction time is 2 times, each 1 h;
Described filtrate is to alkalize to pH10 with strong aqua ammonia;
With the equal amounts of chloroform extraction, it is 5 times again;
Step ⑹ is described to be decocted with water, and is the water that adds 10 times of amounts, and decocting number of times is 2 times, each 1 h;
Described concentrated solution precipitate with ethanol condition is that to be sink to concentration of alcohol (percent by volume) be 80% to concentrated solution alcohol;
Described precipitation is to dissolve with the water of 6 times of amounts again.
The technical scheme that completes the 3rd invention task of the present invention is: the application of above-mentioned anti-pulmonary carcinoma Chinese medicine composition in preparing anti-lung-cancer medicament.
The optimization prescription of anti-pulmonary carcinoma Chinese medicine composition provided by the invention, its prescription and compositions proportioning screening process are as follows:
1. on cellular level, detect the inhibitory action of the active component of different proportionings to growth of tumour cell.
Cell strain: people's pulmonary carcinoma A549 and SPC-A-1 cell strain.
At external acellular inhibition proliferation function, so this experiment selects the proportion relation of Ganoderma total triterpenes, Semen Coicis oil and Bulbus Lilii total alkaloids to carry out the optimum ratio prescription due to the polysaccharide component.
The weight portion of known Ganoderma, Semen Coicis and Bulbus Lilii clinical prescription consumption consists of: Ganoderma 10, Semen Coicis 10, Bulbus Lilii 6, and in three flavor medical materials, the extraction ratio of active component is respectively Ganoderma total triterpenes 3.75%, Semen Coicis oil 6.62% and Bulbus Lilii total alkaloids 1.25%.Therefore, take Ganoderma total triterpenes, Semen Coicis oil, 3 kinds of active components of Bulbus Lilii total alkaloids as the influence factor, on original clinical basis with the prescription amount, use equivalent multiplication method (0.5 times, 1 times, 2 times), in conjunction with medical material, active component content, three dosage determining each active component are the level that affects, and adopt L
9(3
4) orthogonal test table carries out experimental design.According to different dosage ratios, be made into different active component groups, selecting two kinds of human lung carcinoma cell lines of A549 and SPC-A-1 is model, by the MTT activity test, detect the inhibitory action of each active component group on cell proliferation, investigate its anti-tumor activity size, with half-inhibition concentration IC
50For index, the best proportioning dosage of final preferred active component.Orthogonal test factor level table and L
9(3
4) orthogonal experiments is in Table 1,2.
Table 1 orthogonal test factor level table
Table 2 L
9(3
4) orthogonal experiments
For ease of orthogonal experiments is carried out to intuitive analysis and variance analysis, therefore introduce a balance index " degree of membership ", to the IC50 standardization, index degree of membership=(index maximum-desired value)/(index maximum-index minima), maximum, minima that wherein index is maximum, minima is respectively survey IC50, the desired value of desired value for calculating.The analysis result of A549 cell in Table 3,5 and the analysis result of SPC-A-1 cell in Table 4,6.
Table 3 L
9(3
4) orthogonal experiments
| Factor Experiment | A | B | C | D | IC 50Degree of membership |
| 1 | 1 | 1 | 1 | 1 | 0.30 |
| 2 | 1 | 2 | 2 | 2 | 0.25 |
| 3 | 1 | 3 | 3 | 3 | 0.00 |
| 4 | 2 | 1 | 2 | 3 | 0.26 |
| 5 | 2 | 2 | 3 | 1 | 0.01 |
| 6 | 2 | 3 | 1 | 2 | 1.00 |
| 7 | 3 | 1 | 3 | 2 | 0.23 |
| 8 | 3 | 2 | 1 | 3 | 0.98 |
| 9 | 3 | 3 | 2 | 1 | 0.75 |
| k1 | 0.55 | 0.79 | 2.28 | 1.06 | ? |
| k2 | 1.27 | 1.24 | 1.26 | 1.48 | ? |
| k3 | 1.96 | 1.75 | 0.24 | 1.24 | ? |
| k1/3 | 0.18 | 0.26 | 0.76 | 0.35 | ? |
| k2/3 | 0.42 | 0.41 | 0.42 | 0.49 | ? |
| k3/3 | 0.65 | 0.58 | 0.08 | 0.41 | ? |
| R | 0.47 | 0.32 | 0.68 | 0.14 | ? |
Table 4 L
9(3
4) orthogonal experiment data result table
| Factor Experiment | A | B | C | D | IC 50Degree of membership |
| 1 | 1 | 1 | 1 | 1 | 0.23 |
| 2 | 1 | 2 | 2 | 2 | 0.31 |
| 3 | 1 | 3 | 3 | 3 | 0.00 |
| 4 | 2 | 1 | 2 | 3 | 0.27 |
| 5 | 2 | 2 | 3 | 1 | 0.11 |
| 6 | 2 | 3 | 1 | 2 | 1.00 |
| 7 | 3 | 1 | 3 | 2 | 0.24 |
| 8 | 3 | 2 | 1 | 3 | 0.95 |
| 9 | 3 | 3 | 2 | 1 | 0.84 |
| k1 | 0.54 | 0.74 | 2.18 | 1.18 | ? |
| k2 | 1.38 | 1.37 | 1.42 | 1.55 | ? |
| k3 | 2.03 | 1.84 | 0.35 | 1.22 | ? |
| k1/3 | 0.18 | 0.25 | 0.73 | 0.39 | ? |
| k2/3 | 0.46 | 0.46 | 0.47 | 0.52 | ? |
| k3/3 | 0.68 | 0.61 | 0.12 | 0.41 | ? |
| R | 0.50 | 0.37 | 0.61 | 0.12 | ? |
Table 5 analysis of variance table
| Soruces of variation | Sum of deviation square | Degree of freedom | Mean square | F | Significance |
| A | 0.33 | 2.000 | 0.166 | 11.196 | 0.082 |
| B | 0.15 | 2.000 | 0.077 | 5.196 | 0.161 |
| C | 0.69 | 2.000 | 0.347 | 23.432 | 0.041 |
| Error | 0.03 | 2.000 | 0.015 | ? | ? |
Annotate: F
(0.05 2,2)=19.00
Table 6 analysis of variance table
| Soruces of variation | Sum of deviation square | Degree of freedom | Mean square | F | Significance |
| A | 0.37 | 2.000 | 0.186 | 13.534 | 0.069 |
| B | 0.20 | 2.000 | 0.102 | 7.388 | 0.119 |
| C | 0.56 | 2.000 | 0.282 | 20.499 | 0.047 |
| Error | 0.03 | 2.000 | 0.014 | ? | ? |
Annotate: F
(0.05 2,2)=19.00
Comprehensive A549 and SPC-A-1 cell experiment result, can find out according to directly perceived and variance analysis, to half-inhibition concentration IC
50The factor that has the greatest impact is C(Bulbus Lilii total alkaloids), be secondly the A factor, B affects minimum, and optimum combination is A
3B
3C
1, namely Bulbus Lilii total alkaloids size of shared weight portion in compositions has a strong impact on the anti-tumor activity size of said composition, and its proportion is larger, its IC
50Larger.Therefore, in this antitumor Chinese, the best proportioning of Ganoderma total triterpenes, Semen Coicis oil, Bulbus Lilii total alkaloids is 750 mg: 1324 mg: 37.5 mg, namely the best compatibility consumption of crude drug is (weight ratio): Ganoderma 20 weight portions, Semen Coicis 20 weight portions, Bulbus Lilii 3 weight portions.
In vivo on animal model the antitumor action to each active component and compatibility component thereof carry out evaluating drug effect.
It is 1 * 10 that cell density is transferred to
7The Lewis cell suspension inoculation of individual/mL is subcutaneous in the right armpit of C57BL/6 mice, every 0.2 mL.Next day after inoculation, weigh, random packet, 8 every group.Administering mode: gastric infusion.blank group: normal saline, every day 0.4 mL/ time, positive controls: cyclophosphamide (20 mgg
-1d
-1), every day 0.2 mL/ time, medicine group: Ganoderma total triterpenes, Semen Coicis oil, the Bulbus Lilii total alkaloids, Ganoderma total triterpenes+Semen Coicis oil (in the combination of crude drug amount 1:1 ratio), Ganoderma total triterpenes+Semen Coicis oil+Bulbus Lilii total alkaloids (in the combination of crude drug amount 20:20:3 ratio), Ganoderma total triterpenes+Semen Coicis oil+Bulbus Lilii total alkaloids+ganoderan, coixan and Bulbus Lilii polysaccharide (make up in crude drug amount 20:20:3 ratio, ganoderan wherein, coixan and Bulbus Lilii polysaccharide are by its crude drug and Ganoderma total triterpenes, Semen Coicis oil, Bulbus Lilii total alkaloids crude drug crude drug amount 1:1 weight ratio adds), all establish high low dose group (high dose: the total crude drug kg of 30 g
-1d
-1, low dosage: the total crude drug kg of 15 g
-1d
-1), every day 0.4 mL/ time, continuous 14 d.Drug withdrawal next day, weigh, pull out eyeball and get blood, blood sample is in centrifugal 5 min of 5000 rpm, and-20 ℃ of freezing saving backup, take off neck and put to death mice, peels off oxter tumor, liver, Thymus and spleen.Calculate tumour inhibiting rate, liver index, thymus index and spleen index, the content of TNF-α and IL-6 in the mensuration mice plasma.The results are shown in Table 7,8,9.
The average tumor of tumour inhibiting rate (%)=(the average tumor weight of the average tumor weight-administration of model group group)/model group heavy * 100%
Liver index=liver weight (mg)/Mouse Weight (g)
Thymus index=thymic weight (mg)/Mouse Weight (g)
Spleen index=spleen weight (mg)/Mouse Weight (g)
Table 7 active component and compatibility component thereof to the inhibitory action of Lewis tumor-bearing mice tumor (
±
S,
n=8)
Annotate: * compares (* p<0.05) for each group and normal saline group
Result shows with the normal saline group and compares, except Bulbus Lilii total alkaloids low dose group, the resulting Ganoderma total triterpenes of the present invention and the high low dose group of Semen Coicis oil, Bulbus Lilii total alkaloids high dose group and each active component compositions all have inhibitory action to the growth of Lewis tumor in body.Ganoderma total triterpenes, after Semen Coicis oil and the administration of Bulbus Lilii total alkaloids compatibility, its anti-tumor activity is better than one-component (p<0.05), and with Ganoderma total triterpenes, Semen Coicis oil, Bulbus Lilii total alkaloids and ganoderan, coixan, after the administration of Bulbus Lilii polysaccharide compositions, tumour inhibiting rate is the highest, reach 55.13%, tumour inhibiting rate than the Chinese medicine of present national approved ginseng stilbene PINGXIAO JIA0NANG (suppression ratio to transplantability Lewis lung cancer tumor is 42.18%) is high, illustrate and adopt the modern separation means of extracting that the active component in this pharmaceutical composition is farthest extracted and separates and compatibility, can bring into play better the synergistic antitumor effect.
Table 8 active component and compatibility component thereof on the impact of Lewis tumor-bearing mice immune organ (
±
S,
n=8)
Annotate: * compares (* p<0.05) for each group and normal saline group; # compares (# p<0.05) for each group and cyclophosphamide group
Result shows, with the normal saline group, compares, and liver index, spleen index, the thymus index of cyclophosphamide administration group mice all have certain reduction, may to the mouse immune system, have inhibitory action to cause due to cyclophosphamide.With cyclophosphamide administration group, compare the animal immune index of Ganoderma total triterpenes high dose group, Semen Coicis oil high dose group and each compositions high dose group of active component be improved (p<0.05).After Ganoderma total triterpenes, Semen Coicis oil, the administration of Bulbus Lilii total alkaloids compatibility, with the one-component administration, compare, liver index, spleen index and the thymus index of mice all has significance to increase (p<0.05).After the Ganoderma total triterpenes that the present invention obtains, Semen Coicis oil, Bulbus Lilii total alkaloids and the administration of polysaccharide compositions, with the cyclophosphamide positive controls, compare, liver index, spleen index and the thymus index of mice all has significance to increase (P<0.05), illustrate that the compositions that the present invention obtains can pass through the enhancing human body immunity activity, and the performance antitumor action.
Table 9 active component and compatibility component thereof to TNF-a in Lewis tumor-bearing mice blood plasma and
The comparison of IL-6 content (
±
S,
n=8)
Annotate: * compares (* p<0.05) for each group and normal saline group; # compares (# p<0.05) for each group and cyclophosphamide group
Result shows, with the normal saline group, compares, and TNF-a and the IL-6 content of cyclophosphamide administration group significantly reduce, and may to the mouse immune system, have inhibitory action to cause due to cyclophosphamide; With the cyclophosphamide positive controls, compare, after the Ganoderma total triterpenes that the present invention obtains, Semen Coicis oil, Bulbus Lilii total alkaloids and the administration of polysaccharide compositions, the TNF-a in mice plasma and the content of IL-6 all have significance to increase (P<0.05).Illustrate that the compositions that the present invention obtains all has regulating action to tumor-bearing mice cells in vivo factor TNF-a and IL-6, can strengthen antitumor action by the activity that improves the immunity of organism factor.
Chinese medicine composition of the present invention extracts purification effectively by the fat-soluble active component in medical material and polysaccharide component, and the extraction preparation method that adopts is suitable for, and industry is large produces.By the reasonable compatibility between component, anti-pulmonary carcinoma experiment is foundation take inside and outside, final best prescription and the best proportioning dosage of compositions of determining that anti-tumor activity is the strongest, make the anti-lung cancer activity of the Chinese medicine composition that the present invention obtains apparently higher than one-component, fully demonstrated treatment advantage and the characteristic of the anti-pulmonary carcinoma of Chinese medicine compound " multicomponent, multipath, many target spots ".
The specific embodiment
Embodiment 1, anti-pulmonary carcinoma Chinese medicine composition, and the weight portion of crude drug is composed as follows: 20 parts of step ⑴ Ganodermas, 20 parts of Semen Coiciss, 3 parts of Bulbus Liliies.Ganoderma sporophore is pulverized and sieved, adopt supercritical CO
2Extraction extracts Ganoderma total triterpenes class component, and extracting pressure is 30 MPa, and extraction temperature is 45 ℃; Extraction time is 1.5 h, and entrainer (95% ethanol) consumption is 3 mLg
-1Crude drug.Step ⑵: Ganoderma coarse powder residue, add the decocting of 10 times of amounts to boil, decocting number of times is 2 times, each 1 h; Filtrate is concentrated, and it is 80% that concentrated solution alcohol is sink to concentration of alcohol (percent by volume); Collecting precipitation, precipitation is dissolved with the water of 6 times of amounts again; Except insoluble impuritiess such as deproteinizes, concentrate drying, finally obtain ganoderan class component.Step ⑶: Semen Coicis is pulverized and sieved, adopt supercritical CO
2Extraction extracts Semen Coicis oil, and extracting pressure is 22MPa, and extraction temperature is 38 ℃; Extraction time is 2.5 h, and entrainer (95% ethanol) consumption is 3 mLg
-1Crude drug; Step ⑷: Semen Coicis coarse powder residue, add the decocting of 10 times of amounts to boil, decocting number of times is 2 times, each 1 h; Filtrate is concentrated, and it is 80% that concentrated solution alcohol is sink to concentration of alcohol (percent by volume); Collecting precipitation, precipitation is dissolved with the water of 6 times of amounts again; Except insoluble impuritiess such as deproteinizes, concentrate drying, finally obtain coixan class component.Step ⑸: Bulbus Lilii is pulverized and sieved, the volume fraction that adds 7 times of amounts is 80% alcoholic solution (containing 1% acetic acid) extraction, extraction time is 2 times, each 1 h, reclaim ethanol, reclaims liquid and alkalize to pH10 with strong aqua ammonia, again with equal amounts of chloroform extraction 5 times, reclaim chloroform, drying, obtain Bulbus Lilii total alkaloids class component.Step ⑹: Bulbus Lilii coarse powder residue, add the decocting of 10 times of amounts to boil, decocting number of times is 2 times, each 1 h; Filtrate is concentrated, and it is 80% that concentrated solution alcohol is sink to concentration of alcohol (percent by volume); Collecting precipitation, precipitation is dissolved with the water of 6 times of amounts again, and except insoluble impuritiess such as deproteinizes, concentrate drying, finally obtain Bulbus Lilii polysaccharide class component.Step ⑺: by the component mix homogeneously that above each step obtains, obtain described anti-pulmonary carcinoma Chinese medicine composition.Said composition is used for the treatment of pulmonary carcinoma.It is 1 * 10 that cell density is transferred to
7The Lewis cell suspension inoculation of individual/mL is subcutaneous in the right armpit of C57BL/6 mice, every 0.2 mL.Next day after inoculation, weigh, random packet, 8 every group.Administering mode: gastric infusion.Blank group: normal saline, every day 0.4 mL/ time; Positive controls: cyclophosphamide (20 mgg
-1D
-1), every day 0.2 mL/ time; Medicine group: the Chinese medicine composition of the Ganoderma total triterpenes that the present invention obtains, Semen Coicis oil, Bulbus Lilii total alkaloids, ganoderan, coixan and Bulbus Lilii polysaccharide, dosage: high dose 30 g crude drug kg
-1D
-1, low dosage 15 g crude drug kg
-1D
-1, every day 0.4 mL/ time, continuous 14 d.Drug withdrawal next day, weigh, pull out eyeball and get blood, blood sample is in centrifugal 5 min of 5000 rpm, and-20 ℃ of freezing saving backup, take off neck and put to death mice, peels off oxter tumor, liver, Thymus and spleen.Calculate tumour inhibiting rate, liver index, thymus index and spleen index, the content of TNF-α and IL-6 in the mensuration mice plasma.The average tumor of tumour inhibiting rate (%)=(the average tumor weight of the average tumor weight-administration of model group group)/model group heavy * 100%; Liver index=liver weight (mg)/Mouse Weight (g); Thymus index=thymic weight (mg)/Mouse Weight (g); Spleen index=spleen weight (mg)/Mouse Weight (g).
The experimental result demonstration, the tumor weight of this Chinese medicine composition high and low dose group is starkly lower than the normal saline group, and tumour inhibiting rate is respectively 55.13%, 40.77%, with other administration groups, compares, and tumour inhibiting rate has significance to improve (P<0.05).With the normal saline group, compare, liver index, thymus index and the spleen index of this Chinese medicine composition high and low dose group are improved; With positive controls, compare, liver index, thymus index and the spleen index of this Chinese medicine composition high and low dose group all has significance to increase (P<0.05).With normal saline group and cyclophosphamide group, compare, the TNF-a in the mice plasma of this Chinese medicine composition high and low dose group and the content of IL-6 all have significance to increase (P<0.05).
Embodiment 2, and is substantially the same manner as Example 1, but following change is arranged, and the weight portion of crude drug is composed as follows: 5 parts of Ganodermas, 5 parts of Semen Coiciss, 1 part of Bulbus Lilii.Simultaneously, the described extraction conditions of step ⑴ is: pressure 25MPa, and extraction temperature is 43 ℃; Extraction time is 1 h, and entrainer (95% ethanol) consumption is 1 mLg
-1Crude drug; Step ⑵ is described to be decocted with water, and is to add the decocting of 8 times of amounts to boil, and decocting number of times is 1 time, each 2 h; Described concentrated solution precipitate with ethanol condition is that to be sink to concentration of alcohol (percent by volume) be 75% to concentrated solution alcohol; Described precipitation is to dissolve with the water of 4 times of amounts again; The described extraction conditions of step ⑶ is: extracting pressure is 20MPa, and extraction temperature is 35 ℃, and extraction time is 2 h, and entrainer (95% ethanol) consumption is 1 mLg
-1Crude drug; Step ⑷ is described to be decocted with water, and is to add the decocting of 8 times of amounts to boil, and decocting number of times is 1 time, each 1 h; Described concentrated solution precipitate with ethanol condition is that to be sink to concentration of alcohol (percent by volume) be 75% to concentrated solution alcohol; Described precipitation is to dissolve with the water of 4 times of amounts again; Step ⑸ is described to be added ethanol acetate and extracts, and is that to add the volume fraction of 8 times of amounts be that 70% alcoholic solution (containing 1% acetic acid) extracts, and extraction time is 1 time, each 2 h; Described recovery liquid is to alkalize to pH9 with strong aqua ammonia; With the equal amounts of chloroform extraction, it is 3 times again; Step ⑹ is described to be decocted with water, and is to add the decocting of 8 times of amounts to boil, and decocting number of times is 1 time, each 1 h; Described concentrated solution precipitate with ethanol condition is that to be sink to concentration of alcohol (percent by volume) be 75% to concentrated solution alcohol; Described precipitation is that the water of 4 times of amounts dissolves again.
Embodiment 3, and is substantially the same manner as Example 1, but following change is arranged, and the weight portion of crude drug is composed as follows: 40 parts of Ganodermas, 40 parts of Semen Coiciss, 10 parts of Bulbus Liliies.Simultaneously, the described extraction conditions of step ⑴ is: pressure 35MPa, and extraction temperature is 48 ℃; Extraction time is 2 h, and entrainer (95% ethanol) consumption is 2 mLg
-1Crude drug; Step ⑵ is described to be decocted with water, and is to add the decocting of 13 times of amounts to boil, and decocting number of times is 2 times, each 2 h; Described concentrated solution precipitate with ethanol condition is that to be sink to concentration of alcohol (percent by volume) be 85% to concentrated solution alcohol; Described precipitation is to dissolve with the water of 10 times of amounts again; The described extraction conditions of step ⑶ is: extracting pressure is 25MPa, and extraction temperature is 40 ℃, and extraction time is 3 h, and entrainer (95% ethanol) consumption is 2 mLg
-1Crude drug; Step ⑷ is described to be decocted with water, and is to add the decocting of 13 times of amounts to boil, and decocting number of times is 2 times, each 2 h; Described concentrated solution precipitate with ethanol condition is that to be sink to concentration of alcohol (percent by volume) be 85% to concentrated solution alcohol; Described precipitation is to dissolve with the water of 10 times of amounts again; Step ⑸ is described to be added ethanol acetate and extracts, and is that to add the volume fraction of 9 times of amounts be that 85% alcoholic solution (containing 1% acetic acid) extracts, and extraction time is 2 times, each 2 h; Described recovery liquid is to alkalize to pH10 with strong aqua ammonia; With the equal amounts of chloroform extraction, it is 7 times again; Step ⑹ is described to be decocted with water, and is to add the decocting of 13 times of amounts to boil, and decocting number of times is 2 times, each 2 h; Described concentrated solution precipitate with ethanol condition is that to be sink to concentration of alcohol (percent by volume) be 85% to concentrated solution alcohol; Described precipitation is that the water of 10 times of amounts dissolves again.
Embodiment 4, and is substantially the same manner as Example 1, but following change is arranged, and the weight portion of crude drug is composed as follows: 5 parts of Ganodermas, 40 parts of Semen Coiciss, 1 part of Bulbus Lilii.Simultaneously, the described extraction conditions of step ⑴ is: pressure 35MPa, and extraction temperature is 43 ℃; Extraction time is 2 h, and entrainer (95% ethanol) consumption is 2 mLg
-1Crude drug; Step ⑵ is described to be decocted with water, and is to add the decocting of 11 times of amounts to boil, and decocting number of times is 2 times, each 1 h; Described concentrated solution precipitate with ethanol condition is that to be sink to concentration of alcohol (percent by volume) be 85% to concentrated solution alcohol; Described precipitation is to dissolve with the water of 5 times of amounts again; The described extraction conditions of step ⑶ is: extracting pressure is 25MPa, and extraction temperature is 35 ℃, and extraction time is 3 h, and entrainer (95% ethanol) consumption is 2 mLg
-1Crude drug; Step ⑷ is described to be decocted with water, and is to add the decocting of 11 times of amounts to boil, and decocting number of times is 2 times, each 1 h; Described concentrated solution precipitate with ethanol condition is that to be sink to concentration of alcohol (percent by volume) be 85% to concentrated solution alcohol; Described precipitation is to dissolve with the water of 5 times of amounts again; Step ⑸ is described to be added ethanol acetate and extracts, and is that to add the volume fraction of 8 times of amounts be that 85% alcoholic solution (containing 1% acetic acid) extracts, and extraction time is 2 times, each 1 h; Described recovery liquid is to alkalize to pH9 with strong aqua ammonia; With the equal amounts of chloroform extraction, it is 7 times again; Step ⑹ is described to be decocted with water, and is to add the decocting of 11 times of amounts to boil, and decocting number of times is 2 times, each 1 h; Described concentrated solution precipitate with ethanol condition is that to be sink to concentration of alcohol (percent by volume) be 85% to concentrated solution alcohol; Described precipitation is that the water of 5 times of amounts dissolves again.
Embodiment 5, and is substantially the same manner as Example 1, but following change is arranged, and the weight portion of crude drug is composed as follows: 40 parts of Ganodermas, 5 parts of Semen Coiciss, 10 parts of Bulbus Liliies.Simultaneously, the described extraction conditions of step ⑴ is: pressure 25MPa, and extraction temperature is 48 ℃; Extraction time is 1 h, and entrainer (95% ethanol) consumption is 1 mLg
-1Crude drug; Step ⑵ is described to be decocted with water, and is to add the decocting of 13 times of amounts to boil, and decocting number of times is 1 time, each 2 h; Described concentrated solution precipitate with ethanol condition is that to be sink to concentration of alcohol (percent by volume) be 75% to concentrated solution alcohol; Described precipitation is to dissolve with the water of 7 times of amounts again; The described extraction conditions of step ⑶ is: extracting pressure is 20MPa, and extraction temperature is 40 ℃, and extraction time is 2 h, and entrainer (95% ethanol) consumption is 1 mLg
-1Crude drug; Step ⑷ is described to be decocted with water, and is to add the decocting of 13 times of amounts to boil, and decocting number of times is 1 time, each 2 h; Described concentrated solution precipitate with ethanol condition is that to be sink to concentration of alcohol (percent by volume) be 75% to concentrated solution alcohol; Described precipitation is to dissolve with the water of 7 times of amounts again; Step ⑸ is described to be added ethanol acetate and extracts, and is that to add the volume fraction of 6 times of amounts be that 75% alcoholic solution (containing 1% acetic acid) extracts, and extraction time is 1 time, each 2 h; Described recovery liquid is to alkalize to pH10 with strong aqua ammonia; With the equal amounts of chloroform extraction, it is 3 times again; Step ⑹ is described to be decocted with water, and is to add the decocting of 13 times of amounts to boil, and decocting number of times is 1 time, each 2 h; Described concentrated solution precipitate with ethanol condition is that to be sink to concentration of alcohol (percent by volume) be 75% to concentrated solution alcohol; Described precipitation is that the water of 7 times of amounts dissolves again.
Embodiment 6, and is substantially the same manner as Example 1, but following change is arranged, and the weight portion of crude drug is composed as follows: 10 parts of Ganodermas, 10 parts of Semen Coiciss, 1 part of Bulbus Lilii.The described extraction conditions of step ⑴ is: pressure 20MPa, and extraction temperature is 40 ℃; Extraction time is 1 h, and entrainer (95% ethanol) consumption is 1 mLg
-1Crude drug; Step ⑵ is described to be decocted with water, and is to add the decocting of 8 times of amounts to boil, and decocting number of times is 1 time, each 1 h; Described concentrated solution precipitate with ethanol condition is that to be sink to concentration of alcohol (percent by volume) be 60% to concentrated solution alcohol; Described precipitation is to dissolve with the water of 4 times of amounts again; The described extraction conditions of step ⑶ is: extracting pressure is 15MPa, and extraction temperature is 30 ℃, and extraction time is 1 h, and entrainer (95% ethanol) consumption is 1 mLg
-1Crude drug; Step ⑷ is described to be decocted with water, and is to add the decocting of 8 times of amounts to boil, and decocting number of times is 1 time, each 1 h; Described concentrated solution precipitate with ethanol condition is that to be sink to concentration of alcohol (percent by volume) be 60% to concentrated solution alcohol; Described precipitation is to dissolve with the water of 4 times of amounts again; Step ⑸ is described to be added ethanol acetate and extracts, and is that to add the volume fraction of 5 times of amounts be that 70% alcoholic solution (containing 1% acetic acid) extracts, and extraction time is 1 time, each 1 h; Described recovery liquid is to alkalize to pH8 with strong aqua ammonia; With the equal amounts of chloroform extraction, it is 2 times again; Step ⑹ is described to be decocted with water, and is to add the decocting of 8 times of amounts to boil, and decocting number of times is 1 time, each 1 h; Described concentrated solution precipitate with ethanol condition is that to be sink to concentration of alcohol (percent by volume) be 60% to concentrated solution alcohol; Described precipitation is that the water of 4 times of amounts dissolves again.
Embodiment 7, and is substantially the same manner as Example 1, but following change is arranged, and the weight portion of crude drug is composed as follows: 30 parts of Ganodermas, 30 parts of Semen Coiciss, 6 parts of Bulbus Liliies.The described extraction conditions of step ⑴ is: pressure 40MPa, and extraction temperature is 50 ℃; Extraction time is 3 h, and entrainer (95% ethanol) consumption is 4 mLg
-1Crude drug; Step ⑵ is described to be decocted with water, and is to add the decocting of 14 times of amounts to boil, and decocting number of times is 3 times, each 3 h; Described concentrated solution precipitate with ethanol condition is that to be sink to concentration of alcohol (percent by volume) be 90% to concentrated solution alcohol; Described precipitation is to dissolve with the water of 10 times of amounts again; The described extraction conditions of step ⑶ is: extracting pressure is 25MPa, and extraction temperature is 40 ℃, and extraction time is 3 h, and entrainer (95% ethanol) consumption is 4 mLg
-1Crude drug; Step ⑷ is described to be decocted with water, and is to add the decocting of 14 times of amounts to boil, and decocting number of times is 3 times, each 3 h; Described concentrated solution precipitate with ethanol condition is that to be sink to concentration of alcohol (percent by volume) be 90% to concentrated solution alcohol; Described precipitation is to dissolve with the water of 10 times of amounts again; Step ⑸ is described to be added ethanol acetate and extracts, and is that to add the volume fraction of 10 times of amounts be that 90% alcoholic solution (containing 1% acetic acid) extracts, and extraction time is 3 times, each 3 h; Described recovery liquid is to alkalize to pH11 with strong aqua ammonia; With the equal amounts of chloroform extraction, it is 8 times again; Step ⑹ is described to be decocted with water, and is to add the decocting of 14 times of amounts to boil, and decocting number of times is 3 times, each 3 h; Described concentrated solution precipitate with ethanol condition is that to be sink to concentration of alcohol (percent by volume) be 90% to concentrated solution alcohol; Described precipitation is that the water of 10 times of amounts dissolves again.
Embodiment 8, and is substantially the same manner as Example 1, but following change is arranged, and the weight portion of crude drug is composed as follows: 10 parts of Ganodermas, 30 parts of Semen Coiciss, 1 part of Bulbus Lilii.The described extraction conditions of step ⑴ is: pressure 40MPa, and extraction temperature is 40 ℃; Extraction time is 3 h, and entrainer (95% ethanol) consumption is 3 mLg
-1Crude drug; Step ⑵ is described to be decocted with water, and is to add the decocting of 9 times of amounts to boil, and decocting number of times is 3 times, each 1 h; Described concentrated solution precipitate with ethanol condition is that to be sink to concentration of alcohol (percent by volume) be 90% to concentrated solution alcohol; Described precipitation is to dissolve with the water of 6 times of amounts again; The described extraction conditions of step ⑶ is: extracting pressure is 25MPa, and extraction temperature is 30 ℃, and extraction time is 3 h, and entrainer (95% ethanol) consumption is 3 mLg
-1Crude drug; Step ⑷ is described to be decocted with water, and is to add the decocting of 9 times of amounts to boil, and decocting number of times is 3 times, each 1 h; Described concentrated solution precipitate with ethanol condition is that to be sink to concentration of alcohol (percent by volume) be 90% to concentrated solution alcohol; Described precipitation is to dissolve with the water of 6 times of amounts again; Step ⑸ is described to be added ethanol acetate and extracts, and is that to add the volume fraction of 7 times of amounts be that 90% alcoholic solution (containing 1% acetic acid) extracts, and extraction time is 3 times, each 1 h; Described recovery liquid is to alkalize to pH8 with strong aqua ammonia; With the equal amounts of chloroform extraction, it is 8 times again; Step ⑹ is described to be decocted with water, and is to add the decocting of 9 times of amounts to boil, and decocting number of times is 3 times, each 1 h; Described concentrated solution precipitate with ethanol condition is that to be sink to concentration of alcohol (percent by volume) be 90% to concentrated solution alcohol; Described precipitation is that the water of 6 times of amounts dissolves again.
Embodiment 9, and is substantially the same manner as Example 1, but following change is arranged, and the weight portion of crude drug is composed as follows: 30 parts of Ganodermas, 10 parts of Semen Coiciss, 6 parts of Bulbus Liliies.The described extraction conditions of step ⑴ is: pressure 20MPa, and extraction temperature is 50 ℃; Extraction time is 1 h, and entrainer (95% ethanol) consumption is 2 mLg
-1Crude drug; Step ⑵ is described to be decocted with water, and is to add the decocting of 14 times of amounts to boil, and decocting number of times is 1 time, each 3 h; Described concentrated solution precipitate with ethanol condition is that to be sink to concentration of alcohol (percent by volume) be 60% to concentrated solution alcohol; Described precipitation is to dissolve with the water of 9 times of amounts again; The described extraction conditions of step ⑶ is: extracting pressure is 15MPa, and extraction temperature is 40 ℃, and extraction time is 1 h, and entrainer (95% ethanol) consumption is 2 mLg
-1Crude drug; Step ⑷ is described to be decocted with water, and is to add the decocting of 14 times of amounts to boil, and decocting number of times is 1 time, each 3 h; Described concentrated solution precipitate with ethanol condition is that to be sink to concentration of alcohol (percent by volume) be 60% to concentrated solution alcohol; Described precipitation is to dissolve with the water of 9 times of amounts again; Step ⑸ is described to be added ethanol acetate and extracts, and is that to add the volume fraction of 10 times of amounts be that 90% alcoholic solution (containing 1% acetic acid) extracts, and extraction time is 1 time, each 3 h; Described recovery liquid is to alkalize to pH11 with strong aqua ammonia; With the equal amounts of chloroform extraction, it is 2 times again; Step ⑹ is described to be decocted with water, and is to add the decocting of 14 times of amounts to boil, and decocting number of times is 1 time, each 3 h; Described concentrated solution precipitate with ethanol condition is that to be sink to concentration of alcohol (percent by volume) be 60% to concentrated solution alcohol; Described precipitation is that the water of 9 times of amounts dissolves again.
Embodiment 10, and is substantially the same manner as Example 1, but following change is arranged, and the weight portion of crude drug is composed as follows: 5 parts of Ganodermas, 5 parts of Semen Coiciss, 10 parts of Bulbus Liliies.
Embodiment 11, and is substantially the same manner as Example 1, but following change is arranged, and the weight portion of crude drug is composed as follows: 5 parts of Ganodermas, 40 parts of Semen Coiciss, 10 parts of Bulbus Liliies.
Embodiment 12, and is substantially the same manner as Example 1, but following change is arranged, and the weight portion of crude drug is composed as follows: 40 parts of Ganodermas, 5 parts of Semen Coiciss, 1 part of Bulbus Lilii.
Embodiment 13, and is substantially the same manner as Example 1, but following change is arranged, and the weight portion of crude drug is composed as follows: 40 parts of Ganodermas, 40 parts of Semen Coiciss, 1 part of Bulbus Lilii.
Embodiment 14, and is substantially the same manner as Example 1, but following change is arranged, and the weight portion of crude drug is composed as follows: 30 parts of Ganodermas, 30 parts of Semen Coiciss, 1 part of Bulbus Lilii.
Embodiment 15, and is substantially the same manner as Example 1, but following change is arranged, and the weight portion of crude drug is composed as follows: 10 parts of Ganodermas, 30 parts of Semen Coiciss, 6 parts of Bulbus Liliies.
Embodiment 16, and is substantially the same manner as Example 1, but following change is arranged, and the weight portion of crude drug is composed as follows: 10 parts of Ganodermas, 10 parts of Semen Coiciss, 6 parts of Bulbus Liliies.
Embodiment 17, and is substantially the same manner as Example 1, but following change is arranged, and the weight portion of crude drug is composed as follows: 30 parts of Ganodermas, 10 parts of Semen Coiciss, 1 part of Bulbus Lilii.
Embodiment 18, and is substantially the same manner as Example 1, but following change is arranged, and wherein, the weight portion of Ganoderma total triterpenes, Semen Coicis oil, Bulbus Lilii total alkaloids consists of: Ganoderma total triterpenes 1, Semen Coicis oil 1, Bulbus Lilii total alkaloids 1; Ganoderan wherein, coixan and Bulbus Lilii polysaccharide are to add by its crude drug and Ganoderma total triterpenes, Semen Coicis oil, crude drug amount 1:1 weight ratio that the Bulbus Lilii total alkaloids is identical.
Embodiment 19, and is substantially the same manner as Example 1, but following change is arranged, and wherein, the weight portion of Ganoderma total triterpenes, Semen Coicis oil, Bulbus Lilii total alkaloids consists of: Ganoderma total triterpenes 20, Semen Coicis oil 35, Bulbus Lilii total alkaloids 10; Ganoderan wherein, coixan and Bulbus Lilii polysaccharide are to add by its crude drug and Ganoderma total triterpenes, Semen Coicis oil, crude drug amount 1:1 weight ratio that the Bulbus Lilii total alkaloids is identical.
Embodiment 20, and is substantially the same manner as Example 1, but following change is arranged, and wherein, the weight portion of Ganoderma total triterpenes, Semen Coicis oil, Bulbus Lilii total alkaloids consists of: Ganoderma total triterpenes 1, Semen Coicis oil 35, Bulbus Lilii total alkaloids 1; Ganoderan wherein, coixan and Bulbus Lilii polysaccharide are to add by its crude drug and Ganoderma total triterpenes, Semen Coicis oil, crude drug amount 1:1 weight ratio that the Bulbus Lilii total alkaloids is identical.
Embodiment 21, and is substantially the same manner as Example 1, but following change is arranged, and wherein, the weight portion of Ganoderma total triterpenes, Semen Coicis oil, Bulbus Lilii total alkaloids consists of: Ganoderma total triterpenes 1, Semen Coicis oil 1, Bulbus Lilii total alkaloids 10; Ganoderan wherein, coixan and Bulbus Lilii polysaccharide are to add by its crude drug and Ganoderma total triterpenes, Semen Coicis oil, crude drug amount 1:1 weight ratio that the Bulbus Lilii total alkaloids is identical.
Embodiment 22, and is substantially the same manner as Example 1, but following change is arranged, and wherein, the weight portion of Ganoderma total triterpenes, Semen Coicis oil, Bulbus Lilii total alkaloids consists of: Ganoderma total triterpenes 20, Semen Coicis oil 1, Bulbus Lilii total alkaloids 1; Ganoderan wherein, coixan and Bulbus Lilii polysaccharide are to add by its crude drug and Ganoderma total triterpenes, Semen Coicis oil, crude drug amount 1:1 weight ratio that the Bulbus Lilii total alkaloids is identical.
Embodiment 23, and is substantially the same manner as Example 1, but following change is arranged, and wherein, the weight portion of Ganoderma total triterpenes, Semen Coicis oil, Bulbus Lilii total alkaloids consists of: Ganoderma total triterpenes 20, Semen Coicis oil 35, Bulbus Lilii total alkaloids 1; Ganoderan wherein, coixan and Bulbus Lilii polysaccharide are to add by its crude drug and Ganoderma total triterpenes, Semen Coicis oil, crude drug amount 1:1 weight ratio that the Bulbus Lilii total alkaloids is identical.
Embodiment 24, and is substantially the same manner as Example 1, but following change is arranged, and wherein, the weight portion of Ganoderma total triterpenes, Semen Coicis oil, Bulbus Lilii total alkaloids consists of: Ganoderma total triterpenes 20, Semen Coicis oil 1, Bulbus Lilii total alkaloids 10; Ganoderan wherein, coixan and Bulbus Lilii polysaccharide are to add by its crude drug and Ganoderma total triterpenes, Semen Coicis oil, crude drug amount 1:1 weight ratio that the Bulbus Lilii total alkaloids is identical.
Embodiment 25, and is substantially the same manner as Example 1, but following change is arranged, and wherein, the weight portion of Ganoderma total triterpenes, Semen Coicis oil, Bulbus Lilii total alkaloids consists of: Ganoderma total triterpenes 1, Semen Coicis oil 35, Bulbus Lilii total alkaloids 10; Ganoderan wherein, coixan and Bulbus Lilii polysaccharide are to add by its crude drug and Ganoderma total triterpenes, Semen Coicis oil, crude drug amount 1:1 weight ratio that the Bulbus Lilii total alkaloids is identical.
Embodiment 26, and is substantially the same manner as Example 1, but following change is arranged, and the weight ratio of described Ganoderma total triterpenes, Semen Coicis oil, Bulbus Lilii total alkaloids, ganoderan, coixan and Bulbus Lilii polysaccharide is 20:35:1:35:45:4.
Embodiment 27, and is substantially the same manner as Example 1, but following change is arranged, and the weight ratio of described Ganoderma total triterpenes, Semen Coicis oil, Bulbus Lilii total alkaloids, ganoderan, coixan and Bulbus Lilii polysaccharide is 18:33:1:33:43:3.
Embodiment 28, and is substantially the same manner as Example 1, but following change is arranged, and the weight ratio of described Ganoderma total triterpenes, Semen Coicis oil, Bulbus Lilii total alkaloids, ganoderan, coixan and Bulbus Lilii polysaccharide is 22:37:1:37:47:5.
Embodiment 29, and is substantially the same manner as Example 1, but following change is arranged, and the weight ratio of described Ganoderma total triterpenes, Semen Coicis oil, Bulbus Lilii total alkaloids, ganoderan, coixan and Bulbus Lilii polysaccharide is 18:37:1:33:47:3.
Embodiment 30, and is substantially the same manner as Example 1, but following change is arranged, and the weight ratio of described Ganoderma total triterpenes, Semen Coicis oil, Bulbus Lilii total alkaloids, ganoderan, coixan and Bulbus Lilii polysaccharide is 22:33:1:37:43:5.
Embodiment 31, and is substantially the same manner as Example 1, but following change is arranged, in described compositions wherein the Ganoderma total triterpenes extraction ratio be 3.75%, purity is 61.50%; The Semen Coicis oil extraction ratio is 6.62%, and purity is 74.35%; Bulbus Lilii total alkaloids extraction ratio is 1.25%, and purity is 59.92%; The ganoderan extraction ratio is 6.56%, and purity is 57.70%; The coixan extraction ratio is 8.40%, and purity is 64.42%; The Bulbus Lilii polysaccharide extraction ratio is 4.84%, and purity is 62.53%.
Claims (9)
1. an anti-pulmonary carcinoma Chinese medicine composition, is characterized in that, the weight portion of said composition crude drug is composed as follows: Ganoderma 5 ~ 40, Semen Coicis 5 ~ 40, Bulbus Lilii 1 ~ 10;
Said composition is comprised of Ganoderma total triterpenes, Semen Coicis oil, Bulbus Lilii total alkaloids, ganoderan, coixan and 6 active components of Bulbus Lilii polysaccharide, wherein, the weight portion of Ganoderma total triterpenes, Semen Coicis oil, Bulbus Lilii total alkaloids consists of: Ganoderma total triterpenes 1 ~ 20, Semen Coicis oil 1 ~ 35, Bulbus Lilii total alkaloids 1 ~ 10; Ganoderan wherein, coixan and Bulbus Lilii polysaccharide add by its crude drug and Ganoderma total triterpenes, Semen Coicis oil, Bulbus Lilii total alkaloids crude drug crude drug amount 1:1 weight ratio.
2. anti-pulmonary carcinoma Chinese medicine composition according to claim 1, is characterized in that, the weight portion of described crude drug consists of: Ganoderma 10 ~ 30, Semen Coicis 10 ~ 30, Bulbus Lilii 1 ~ 6.
3. anti-pulmonary carcinoma Chinese medicine composition according to claim 2, is characterized in that, the weight portion of described crude drug consists of: Ganoderma 20, Semen Coicis 20, Bulbus Lilii 3.
4. one of according to claim 1-3 described anti-pulmonary carcinoma Chinese medicine compositions, it is characterized in that, the weight ratio of described Ganoderma total triterpenes, Semen Coicis oil, Bulbus Lilii total alkaloids, ganoderan, coixan and Bulbus Lilii polysaccharide is 18-22:33-37:1:33-37:43-47:3-5.
5. anti-pulmonary carcinoma Chinese medicine composition according to claim 4, is characterized in that, the weight ratio of described Ganoderma total triterpenes, Semen Coicis oil, Bulbus Lilii total alkaloids, ganoderan, coixan and Bulbus Lilii polysaccharide is 20:35:1:35:45:4; Wherein, the Ganoderma total triterpenes extraction ratio is 3.75%, and purity is 61.50%; The Semen Coicis oil extraction ratio is 6.62%, and purity is 74.35%; Bulbus Lilii total alkaloids extraction ratio is 1.25%, and purity is 59.92%; The ganoderan extraction ratio is 6.56%, and purity is 57.70%; The coixan extraction ratio is 8.40%, and purity is 64.42%; The Bulbus Lilii polysaccharide extraction ratio is 4.84%, and purity is 62.53%.
6. the preparation method of the described anti-pulmonary carcinoma Chinese medicine composition of claim 1, is characterized in that, step is as follows:
Step ⑴: Ganoderma sporophore is pulverized and sieved, adopt supercritical CO
2Extraction extracts Ganoderma total triterpenes class component;
Step ⑵: Ganoderma coarse powder residue decocts with water, and filtrate is concentrated, the ethanol precipitation, and collecting precipitation, the precipitation water dissolves again, and except insoluble impuritiess such as deproteinizes, concentrate drying, finally obtain ganoderan class component;
Step ⑶: Semen Coicis is pulverized and sieved, adopt supercritical CO
2Extraction extracts Semen Coicis oil;
Step ⑷: Semen Coicis coarse powder residue decocts with water, and filtrate is concentrated, the ethanol precipitation, and collecting precipitation, the precipitation water dissolves again, and except insoluble impuritiess such as deproteinizes, concentrate drying, finally obtain coixan class component;
Step ⑸: Bulbus Lilii is pulverized and sieved, with acid ethanol solution, extract, reclaim ethanol, reclaim liquid and alkalize with strong aqua ammonia, then use chloroform extraction, reclaim chloroform, drying, obtain Bulbus Lilii total alkaloids class component;
Step ⑹: Bulbus Lilii coarse powder residue decocts with water, and filtrate is concentrated, the ethanol precipitation, and collecting precipitation, the precipitation water dissolves again, and except insoluble impuritiess such as deproteinizes, concentrate drying, finally obtain Bulbus Lilii polysaccharide class component;
Step ⑺: by the component mix homogeneously that above each step obtains, obtain described anti-pulmonary carcinoma Chinese medicine composition.
7. the preparation method of anti-pulmonary carcinoma Chinese medicine composition according to claim 6, is characterized in that, concrete operation step is:
Step ⑴: Ganoderma sporophore is pulverized and sieved, adopt supercritical CO
2Extraction extracts Ganoderma total triterpenes class component, and extracting pressure is 20 ~ 40MPa, and extraction temperature is 40 ~ 50 ℃; Extraction time is 1 ~ 3 h, and entrainer 95% ethanol consumption is 1 ~ 4 mLg
-1Crude drug;
Step ⑵: Ganoderma coarse powder residue, add the decocting of 8 ~ 14 times of amounts to boil, decocting number of times is 1 ~ 3 time, each 1 ~ 3h, and filtrate is concentrated, it is 60 ~ 90% that concentrated solution alcohol is sink to the concentration of alcohol percent by volume, collecting precipitation, precipitation is dissolved with the water of 4 ~ 10 times of amounts again, except insoluble impuritiess such as deproteinizes, concentrate drying, finally obtain ganoderan class component;
Step ⑶: Semen Coicis is pulverized and sieved, adopt supercritical CO
2Extraction extracts Semen Coicis oil, and extracting pressure is 15 ~ 25MPa, and extraction temperature is 30 ~ 40 ℃, and extraction time is 1 ~ 3 h, and entrainer 95% ethanol consumption is 1 ~ 4 mLg
-1Crude drug;
Step ⑷: Semen Coicis coarse powder residue, add the decocting of 8 ~ 14 times of amounts to boil, decocting number of times is 1 ~ 3 time, each 1 ~ 3 h, and filtrate is concentrated, it is 60 ~ 90% that concentrated solution alcohol is sink to the concentration of alcohol percent by volume, collecting precipitation, precipitation is dissolved with the water of 4 ~ 10 times of amounts again, except insoluble impuritiess such as deproteinizes, concentrate drying, finally obtain coixan class component;
Step ⑸: Bulbus Lilii is pulverized and sieved, the volume fraction that adds 5 ~ 10 times of amounts is that 70%-90% the alcoholic solution that contains 1% acetic acid extract, extraction time is 1 ~ 3 time, each 1 ~ 3 h, reclaim ethanol, reclaims liquid and alkalize to pH8 ~ 11 with strong aqua ammonia, again with equal amounts of chloroform extraction 2 ~ 8 times, reclaim chloroform, drying, obtain Bulbus Lilii total alkaloids class component;
Step ⑹: Bulbus Lilii coarse powder residue, add the decocting of 8 ~ 14 times of amounts to boil, decocting number of times is 1 ~ 3 time, each 1 ~ 3 h, and filtrate is concentrated, it is 60 ~ 90% that concentrated solution alcohol is sink to the concentration of alcohol percent by volume, collecting precipitation, precipitation is dissolved with the water of 4 ~ 10 times of amounts again, except insoluble impuritiess such as deproteinizes, concentrate drying, finally obtain Bulbus Lilii polysaccharide class component;
Step ⑺: by the component mix homogeneously that above each step obtains, obtain described anti-pulmonary carcinoma Chinese medicine composition.
8. the preparation method of anti-pulmonary carcinoma Chinese medicine composition according to claim 7, is characterized in that,
The described extraction conditions of step ⑴ is: extracting pressure is 30 MPa, and extraction temperature is 45 ℃; Extraction time is 1.5 h, and entrainer 95% ethanol consumption is 3 mLg
-1Crude drug;
Step ⑵ is described to be decocted with water, and is to add the decocting of 10 times of amounts to boil, and decocting number of times is 2 times, each 1 h;
Described concentrated solution precipitate with ethanol condition is that to be sink to the concentration of alcohol percent by volume be 80% to concentrated solution alcohol;
Described precipitation is to dissolve with the water of 6 times of amounts again;
The described extraction conditions of step ⑶ is: extracting pressure is 22MPa, and extraction temperature is 38 ℃; Extraction time is 2.5 h, and entrainer 95% ethanol consumption is 3 mLg
-1Crude drug;
Step ⑷ is described to be decocted with water, and is to add the decocting of 10 times of amounts to boil, and decocting number of times is 2 times, each 1 h;
Described concentrated solution precipitate with ethanol condition is that to be sink to the concentration of alcohol percent by volume be 80% to concentrated solution alcohol;
Described precipitation is to dissolve with the water of 6 times of amounts again;
Step ⑸ is described to be added ethanol acetate and extracts, be add the volume fraction of 7 times of amounts be 80% and the alcoholic solution that contains 1% acetic acid extract, extraction time is 2 times, each 1 h;
Described recovery liquid is to alkalize to pH10 with strong aqua ammonia;
With the equal amounts of chloroform extraction, it is 5 times again;
Step ⑹ is described to be decocted with water, and is to add the decocting of 10 times of amounts to boil, and decocting number of times is 2 times, each 1 h;
Described concentrated solution precipitate with ethanol condition is that to be sink to the concentration of alcohol percent by volume be 80% to concentrated solution alcohol;
Described precipitation is to dissolve with the water of 6 times of amounts again.
9. the application of anti-pulmonary carcinoma Chinese medicine composition claimed in claim 1 in preparing anti-lung-cancer medicament.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1990032A (en) * | 2005-12-31 | 2007-07-04 | 天津天士力制药股份有限公司 | Composite intravenous injection emulsion of glossy ganoderma spore oil and coix seed oil and method for making same |
| CN101773625A (en) * | 2010-03-03 | 2010-07-14 | 南京中医药大学 | Anticancerogen, preparation method and application thereof |
-
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN101773625A (en) * | 2010-03-03 | 2010-07-14 | 南京中医药大学 | Anticancerogen, preparation method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| 彭程.百合化学成分及其提取方法研究进展.《 西北民族大学学报(自然科学版)》.2011,第32卷(第4期),第11-16页. |
| 百合化学成分及其提取方法研究进展;彭程;《 西北民族大学学报(自然科学版)》;20111231;第32卷(第4期);第11-16页 * |
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