CN1478538A - Chinese medicinal composition for treating prostate cancer, its preparation method and its application in the preparation of medicine for treating prostate cancer - Google Patents

Chinese medicinal composition for treating prostate cancer, its preparation method and its application in the preparation of medicine for treating prostate cancer Download PDF

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CN1478538A
CN1478538A CNA021366551A CN02136655A CN1478538A CN 1478538 A CN1478538 A CN 1478538A CN A021366551 A CNA021366551 A CN A021366551A CN 02136655 A CN02136655 A CN 02136655A CN 1478538 A CN1478538 A CN 1478538A
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extracting
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ethanol
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CN1220519C (en
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杨亿泓
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Shanghai Zhongyao Bio Technology Co ltd
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Shanghai Zhongyao Biological Science & Technology Co Ltd
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Abstract

A Chinese medicine for treating prostatic cancer is preapred from 7 Chinese-medicinal materials including ganoderma, chrysanthemum flower, liquorice root, notoginseng, etc through extracting their active components. Its advantages are high curative effect and low by-effect.

Description

Traditional Chinese medicine composition for treating prostate cancer, preparation method thereof and application thereof in preparation of medicine for treating prostate cancer
(1) Field of the invention
The invention relates to a traditional Chinese medicine composition for treating prostate cancer, a preparation method of the composition and application of the composition in preparing a medicine for treating prostate cancer.
(2) Background of the invention
Prostate cancer is one of the major causes of cancer death in men and can be divided into two types, sex hormone-dependent and non-sex hormone-dependent. Usually only laser irradiation, implantation of radioactive substances or cryosurgery can be performed from the outside. For some patients, these treatments are only "restrictive" for the disease for several years. Most patients receive chemotherapy simultaneously, which can kill cancer cells but also severely damage normal cells in the body, with significant side effects. The effective rate is not ideal enough for treating the sex hormone-dependent prostate cancer by applying the sex hormone; for the non-sex hormone dependent prostate cancer, no specific medicine is available for treatment at present. When patients are diagnosed with stage three or fourth cancer, or with recurrent metastases of prostate cancer, the vast majority of patients are left to die. Therefore, a treatment method with less side effect and convenient treatment is highly required, in other words, a novel medicine with less side effect and high curative effect is highly required, and long-term research by the inventor finds that the treatment purpose can be achieved by one traditional Chinese medicine.
(3) Summary of the invention
One purpose of the invention is to provide a Chinese medicinal composition for treating prostate cancer, which has good curative effect and little side effect;
the invention also aims to provide a preparation method of the traditional Chinese medicine composition;
the invention also aims to provide application of the traditional Chinese medicine composition in preparing a medicine for treating prostatic cancer.
These objects of the invention are achieved by the following idea: the traditional Chinese medicine composition for treating prostate cancer is characterized by being a medicament prepared from the following raw materials in parts by weight:
ganoderma lucidum 3-4
1-2 of scutellaria
Rabdosia rubescens (Hemsl.) Hara 1-2
Folium Isatidis 1-2
0.5-1.5 of chrysanthemum
Radix Glycyrrhizae 0.5-1.5
0.5-1.5 of pseudo-ginseng
The optimal weight ratio of the raw materials is as follows: ganoderma lucidum, Scutellaria baicalensis, Rabdosia rubescens, folium isatidis, chrysanthemum, liquorice and pseudo-ginseng in a ratio of 3: 1.5: 1.2: 0.9.
The best producing place of the scutellaria baicalensis is Sichuan, and the best collection time is autumn; the best producing area of the pseudo-ginseng is Yunnan, and the best collection time is autumn (before blooming); the best producing area of the folium isatidis is south, the best collection time is autumn, the best producing area of the chrysanthemum is Zhejiang, and the best collection time is autumn; the best production place of the rabdosia rubescens is Henan, and the best collection time is May; the Ganoderma is obtained by cultivating/fermenting Ganoderma polysaccharide obtained from Shanghai agricultural family, wherein the Ganoderma polysaccharide contains Ganoderma polypeptide and Ganoderma beta-D-glucan as required active ingredients; the best producing place of licorice is Gansu, and the best collecting time is autumn.
The invention also relates to a preparation method of the traditional Chinese medicine composition, which comprises a mixed extraction preparation method or a target substance extraction preparation method, wherein the mixed extraction preparation method comprises the following steps:
1) preparing raw materials:
mixing the following components: mixing the scutellaria baicalensis, the rabdosia rubescens, the folium isatidis, the chrysanthemum, the liquorice and the panax notoginseng according to the weight ratio of 3-4: 1-2: 0.5-1.5, and preferably further processing the mixture into traditional Chinese medicine coarse powder or traditional Chinese medicine fluid extract, wherein the processing method is well known in the technical field; the mixture is divided into six equal parts;
2) extracting alkaloid:
i) percolating or leaching a part of the Chinese medicinal mixture obtained in step 1) with 0.1% ethanol hydrochloride solution to obtain acidic ethanol extractive solution;
ii) concentrating under reduced pressure to obtain a concentrate;
iii) washing with acidic water (pH 4-5), preferably freezing the acidic aqueous solution overnight in one embodiment, filtering to obtain a residue, and washing the residue with acidic water (pH 4-5) to obtain an acidic aqueous solution;
iv) adding ammonia water into the acidic water solution obtained in the step iii) for precipitation, and filtering to obtain total alkaloid precipitate; or
a) Adding a dilute acid to the acidic aqueous solution obtained in step iii) to a pH of 2, and extracting with chloroform to obtain a chloroform layer and an aqueous layer; evaporating the chloroform in the chloroform layer to obtain weak alkaloid;
b) adding alkali into the water layer until the pH value is 6-7, extracting with chloroform to obtain a water layer and a chloroform layer, and evaporating chloroform in the chloroform layer to obtain strong alkaloid;
c) adjusting the pH of the water layer obtained in b) to 10 with alkali, extracting with butanol, and evaporating butanol in the butanol layer to obtain water-soluble alkaloid;
mixing the alkaloids obtained from a), b) and c) to obtain total alkaloids.
The chloroform and butanol are preferably recovered for recycling in the extraction step. The alkaloid residue is preferably dried at low temperature and crystallized.
3) And (3) extracting polysaccharide:
extracting a part of the Chinese medicinal mixture obtained in step 1) with 95-100 deg.C hot water, preferably for 2 hr, discarding residue, standing the filtrate for 12 hr, adding ethanol with concentration of more than 50% into the supernatant, and centrifuging to obtain polysaccharide precipitate;
the polysaccharide precipitate is preferably refined with diethyl ether.
4) And (3) lactone extraction:
refluxing a portion of the Chinese medicinal mixture obtained in step 1) with diethyl ether, removing the pigment, preferably by polyamide column, recovering the diethyl ether to obtain total lactones;
5) extracting saponin:
refluxing a part of the traditional Chinese medicine mixture obtained in the step 1) with petroleum ether for 2-4 times, evaporating the petroleum ether to obtain degreased coarse powder, extracting with 95% ethanol, and concentrating under reduced pressure to obtain a concentrated solution;
a) sequentially extracting the concentrated solution with chloroform and ethanol, and recovering chloroform and ethanol under reduced pressure to obtain crude product of total glycosides; or
b) Extracting the concentrated solution with butanol to obtain butanol layer, and recovering butanol under reduced pressure to obtain crude product of total glycosides.
6) Extracting the coumarin:
decocting one part of the Chinese medicinal mixture obtained in the step 1) with water for 1-2 hours, concentrating the water decoction, adding concentrated hydrochloric acid (30%), removing impurity insoluble substances, and standing clear liquid to obtain crude crystals of the coumarin; it is preferably dried and washed with acetone, dried, recrystallized by adding water, heated, filtered, and decolorized to obtain an aqueous solution, and cooled to obtain the coumarin as a light yellow paste product.
7) And (3) extracting flavone:
a) soaking a part of the Chinese medicinal mixture obtained in step 1) with 70-80% ethanol, recovering ethanol from ethanol solution under reduced pressure, dissolving the residue with water, and filtering to obtain water solution; extracting the water solution with ethyl acetate, and concentrating the ethyl acetate solution under reduced pressure to obtain total flavonoids.
Mixing the alkaloid extracted in the steps 2) to 7), polysaccharide, lactone, saponin, coumarins and flavone to obtain the traditional Chinese medicine composition for treating prostate cancer.
The method for extracting and preparing the target substance comprises the following steps:
1) extracting baicalin:
i) adding 10 times (volume) of water into the radix Scutellariae components, decocting for 1-2 hr, and filtering;
ii) adjusting the pH of the filtrate to 1-2 with acid, maintaining the temperature at 80-90 deg.C for 30-40 min, and centrifuging to precipitate; adding water into the precipitate, stirring, adding alkali to adjust pH to neutral, adding 3-5 times (volume) of ethanol, and filtering;
iii) adding acid to the filtrate to adjust pH to 1-2, stirring, maintaining at 80-90 deg.C for 30-40 min, and filtering;
iv) washing the obtained precipitate with water and 50% ethanol respectively, and washing with 95% ethanol or recrystallizing to obtain baicalin.
2) Extracting notoginsenoside:
i) extracting soluble components in the coarse powder of radix Notoginseng with methanol with concentration below 50%, concentrating the methanol extractive solution under reduced pressure, and adding 3-5 times (volume) of water into the residue;
ii) extracting the aqueous solution with diethyl ether, extracting the aqueous layer with n-butanol, evaporating to dryness under reduced pressure, performing silica gel column chromatography, and purifying with CHCl3-MeOH-H2Eluting with O at a ratio of 65: 35: 10 to obtain notoginsenoside.
3) Extracting rubescensine A
Extracting Rabdosia Rubescens (Hemsl.) Hara leaf dry powder with diethyl ether, discarding residue, and recovering diethyl ether from diethyl ether solution to obtain green brown residue; dissolving the residue with methanol, decolorizing to obtain clear methanol solution, concentrating under reduced pressure, standing at room temperature overnight, filtering, evaporating the methanol mother liquor to dryness, and grinding; preferably with neutral Al2O3Adsorbing, eluting with diethyl ether, and crystallizing.
4) Extracting indirubin:
drying folium Isatidis to obtain dried indigo naturalis, adding 30% concentrated hydrochloric acid in several times until no foam is generated, filtering, washing the precipitate with water to neutrality, and drying; adding methanol, refluxing for 2-4 times to obtain methanol extractive solution, filtering, recovering methanol from methanol solution, extracting residue with petroleum ether, removing petroleum ether, treating residue with 3% NaOH solution, washing precipitate with water to neutrality, and extracting with ethyl acetate to obtain indirubin.
5) Extracting chrysanthemum flavone
Pulverizing flos Chrysanthemi, extracting with 50-70% ethanol, concentrating under reduced pressure, adding 90-95% ethanol, precipitating, filtering, concentrating the filtrate until ethanol is removed, dissolving the residue with water, filtering, passing the filtrate through macroporous adsorbent resin (DM130), washing with deionized water until the column is colorless, eluting with 95% ethanol for multiple times, collecting flavone, and crystallizing.
6) Extracting liquiritigenin and isoliquiritigenin
Extracting Glycyrrhrizae radix with 3-4 times (volume) of 90-95% ethanol, extracting the ethanol solution with petroleum ether, mixing the water layer with silica gel, and adding MeOH-H2Eluting with O at a ratio of 7: 3, and concentrating the eluate to obtain residue;
adding water to the residue to dissolve completely, extracting with ethyl acetate, and extracting ethyl acetate layer with 5% Na2CO3Extracting with dilute acid to adjust pH to 5-6, extracting with ethyl acetate, drying, separating with polyamide column, and gradient eluting with 10-90% ethanol water solution to obtain liquiritigenin and isoliquiritigenin.
7) Mixing ganoderan (commercially available, produced in Shanghai agricultural department) containing ganoderan peptide and ganoderan beta-D glucan with the active ingredients extracted in the steps 1) -6) to obtain the product of the invention.
The ganoderma lucidum glycopeptide and ganoderma lucidum beta-D glucan can also be extracted by the following method:
i.a) removing impurities from the ganoderma lucidum, crushing, adding 8-10 times of water, soaking for 24 hours, heating to 95-100 ℃, and stirring for 8-10 hours;
b) filtering, preferably centrifuging or separating the extractive solution and residue with plate-frame separator to obtain filtrate and residue;
c) adding 3-4 times of water into the residue, leaching, preferably stirring at 95-100 deg.C for 8 hr; repeating steps b) and c)
II.a) heating the ganoderma lucidum fermentation liquor (containing the fungus balls) to 95-100 ℃, and stirring for 4 hours;
b) filtering, preferably centrifuging or separating the extractive solution and the bacteria balls by plate-and-frame separation;
c) adding 3-4 times (volume) of water into the residue containing the bacteria balls, extracting for 2 hr, filtering, separating the extractive solution and residue,
d) i.b), c) and II.c) are combined, the filtrate is concentrated to 1/8-1/10 of the original volume, edible alcohol (3-5 times) is added until the alcohol reaches about 70 percent, the mixture is kept still for alcohol precipitation for 24 hours, a centrifugal machine is used for separating precipitate, the alcohol is recovered, and the precipitate is dried. Or,
soxhlet extracting Ganoderma fruiting body with ethyl acetate for 4 hr, vacuum filtering, Soxhlet extracting the residue with acetone for 4 hr, vacuum filtering, soaking the residue in 90% ethanol for 24 hr, centrifuging, and vacuum filtering; extracting the residue with 0.2 mol/L phosphate buffer (PBS, pH 7.0) at 80 deg.C for three times, 4 hr/time, suction filtering, discarding residue, removing protein from the buffer, centrifuging, dialyzing the obtained supernatant, preferably with clear water for 7 days, and dialyzing with distilled water for 3 days;
adding a large amount of acetone into the non-dialyzed solution, precipitating, discarding supernatant, and washing precipitate with acetone for 6 times to obtain powdery solid of the desired product.
The preparation method of the traditional Chinese medicine composition further comprises the step 8):
a) crushing the active ingredients obtained in the steps 1) to 7) to fine powder with the particle size of less than or equal to 200 microns;
b) pulverizing, drying Sedum delavayi seed (Phoenix DACTYLIFERA L) or PUNICA granatum seed (PUNICA GRANAT-UN L), extracting with 8 times of anhydrous ethanol, preferably three times, mixing filtrates, concentrating under reduced pressure, treating with potassium acetylide to obtain powder,
c) the substances obtained from a) and b) are mixed in a weight ratio of 100-200: 1.
In one embodiment of the invention, the mixture obtained in step c) above is encapsulated.
In general, the products of the invention can be formulated for use as desired in a variety of dosage forms, preferably in the form of capsules for oral administration, the excipients and formulation techniques being well known in the art of pharmacy and those skilled in the art being able to formulate the above formulations according to the relevant literature and procedures known in the art.
The traditional Chinese medicine composition has the following characteristics:
1. anti-oxidation effect, eliminating free radicals;
2. bidirectionally regulating the number of red blood cells;
3. bidirectional regulation of the number of leukocytes;
4. no toxicity;
5. has remarkable antiviral effect;
6. induce cancer cell death;
7. regulating the central nervous system.
In order to show the treatment effect of the traditional Chinese medicine composition on prostate cancer, 6 patients are selected to take the traditional Chinese medicine composition, and the effect is shown in the following table 1:
TABLE 1 Effect of six patients taking the Chinese medicinal composition of the present invention
Age (age) PSA before taking the Chinese medicinal composition of the invention PSA after taking the Chinese medicinal composition of the invention
74 136.0 76(5 weeks)
73 308.0 233(2 weeks)
52 40.6 9.0(7 weeks)
73 89.0 7.12(11 weeks)
65 8.3 4.9(2 months)
60 37 15(2 months)
Note: PSA is an important index for marking prostate cancer, and high PSA indicates that prostate cancer is suffered.
From the above results, it can be seen that after all patients with prostate cancer take the Chinese medicinal composition of the present invention, the PSA index is reduced, i.e. the Chinese medicinal composition of the present invention has a therapeutic effect on prostate cancer. The life quality of all patients is improved, the appetite is increased, and the energy is vigorous.
In another clinical trial, 36 cases of sex hormone-dependent prostate cancers were all effective after taking the Chinese medicinal composition of the present invention. The effective rate of the traditional Chinese medicine composition reaches 60-70 percent after the traditional Chinese medicine composition is taken by prostate cancer which is not dependent on sex hormone. The clinical results show that the curative effect of the product of the invention is obviously superior to that of the medicines commonly used in the prior art.
(4) Detailed description of the preferred embodiments
The invention is further illustrated by the following examples.
Example 1
Weighing the raw materials (kilogram) according to the following proportion
Ganoderma lucidum 3. baicalensis 1. Rabdosia rubescens 1
Folium Isatidis 2 flos Chrysanthemi 1.5 Glycyrrhrizae radix 0.5
Notoginseng radix 0.5
Mixing the raw materials, grinding into traditional Chinese medicine coarse powder, and dividing the coarse powder into six equal parts for the following 1) -6) extraction steps;
1) extracting alkaloid:
i) percolating one part of the above coarse powder with 0.1% hydrochloric acid ethanol (95%) solution or leaching in several times to obtain acidic ethanol extractive solution;
ii) concentrating under reduced pressure to obtain a concentrate;
iii) washing with acidic water (pH 4-5), preferably freezing the acidic aqueous solution overnight in one embodiment, filtering to obtain a residue, and washing the residue with acidic water (pH 4-5) to obtain an acidic aqueous solution;
iv) adding ammonia water into the acidic water solution obtained in the step iii) for precipitation, and filtering to obtain total alkaloid precipitate; or
a) Adding dilute hydrochloric acid to the acidic aqueous solution obtained in step iii) to a pH of 2, and extracting with chloroform to obtain a chloroform layer and an aqueous layer; evaporating the chloroform from the chloroform layer to obtain a weak alkaloid residue;
b) adding alkali into the water layer until the pH value is 6, extracting with chloroform to obtain a water layer and a chloroform layer, and evaporating chloroform in the chloroform layer to obtain residue of strong alkaloid;
c) adjusting the pH of the water layer obtained in the step b) to 10 with sodium hydroxide solution, extracting with butanol, and evaporating the butanol in the butanol layer to obtain water-soluble alkaloid;
mixing the alkaloids obtained from a), b) and c) to obtain total alkaloids.
And recovering the chloroform and the butanol for recycling in the extraction step. Drying the alkaloid residue at low temperature, and crystallizing.
2) And (3) extracting polysaccharide:
extracting the above obtained Chinese medicinal coarse powder with 95 deg.C hot water for 2 hr, discarding residue, standing the filtrate for 12 hr, adding 60% ethanol into the supernatant, and centrifuging to obtain polysaccharide precipitate;
the polysaccharide precipitate is refined by diethyl ether.
3) And (3) lactone extraction:
refluxing the obtained coarse powder with diethyl ether, removing pigment with polyamide column, and recovering diethyl ether to obtain total lactone;
4) extracting saponin:
refluxing the obtained Chinese medicinal coarse powder with petroleum ether, evaporating petroleum ether to obtain defatted coarse powder, extracting with 95% ethanol, and concentrating under reduced pressure to obtain concentrated solution;
a) sequentially extracting the concentrated solution with chloroform and ethanol, and recovering chloroform and ethanol under reduced pressure to obtain saponin crude product; or
b) Extracting the concentrated solution with butanol to obtain butanol layer, and recovering butanol under reduced pressure to obtain saponin crude product.
5) Extracting the coumarin:
decocting the above obtained coarse powder in water for 1 hr, adding concentrated hydrochloric acid (30%) into the concentrated decoction, removing impurities insoluble substances, and standing to obtain coarse crystal of coumarin; drying, washing the crystal with acetone, drying, adding water, recrystallizing, heating, filtering, decolorizing to obtain water solution, and cooling to obtain light yellow pasty product.
6) And (3) extracting flavone:
a) soaking the coarse powder in 70% ethanol, recovering ethanol under reduced pressure, dissolving the residue in water, and filtering to obtain water solution; extracting the water solution with ethyl acetate, and concentrating the ethyl acetate solution under reduced pressure to obtain total flavonoids.
Mixing the alkaloid extracted in the steps 1) -6), polysaccharide, lactone, saponin, coumarins and flavone to obtain the traditional Chinese medicine composition for treating prostate cancer.
Example 2
1) Extracting baicalin:
i) adding 10 times (volume) of water into 2 kg of scutellaria baicalensis, decocting for 1 hour, and filtering;
ii) adjusting the filtrate to pH2 with acid, maintaining at 80 deg.C for 30 min, and centrifuging to precipitate; adding water into the precipitate, stirring, adding alkali to adjust pH to neutral, adding 5 times (volume) of ethanol, and filtering;
iii) adding hydrochloric acid to the filtrate to adjust the pH to 2, stirring, maintaining at 80 deg.C for 30 min, and filtering;
iv) washing the obtained precipitate with water and 50% ethanol respectively, and washing with 95% ethanol or recrystallizing to obtain baicalin.
2) Extracting notoginsenoside:
i) extracting 1.5 kg of soluble components in the root coarse powder of Panax notoginseng with 40% methanol, concentrating the methanol extract under reduced pressure, and adding 5 times (volume) of water to the residue;
ii) extracting the aqueous solution with diethyl ether, extracting the aqueous layer with n-butanol, evaporating to dryness under reduced pressure, performing silica gel column chromatography, and purifying with CHCl3-MeOH-H2Eluting with O at a ratio of 65: 35: 10 to obtain notoginsenoside.
3) Extracting rubescensine A
Extracting 2 kg of Rabdosia Rubescens (Hemsl.) Hara leaf dry powder with diethyl ether, discarding residue, and recovering diethyl ether from diethyl ether solution to obtain green brown residue; dissolving the residue with methanol, decolorizing to obtain clear methanol solution, concentrating under reduced pressure, standing at room temperature overnight, filtering, evaporating the methanol mother liquor to dryness, and grinding; reuse of neutral Al2O3Adsorbing, eluting with diethyl ether, and crystallizing.
4) Extracting indirubin:
1.5 kg of dyers woad leaf is dried and processed into dry indigo naturalis, 30 percent concentrated hydrochloric acid is added in several times until no foam is generated, the filtration is carried out, the precipitate is washed to be neutral by water and dried; adding methanol, refluxing for 2-4 times to obtain methanol extractive solution, filtering, recovering methanol from methanol solution, extracting residue with petroleum ether, removing petroleum ether, treating residue with 3% NaOH solution, washing precipitate with water to neutrality, and extracting with ethyl acetate to obtain indirubin.
5) Extracting chrysanthemum flavone
Pulverizing 1.5 kg flos Chrysanthemi, extracting with 50% ethanol, concentrating under reduced pressure, adding ethanol, precipitating, filtering, concentrating the filtrate until there is no ethanol, dissolving the residue with water, filtering, passing the filtrate through DM130 macroporous adsorbent resin, washing with deionized water until the column is colorless, eluting with 95% ethanol for multiple times, collecting flavone, and crystallizing.
6) Extracting liquiritigenin and isoliquiritigenin
1.5 kg of licorice was treated with 95% ethyl in an amount 3 times (by volume) that of licoriceExtracting with ethanol, extracting with petroleum ether, eluting water layer with silica gel column, and eluting with MeOH-H2Eluting with O at a ratio of 7: 3, and concentrating the eluate to obtain residue;
adding water to the residue to dissolve completely, extracting with ethyl acetate, and extracting ethyl acetate layer with 5% Na2CO3Extracting with dilute hydrochloric acid, adjusting pH of sodium carbonate water solution to 5-6, extracting with ethyl acetate, drying ethyl acetate solution, separating with 60 mesh polyamide column, and gradient eluting with 10-90% ethanol water solution to obtain liquiritigenin and isoliquiritigenin.
7) I.a) removing impurities from the ganoderma lucidum, crushing, adding 8 times of water, soaking for 24 hours, heating to 95 ℃, and stirring for 8 hours;
b) centrifugally separating the extracting solution and the dregs to obtain filtrate and dregs;
c) adding 3 times of water into the dregs of a decoction for leaching, and stirring for 8 hours at 95 ℃; repeating steps b) and c),
II.a) heating the ganoderma lucidum fermentation liquor (containing the fungus balls) to 95 ℃, and stirring for 4 hours;
b, centrifugally separating the extracting solution from the bacteria balls;
c) adding 3 times (volume) of water into the residue containing the bacteria balls, extracting for 2 hr, filtering, separating the extractive solution and residue,
d) mixing I.b), c) and II.c), concentrating to 1/8, adding edible alcohol (3-5 times) until the alcohol content reaches about 70%, standing for alcohol precipitation for 24 hr, separating precipitate with centrifuge, recovering alcohol, and drying the precipitate.
Mixing the active ingredients extracted in the steps 1) to 7) to obtain the traditional Chinese medicine composition (1).
Pulverizing the traditional Chinese medicine composition (1) into fine powder (2) with the particle size less than or equal to 200 microns;
pulverizing, drying Sedum indicum seed (Pheonix DACTYLIFERA L), extracting with 8 times of anhydrous ethanol, preferably three times, mixing filtrates, concentrating under reduced pressure, treating with potassium acetylide to obtain powder (3),
mixing the fine powder (2) and the powder (3) according to the weight ratio of 100-200: 1, and then encapsulating to obtain the capsule of the traditional Chinese medicine composition.
Example 3
1) Extracting baicalin:
i) adding 10 times (volume) of water into 1.5 kg of scutellaria baicalensis, decocting for 1 hour, and filtering;
ii) adjusting the filtrate to pH2 with dilute hydrochloric acid, maintaining at 80 deg.C for 30 min, and centrifuging to precipitate; adding water into the precipitate, stirring, adding alkali to adjust pH to neutral, adding 3 times (volume) of ethanol, and filtering;
iii) adding hydrochloric acid to the filtrate to adjust the pH to 2, stirring, maintaining at 80 deg.C for 30 min, and filtering;
iv) washing the obtained precipitate with water and 50% ethanol respectively, and washing with 95% ethanol or recrystallizing to obtain baicalin.
2) Extracting notoginsenoside:
i) extracting 0.9 kg of soluble components in the root coarse powder of Panax notoginseng with 40% methanol, concentrating the methanol extract under reduced pressure, and adding 5 times (volume) of water to the residue;
ii) extracting the aqueous solution with diethyl ether, extracting the aqueous layer with n-butanol, evaporating to dryness under reduced pressure, performing silica gel column chromatography, and purifying with CHCl3-MeOH-H2Eluting with O at a ratio of 65: 35: 10 to obtain notoginsenoside.
3) Extracting rubescensine A
Extracting 1.2 kg of Rabdosia Rubescens (Hemsl.) Hara leaf dry powder with diethyl ether, discarding residue, and recovering diethyl ether from diethyl ether solution to obtain green brown residue; dissolving the residue with methanol, decolorizing to obtain clear methanol solution, concentrating under reduced pressure, standing at room temperature overnight, filtering, evaporating the methanol mother liquor to dryness, and grinding; reuse of neutral Al2O3Adsorbing, eluting with diethyl ether, and crystallizing.
4) Extracting indirubin:
1.2 kg of dyers woad leaf is dried and processed into dry indigo naturalis, 30 percent concentrated hydrochloric acid is added in several times until no foam is generated, the filtration is carried out, the precipitate is washed to be neutral by water and dried; adding methanol, refluxing for 1 hr to obtain methanol extractive solution, filtering, recovering methanol from methanol solution, extracting the residue with petroleum ether, removing petroleum ether, treating the residue with 3% NaOH solution, washing the precipitate with water to neutrality, and extracting with ethyl acetate to obtain indirubin.
5) Extracting chrysanthemum flavone
Pulverizing 0.9 kg flos Chrysanthemi, extracting with 50% ethanol, concentrating under reduced pressure, adding 70% ethanol, precipitating, filtering, concentrating the filtrate until ethanol is removed, dissolving the residue with water, filtering, passing the filtrate through DM130 macroporous adsorbent resin, washing with deionized water until the column is colorless, eluting with 95% ethanol for multiple times, collecting flavone, and crystallizing.
6) Extracting liquiritigenin and isoliquiritigenin
Extracting 0.9 kg Glycyrrhrizae radix with 4 times (volume) 95% ethanol, extracting the ethanol solution with petroleum ether, mixing the water layer with silica gel, and adding MeOH-H2Eluting with O at a ratio of 7: 3, and concentrating the eluate to obtain residue;
adding water to the residue to dissolve completely, extracting with ethyl acetate, and extracting ethyl acetate layer with 5% Na2CO3Extracting with dilute acid to adjust pH to 5-6, extracting with ethyl acetate, drying, separating with polyamide column, and gradient eluting with 10-90% ethanol water solution to obtain liquiritigenin and isoliquiritigenin.
7) Ganoderma lucidum polysaccharide obtained from Shanghai agricultural family, the amount of the Ganoderma lucidum polysaccharide is 3 kg of Ganoderma lucidum raw material, the Ganoderma lucidum polysaccharide containing Ganoderma lucidum glycopeptide and Ganoderma lucidum beta-D glucan is mixed with the active ingredients extracted in the above steps 1) -6), the mixture is pulverized into fine powder, and the fine powder is encapsulated for use.

Claims (8)

1. A traditional Chinese medicine composition for treating prostate cancer is characterized by being prepared from the following raw materials in parts by weight:
ganoderma lucidum 3-4
1-2 of scutellaria
Rabdosia rubescens (Hemsl.) Hara 1-2
Folium Isatidis 1-2
0.5-1.5 of chrysanthemum
Radix Glycyrrhizae 0.5-1.5
0.5-1.5 of pseudo-ginseng
2. The traditional Chinese medicine composition according to claim 1, wherein the weight ratio of each raw material is as follows:
ganoderma, Scutellariae radix, Rabdosia Rubescens, folium Isatidis, flos Chrysanthemi, Glycyrrhrizae radix, Notoginseng radix (3: 1.5: 1.2: 0.9)
3. The method for preparing a Chinese medicinal composition according to claim 1, which comprises a mixed extraction preparation method or a target extraction preparation method.
4. The method of claim 3, wherein the mixed extraction method comprises:
1) preparing raw materials:
pulverizing and mixing Ganoderma, Scutellariae radix, Rabdosia Rubescens (Hemsl.) Hara, folium Isatidis, flos Chrysanthemi, Glycyrrhrizae radix, and Notoginseng radix at weight ratio of 3-4: 1-2: 0.5-1.5, and dividing the mixture into six equal parts;
2) extracting alkaloid:
i) percolating or leaching a part of the Chinese medicinal mixture obtained in step 1) with 0.1% ethanol hydrochloride solution to obtain acidic ethanol extractive solution;
ii) concentrating under reduced pressure to obtain a concentrate;
iii) washing with acidic water (pH 4-5), filtering to obtain residue, and washing the residue with acidic water (pH 4-5) to obtain acidic water solution;
iv) adding ammonia water into the acidic water solution obtained in the step iii) for precipitation, and filtering to obtain total alkaloid precipitate; or
a) Adding a dilute acid to the acidic aqueous solution obtained in step iii) to a pH of 2, and extracting with chloroform to obtain a chloroform layer and an aqueous layer; evaporating the chloroform in the chloroform layer to obtain weak alkaloid;
b) adding alkali into the water layer until the pH value is 6-7, extracting with chloroform to obtain a water layer and a chloroform layer, and evaporating chloroform in the chloroform layer to obtain strong alkaloid;
c) adjusting the pH of the water layer obtained in b) to 10 with alkali, extracting with butanol, and evaporating butanol in the butanol layer to obtain water-soluble alkaloid;
d) mixing the alkaloids obtained from a), b) and c) to obtain total alkaloids;
3) and (3) extracting polysaccharide:
extracting a part of the traditional Chinese medicine mixture obtained in the step 1) with hot water at 95-100 ℃, removing residues, standing the filtrate for 12 hours, adding ethanol with the concentration of more than 50% into the supernatant, and centrifuging to obtain polysaccharide precipitate;
4) and (3) lactone extraction:
refluxing a part of the traditional Chinese medicine mixture obtained in the step 1) with diethyl ether, removing pigments, and recovering the diethyl ether to obtain total lactones;
5) extracting saponin:
refluxing a part of the traditional Chinese medicine mixture obtained in the step 1) with petroleum ether, evaporating the petroleum ether to obtain degreased coarse powder, extracting with 90-95% ethanol, and concentrating under reduced pressure to obtain concentrated solution;
a) sequentially extracting the concentrated solution with chloroform and ethanol, and recovering chloroform and ethanol under reduced pressure to obtain crude product of total glycosides; or
b) Extracting the concentrated solution with butanol, and recovering butanol under reduced pressure to obtain saponin crude product;
6) extracting the coumarin:
decocting one part of the Chinese medicinal mixture obtained in the step 1) with water for 1-2 hours, concentrating the water decoction, adding concentrated hydrochloric acid, removing impurity insoluble substances, and standing clear liquid to obtain crude crystals of the coumarin;
7) and (3) extracting flavone:
soaking a part of the Chinese medicinal mixture obtained in step 1) with 70-80% ethanol, recovering ethanol from ethanol solution under reduced pressure, dissolving the residue with water, and filtering to obtain water solution; extracting the water solution with ethyl acetate, and concentrating the ethyl acetate solution under reduced pressure to obtain total flavonoids;
mixing the alkaloid extracted in the steps 2) -7), polysaccharide, lactone, saponin, coumarins and flavone to obtain the traditional Chinese medicine composition.
5. The method according to claim 3, wherein the method for extracting the target substance comprises:
1) extracting baicalin:
i) adding 10-15 times (volume) of water into the Scutellariae radix components, decocting for 1-2 hr, and filtering;
ii) adjusting the pH of the filtrate to 1-2 with acid, maintaining the temperature at 80-90 deg.C for 30-40 min, and centrifuging to precipitate; adding water into the precipitate, stirring, adding alkali to adjust pH to neutral, adding 3-5 times (volume) of ethanol, and filtering;
iii) adding acid to the filtrate to adjust pH to 1-2, stirring, maintaining at 80-90 deg.C for 30-40 min, and filtering;
iv) washing the obtained precipitate with water and 50% ethanol respectively, and then washing with 95% ethanol or recrystallizing to obtain baicalin;
2) extracting notoginsenoside:
i) extracting soluble components in the coarse powder of radix Notoginseng with methanol with concentration below 50%, concentrating the methanol extractive solution under reduced pressure, and adding 3-5 times (volume) of water into the residue;
ii) extracting the aqueous solution with diethyl ether, extracting the aqueous layer with n-butanol, evaporating to dryness under reduced pressure, performing silica gel column chromatography, and purifying with CHCl3-MeOH-H2Eluting with water at a ratio of O to water of 65: 35: 10 to obtain notoginsenoside;
3) extracting rubescensine A
Extracting Rabdosia Rubescens (Hemsl.) Hara leaf dry powder with diethyl ether, discarding residue, and recovering diethyl ether from diethyl ether solution to obtain green brown residue; dissolving the residue with methanol, decolorizing to obtain clear methanol solution, concentrating under reduced pressure, standing at room temperature overnight, filtering, evaporating the methanol mother liquor to dryness, and grinding; eluting with diethyl ether, and crystallizing;
4) extracting indirubin:
drying folium Isatidis to obtain dried indigo naturalis, adding 30% concentrated hydrochloric acid in several times until no foam is generated, filtering, washing the precipitate with water to neutrality, and drying; refluxing with methanol for 2-4 times to obtain methanol extractive solution, filtering, recovering methanol from methanol solution, extracting residue with petroleum ether, removing petroleum ether, treating residue with 3% NaOH solution, washing precipitate with water to neutrality, and extracting with ethyl acetate to obtain indirubin;
5) extracting chrysanthemum flavone
Pulverizing flos Chrysanthemi, extracting with 50-70% ethanol, concentrating under reduced pressure, adding 90-95% ethanol, precipitating, filtering, concentrating the filtrate until ethanol is removed, dissolving the residue with water, filtering, passing the filtrate through macroporous adsorbent resin, washing with deionized water until the column is colorless, eluting with 95% ethanol for multiple times, collecting flavone, and crystallizing;
6) extracting liquiritigenin and isoliquiritigenin
Extracting Glycyrrhrizae radix with 3-4 times (volume) of 90-95% ethanol, extracting the ethanol solution with petroleum ether, mixing the water layer with silica gel, and adding MeOH-H2Eluting with O7: 3, and concentrating the eluate to obtain residue;
adding water to the residue to dissolve completely, extracting with ethyl acetate, and separating ethyl acetate layer with 5% Na2CO3Extracting with dilute acid to adjust pH to 5-6, extracting with ethyl acetate, drying ethyl acetate, separating with polyamide column, and gradient eluting with 10-90% ethanol water solution to obtain liquiritigenin and isoliquiritigenin;
7) mixing ganoderan containing ganoderan peptide and ganoderan beta-D glucan with the active ingredients extracted in the steps 1) -6) to obtain the traditional Chinese medicine composition.
6. The method of claim 5, further comprising step 8):
a) crushing the active ingredients obtained in the steps 1) to 7) to fine powder with the particle size of less than or equal to 200 microns;
b) pulverizing, drying semen Ziziphi Spinosae/semen Granati/semen Punicae Granati, extracting with 8 times volume of anhydrous ethanol, concentrating under reduced pressure, treating with potassium acetylide to obtain powder,
c) the substances obtained from a) and b) are mixed in a weight ratio of 100-200: 1.
7. The method of claim 6, further comprising step d): encapsulating the mixture obtained in c).
8. The use of the Chinese medicinal composition of claim 1 in the preparation of a medicament for the treatment of prostate cancer.
CN02136655.1A 2002-08-26 2002-08-26 Chinese medicinal composition for treating prostate cancer, its preparation method and its application in the preparation of medicine for treating prostate cancer Expired - Lifetime CN1220519C (en)

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CN105106307A (en) * 2015-08-10 2015-12-02 上海中耀生物科技有限公司 Traditional Chinese medicine composition for treating prostate cancer, and preparation method and application of traditional Chinese medicine composition
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CN101495108B (en) * 2006-05-11 2014-10-15 活性植物科技有限公司 Composition for the treatment of resistant cancers comprising oridonin
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CN104435657A (en) * 2013-11-13 2015-03-25 程惠华 Medicine for preventing and treating side effects of hormone deprivation therapy and preparation method of medicine
CN104435657B (en) * 2013-11-13 2018-01-16 程惠华 A kind of medicine for preventing and treating prostate cancer endocrine therapy side effect and preparation method thereof
CN105106307A (en) * 2015-08-10 2015-12-02 上海中耀生物科技有限公司 Traditional Chinese medicine composition for treating prostate cancer, and preparation method and application of traditional Chinese medicine composition
WO2017024928A1 (en) * 2015-08-10 2017-02-16 上海中耀生物科技有限公司 Chinese medicinal composition for treating prostate cancer and preparation method and use thereof
US20180050073A1 (en) * 2015-08-10 2018-02-22 Shanghai Zhongyao Bio-Technology Co., Ltd. Traditional chinese medicine composition for treating prostate cancer, preparation method and application thereof
US10639338B2 (en) * 2015-08-10 2020-05-05 Shanghai Zhongyao Bio-Technology Co., Ltd. Traditional Chinese medicine composition for treating prostate cancer, preparation method and application thereof
CN106344830A (en) * 2016-10-10 2017-01-25 南宁多灵生物科技有限公司 Traditional Chinese medicine composition for treating prostatic cancer

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