CN102671113B - Traditional Chinese medicine composition for treating nodules of breasts and preparation method of traditional Chinese medicine composition - Google Patents
Traditional Chinese medicine composition for treating nodules of breasts and preparation method of traditional Chinese medicine composition Download PDFInfo
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Abstract
The invention discloses a traditional Chinese medicine composition for treating nodules of breasts and a preparation method of the traditional Chinese medicine composition. Raw materials of the traditional Chinese medicine composition include 15 traditional Chinese medicines. The preparation method includes respectively extracting and concentrating the raw materials; mixing and crushing obtained extracts; and adding a proper quantity of excipients into the mixed and crushed extracts to prepare the preparation.
Description
Technical field
The present invention relates to a kind of Chinese medicine composition for the treatment of nodules of the breast, is raw material by 15 flavor Chinese crude drugs, and through extracting, pulverizing is made.The invention still further relates to the Chinese medicine composition preparation method for the treatment of nodules of the breast.
Background technology
Cyclomastopathy is the modal cystic hyperplasia of breast of women, and its sickness rate accounts for the first place of mastopathy.This disease sickness rate was the trend risen year by year in the last few years, and the age also more and more becomes younger.In adolescence or young women, premenstrual distending pain of the breast is arranged, pain can involve the shoulder back sometimes, through the spontaneous remission gradually of rear udder attachment pain, only can contact mammary gland and a bit thicken, without obvious tuberosity, these are that physiological changes, and belong to physiological hypertrophy.Although be not disease, need to pay much attention to, although can not treat cyclomastopathy partly easily cancerate initiation tumor or even cancer early stage.Cyclomastopathy is normal breast lobule physiological hypertrophy and subinvolution, and the mammary gland normal configuration gets muddled, and belongs to pathological proliferation, and it is neither an inflammation class disease of non-tumor again.Be mainly in 30-50 year women, onset peak is 35-40 year.
Because mechanism and the cause of disease that cyclomastopathy is occurred there is no definite understanding, treatment at present is upper is symptomatic treatment substantially.But part patient falls ill, how rear several months to 1～2 year normal afterwards spontaneous remission, do not need treatment.Cyclomastopathy has a lot of types, and physiological cyclomastopathy, as Simple proliferation of mammary gland, does not need special handling, can disappear voluntarily.Because the cyclomastopathy that spirit, emotion and anthropic factor cause, by adjustment (other organ disease as relevant to the mastopathy generation as timely diagnosis and treatment of self, regulate emotion, alleviate stress, change unsound dietary habit, discontinue the habit of smoking and drinking etc.) also can disappear or alleviate.Pathologic cyclomastopathy, need active treatment, and becoming it is the cystic hyperplasia type, due to the possibility that has canceration, can not adopt a casual attitude.
The western medicine medicine has 5% potassium iodide, and the pain severe patient can be tried out methyl testosterone or tamoxifen, within menstruation the last week, start oral, in order to avoid further upset the trickle balance between the human hormone.Chinese traditional treatment is generally the cause of disease, the pathogenesis for cyclomastopathy, with regulating QI to relieve pain, and blood circulation promoting and blood stasis dispelling, hard masses softening and resolving is main, is aided with reinforcing kidney and strengthening resistance, strengthening vital QI to eliminate pathogenic factors, the method that the raising immunity of organisms is prescription.The Western medicine hormone medicine is felt simply helpless to this disease treatment.
Therefore under instructing, seeks Chinese medical discrimination a kind of effective Chinese patent medicine imperative with the therapeutic effect that improves treatment nodules of the breast disease.
Summary of the invention
The invention provides Chinese medicine composition be used for the treatment of nodules of the breast and preparation method thereof:
The composition of raw materials for preparing the present composition is:
Concha Ostreae 130-160 part, Radix Astragali 210-250 part, Rhizoma Sparganii 20-40 part, Fructus Hordei Germinatus 20-30 part, Radix Asparagi 140-170 part, Myrrha 50-70 part, Herba Epimedii 140-170 part, Radix Salviae Miltiorrhizae 140-170 part, Rhizoma Atractylodis Macrocephalae 20-40 part, Sargassum 140-170 part, Radix Bupleuri 20-40 part, Rhizoma Curcumae 20-40 part, Endothelium Corneum Gigeriae Galli 30-50 part, Pericarpium Citri Reticulatae Viride 20-40 part, Olibanum 20-40 part;
The consumption proportion of above-mentioned raw materials formula is preferably:
Concha Ostreae 140-160 part, Radix Astragali 215-245 part, Rhizoma Sparganii 25-35 part, Fructus Hordei Germinatus 23-28 part, Radix Asparagi 150-160 part, Myrrha 55-70 part, Herba Epimedii 145-165 part, Radix Salviae Miltiorrhizae 145-165, Rhizoma Atractylodis Macrocephalae 25-35 part, Sargassum 145-165 part, Radix Bupleuri 25-35 part, Rhizoma Curcumae 25-35 part, Endothelium Corneum Gigeriae Galli 35-50 part, Pericarpium Citri Reticulatae Viride 25-35 part, Olibanum 25-40 part;
The consumption proportion of above-mentioned raw materials formula is more preferably:
Concha Ostreae 150-160 part, Radix Astragali 220-240 part, Rhizoma Sparganii 25-35 part, Fructus Hordei Germinatus 23-28 part, Radix Asparagi 150-160 part, Myrrha 60-65 part, Herba Epimedii 150-160 part, Radix Salviae Miltiorrhizae 150-160, Rhizoma Atractylodis Macrocephalae 28-32 part, Sargassum 150-160 part, Radix Bupleuri 25-35 part, Rhizoma Curcumae 25-35 part, Endothelium Corneum Gigeriae Galli 40-45 part, Pericarpium Citri Reticulatae Viride 30-35 part, Olibanum 30-35 part;
The optimum amount proportioning of above-mentioned raw materials formula is:
157 parts of Concha Ostreaes, 235.6 parts of the Radixs Astragali, 31.4 parts of Rhizoma Sparganii, 26.2 parts, Fructus Hordei Germinatus, 157 parts of Radix Asparagis, 62.8 parts of Myrrhas, 157 parts of Herba Epimedii, 157 parts of Radix Salviae Miltiorrhizaes, 31.4 parts of the Rhizoma Atractylodis Macrocephalaes, 157 parts of Sargassums, 31.4 parts of Radix Bupleuri, 31.4 parts of Rhizoma Curcumae, 42 parts of Endothelium Corneum Gigeriae Galli, 31.4 parts, Pericarpium Citri Reticulatae Viride, 31.4 parts of Olibanums.
The application's pharmaceutical composition, in preparation process, for the different qualities of material medicine, adopt specific extraction process, to improve the content of single dose effective ingredient, improves drug effect, and reduced the Drug side reaction odds by process optimization.
The preparation method of pharmaceutical composition of the present invention is:
1) get the crude drug of following weight portion: Concha Ostreae 130-160 part, Radix Astragali 210-250 part, Rhizoma Sparganii 20-40 part, Fructus Hordei Germinatus 20-30 part, Radix Asparagi 140-170 part, Myrrha 50-70 part, Herba Epimedii 140-170 part, Radix Salviae Miltiorrhizae 140-170 part, Rhizoma Atractylodis Macrocephalae 20-40 part, Sargassum 140-170 part, Radix Bupleuri 20-40 part, Rhizoma Curcumae 20-40 part, Endothelium Corneum Gigeriae Galli 30-50 part, Pericarpium Citri Reticulatae Viride 20-40 part, Olibanum 20-40 part;
The Concha Ostreae of 2) getting weight portion described in step 1 adds acid extraction, obtains the acid extraction thing;
3) get Rhizoma Sparganii, Radix Bupleuri, the Rhizoma Atractylodis Macrocephalae, the Rhizoma Curcumae of weight portion described in step 1, mixed extraction volatile oil, the medicinal residues extracting in water, obtain the first water extract;
4) get Myrrha, Herba Epimedii, Radix Salviae Miltiorrhizae, Pericarpium Citri Reticulatae Viride, the Olibanum ethanol extraction of weight portion described in step 1, obtain alcohol extract; The medicinal residues extracting in water obtains the second water extract;
5) Radix Astragali, Fructus Hordei Germinatus, Radix Asparagi, Sargassum, the Endothelium Corneum Gigeriae Galli extracting in water of getting weight portion described in step 1 obtain the 3rd water extract;
6) above-mentioned first and second merged and concentrate with three water extracts, after the concentrate drying under reduced pressure, with acid extraction thing and alcohol extract co-grinding, spray into volatile oil, sealing is placed.
Preferred preparation method is:
1) get the crude drug of following weight portion: Concha Ostreae 140-160 part, Radix Astragali 215-245 part, Rhizoma Sparganii 25-35 part, Fructus Hordei Germinatus 23-28 part, Radix Asparagi 150-160 part, Myrrha 55-70 part, Herba Epimedii 145-165 part, Radix Salviae Miltiorrhizae 145-165, Rhizoma Atractylodis Macrocephalae 25-35 part, Sargassum 145-165 part, Radix Bupleuri 25-35 part, Rhizoma Curcumae 25-35 part, Endothelium Corneum Gigeriae Galli 35-50 part, Pericarpium Citri Reticulatae Viride 25-35 part, Olibanum 25-40 part;
2) the Concha Ostreae acid adding decocting of getting weight portion described in step 1 boils 1-3 time, and each 1-3 hour, filter, and obtains the acid extraction thing;
3) Rhizoma Sparganii, Radix Bupleuri, the Rhizoma Atractylodis Macrocephalae, the Rhizoma Curcumae of getting weight portion described in step 1 are soaked 2-4 hour, extract volatile oil, minute get volatile oil standby; Medicinal residues decoct with water 1-3 time, and each 1-3 hour, filter, and merges decoction liquor, obtains the first water extract;
4) get Myrrha, Herba Epimedii, Radix Salviae Miltiorrhizae, Pericarpium Citri Reticulatae Viride, the Olibanum alcohol reflux 1-3 time of weight portion described in step 1, merge extractive liquid,, reclaim ethanol to the thick paste shape, and drying under reduced pressure obtains alcohol extract; Medicinal residues decoct with water 1-3 time, and each 1-3 hour merges decoction liquor and obtains the second water extract;
5) Radix Astragali, Fructus Hordei Germinatus, Radix Asparagi, Sargassum, the Endothelium Corneum Gigeriae Galli of getting weight portion described in step 1 decoct with water 1-3 time, and each 1-3 hour, merge decoction liquor, filters to obtain the 3rd water extract;
6) first and second and three water extracts are merged to concentrating under reduced pressure, after the concentrate drying under reduced pressure, with acid extraction thing and alcohol extract co-grinding, spray into volatile oil, airtight placement.
Further preferred preparation method is:
1) get the crude drug of following weight portion: Concha Ostreae 150-160 part, Radix Astragali 220-240 part, Rhizoma Sparganii 25-35 part, Fructus Hordei Germinatus 23-28 part, Radix Asparagi 150-160 part, Myrrha 60-65 part, Herba Epimedii 150-160 part, Radix Salviae Miltiorrhizae 150-160, Rhizoma Atractylodis Macrocephalae 28-32 part, Sargassum 150-160 part, Radix Bupleuri 25-35 part, Rhizoma Curcumae 25-35 part, Endothelium Corneum Gigeriae Galli 40-45 part, Pericarpium Citri Reticulatae Viride 30-35 part, Olibanum 30-35 part;
2) the Concha Ostreae acid adding decocting of getting weight portion described in step 1 boils 1-3 time, and each 1-3 hour, filter, and filtrate is concentrated into dry, and crushed after being dried obtains the acid extraction thing;
3), after Rhizoma Sparganii, Radix Bupleuri, the Rhizoma Atractylodis Macrocephalae, the Rhizoma Curcumae of getting weight portion described in step 1 soaked 2-4 hour, with extraction by steam distillation volatile oil 5-7 hour, minute get volatile oil standby; Decoction liquor filters, and medicinal residues decoct with water 1-3 time, and each 1-3 hour, filter, and merges decoction liquor, obtains the first water extract;
4) get Myrrha, Herba Epimedii, Radix Salviae Miltiorrhizae, Pericarpium Citri Reticulatae Viride, the Olibanum 70-90% alcohol reflux secondary of weight portion described in step 1, merge secondary raffinate, filter, reclaim ethanol to the thick paste shape, drying under reduced pressure obtains alcohol extract, standby; Medicinal residues decoct with water secondary, and each 1-3 hour, filter, and merge decoction liquor and obtain the second water extract;
5) Radix Astragali, Fructus Hordei Germinatus, Radix Asparagi, Sargassum, the Endothelium Corneum Gigeriae Galli of getting weight portion described in step 1 decoct with water 1-3 time, and each 1-3 hour, merge the secondary decoction liquor, filters to obtain the 3rd water extract;
6) the, two and three water extracts are merged to concentrating under reduced pressure, with acid extraction thing and alcohol extract co-grinding, spray into volatile oil after the concentrate drying under reduced pressure, airtight placement.
More preferred preparation method is:
1) get the crude drug of following weight portion: 157 parts of Concha Ostreaes, 235.6 parts of the Radixs Astragali, 31.4 parts of Rhizoma Sparganii, 26.2 parts, Fructus Hordei Germinatus, 157 parts of Radix Asparagis, 62.8 parts of Myrrhas, 157 parts of Herba Epimedii, 157 parts of Radix Salviae Miltiorrhizaes, 31.4 parts of the Rhizoma Atractylodis Macrocephalaes, 157 parts of Sargassums, 31.4 parts of Radix Bupleuri, 31.4 parts of Rhizoma Curcumae, 42 parts of Endothelium Corneum Gigeriae Galli, 31.4 parts, Pericarpium Citri Reticulatae Viride, 31.4 parts of Olibanums, for following step;
2) Concha Ostreae powder of getting weight portion described in step 1 is broken into coarse powder, adds 5 times of amounts and adjusts the sour water of pH value to 2-3 with glacial acetic acid, decocts secondary, and each 2 hours, filter, filtrate is concentrated into dry, after drying, pulverizes to obtain the acid extraction thing;
3) get water soaking that Rhizoma Sparganii, the Rhizoma Atractylodis Macrocephalae, Radix Bupleuri, the Rhizoma Curcumae of weight portion described in step 1 add 10 times of amounts after 3 hours, with extraction by steam distillation volatile oil 6 hours, minute get volatile oil, another device is preserved; Decoction liquor filters, and the decocting that medicinal residues add 10 times of amounts boils secondary, and each 2 hours, filter, merge decoction liquor and obtain the first water extract;
4) get Myrrha, Herba Epimedii, Radix Salviae Miltiorrhizae, Pericarpium Citri Reticulatae Viride, the 80% alcohol reflux secondary for Olibanum of weight portion described in step 1, the alcohol reflux 3 hours that adds for the first time 8 times of amounts, the alcohol reflux 2 hours that adds for the second time 6 times of amounts, merge secondary raffinate, filter, reclaim ethanol to the thick paste shape, drying under reduced pressure obtains alcohol extract; The decocting that medicinal residues add 10 times of amounts boils secondary, and each 2 hours, filter, merge decoction liquor and obtain the second water extract;
5) decocting that the Radix Astragali, Fructus Hordei Germinatus, Radix Asparagi, Sargassum, the Endothelium Corneum Gigeriae Galli of getting weight portion described in step 1 adds 10 times of amounts boils secondary, and each 2 hours, merge the secondary decoction liquor, filter to obtain the 3rd water extract, standby;
6) first and second and three water extracts are merged, when being evaporated to 60 ℃ of relative densities and being 1.25-1.35, after drying under reduced pressure, with acid extraction thing and alcohol extract co-grinding, spray into volatile oil, airtight placement.
Aforementioned pharmaceutical compositions of the present invention, can make capsule, drop pill, pill,, acceptable dosage form on granule, tablet, suspensoid, injection, syrup, tincture, powder, medicinal tea, local medical solution, spray, suppository, microcapsule or other pharmaceuticss.
Above-mentioned dosage form carrier used in the preparation process is pharmaceutically acceptable carrier that commonly use or conventional, as diluent: include but not limited to sucrose, dextrin, starch, lactose, mannitol, xylitol, chitosan, SHUANGQITANG, soluble starch, Pulvis Talci or water solublity dextrin; Disintegrating agent includes but not limited to starch, sodium carboxymethyl cellulose, microcrystalline Cellulose, micropowder silica gel, hydroxypropyl starch, soluble starch, water solublity dextrin; Inclusion agents includes but not limited to a-cyclodextrin, B-cyclodextrin and N-LOK modified starch; Wetting agent includes but not limited to that water, ethanol, polyvinylpyrrolidone, hydroxypropyl cellulose, the above-mentioned pharmaceutically acceptable carrier of Polyethylene Glycol can be used separately, also can combine use.
The preparation process is preferably first and second and three water extracts is merged, and concentrating under reduced pressure, with acid extraction thing and alcohol extract co-grinding, add appropriate amount of auxiliary materials after drying under reduced pressure, granulates, and sprays into volatile oil, and 24h is placed in sealing, incapsulates.The starch that wherein said adjuvant is conventional amount used, cross linked polyvinyl pyrrolidone, polyvinylpyrrolidone, micropowder silica gel.
Pharmaceutical composition of the present invention, carried out a series of pharmacodynamics tests, and result is as follows:
Report on Animal
One, animal
SD kind rat, female unpregnancy, body weight 180～220g, provided by the Traditional Chinese Medicine Research Institute, Shanxi Province Experimental Animal Center.No. 08-25, the moving word of Shan doctor.
Two, tested medicine
1. breast peace sheet, be Film coated tablets, and extract powder is brown dry powder, the easy moisture absorption, and 2.0g crude drug/g dry powder, come from Xi'an Xintong Medicine Research Co., Ltd..Facing the used time is made into 3%, 6% concentration with distilled water.
2. test sample, i.e. drug regimen of the present invention, its concrete preparation method is put down in writing by embodiment 20, and 5.2g crude drug/g dry powder, come from Xi'an Xintong Medicine Research Co., Ltd..Facing the used time is made into 3%, 6% concentration with distilled water.
3 BUPIXIAO PIAN: this product is coated tablet, after removing sugar-coat, and aobvious brownish black, feeble QI bitter in the mouth, salty.0.32g/ sheet, economize Huan's core pharmaceutcal corporation, Ltd by LiaoNing, China and produce.Lot number: 020324, face the used time to be made into 1.6% concentration with distilled water.
4. estradiol benzoate injection (2mg/ml) is produced by Shanghai General Pharmaceutical Co., ltd..Lot number 01,080,111 5.09% sodium chloride injection is produced by Jingxi district, Xi'an pharmaceutical factory, lot number 000708-10.
Three, test method
Rat is divided into to 7 groups at random, 10 every group, (1) Normal group; (2) model group: estradiol benzoate injection (2mg/ml) (3) breast peace sheet 0.3g/kg:(4) breast peace sheet 0.6g/kg; (5) test sample 0.3g/kg; (6) test sample 0.6g/kg; (7) BUPIXIAO PIAN 1.6g/kg, except Normal group, all the other 6 groups of rats replace the female alcohol of benzene injection formic acid (0.8mg/kg) once in front oxter every other day, inject altogether 10 times, and gastric infusion, press above dosage gastric infusion every day once simultaneously.Normal group and model group gavage equal-volume distilled water 10ml/kg, rats in normal control group is alternately injected equal-volume 0.9% sodium chloride injection every other day in front oxter, after administration 20 days, put to death animal, measure first pair of breast diameter of every rat chest (footpath, vertically footpath anyhow) with precision vernier callipers; Get the mammary gland of second pair of breast of chest, carry out embedding, section, HE dyeing, its morphological changes of various tissue components of Microscopic observation, and measure lobules of mammary gland number, acinus number, alveolar lumen diameter and conduit diameter; Get the mammary gland of the 3rd pair of breast and measure footpath anyhow, mammary gland thickness, the internal organs such as this treatment with external measures uterus, thymus and spleen, weigh and calculate its organ coefficient.
Four, result of the test
1, the effect of para Toluic Acid's estradiol hyperplasia of mammary glands caused
Measure the footpath anyhow of first pair of breast of every rat chest with precision vernier callipers, vertical footpath, the area of calculating breast, formula is π r
2measure the footpath anyhow of the mammary gland of the 3rd pair of breast of every rat, thickness, the volume of calculating breast, formula π r simultaneously
2h.The results are shown in Table 1.Normal blank group udder size is normal.Estrogen group breast area and volume increase, compare remarkable increase (p<0.001) with Normal group, test sample group and breast peace sheet group heavy dose obviously reduce breast area and volume with low dose of, the rat mammary gland hypertrophy is all had to certain inhibitory action, under same dose, the drug action of test sample obviously is better than breast peace sheet, illustrate by preparation process amelioration, improved drug effect, reduced dosage.
The impact (X ± SD) on breast area and volume of table 1 breast peace sheet and test sample
* * compares P<0.001 with normal control
△ compares P<0.05 with model group
△ △ compares P<0.01 with model group
△ △ △ compares P<0.001 with model group
2, on the impact of animal viscera coefficient
Model group significantly reduces the thymus coefficient, and Spleen coefficient is without significant change, and the uterus coefficient obviously increases, and with Normal group, compares marked difference is all arranged.Heavy dose of and the small dose group of test sample group and breast peace sheet to thymus coefficient and Spleen coefficient without significant change, the uterus coefficient all significantly reduces (P<0.01), RUPIXIAO group thymus coefficient and Spleen coefficient and the more equal no significant difference of model group, but the uterus coefficient obviously reduces (P<0.01).In Table 2.
The impact (x ± SD) of table 2 on the animal viscera coefficient
* * compares P<0.001 with matched group
△ △ compares P<0.01 with model group
△ △ △ compares P<0.001 with model group
3, on the impact of mammary gland tissue
The rats in normal control group breast is little, mammary gland is in the quiescent stage state, without proliferative lesion, fat and connective tissue are more, acinus is few, lobule is not obvious, the gland catheter lumen is without expansion, the model group rat breast increases, cyclomastopathy is diffusivity, without local enclosed mass, fat and connective tissue obviously reduce, acinus number and lobule digital display work increase, alveolar lumen and gland catheter lumen are obviously expanded, the cell that alveolar lumen includes secretions and comes off, test sample group and the above-mentioned variation of RUPIXIAO group mammary gland tissue have clear improvement, breast peace sheet group has to a certain extent and improves mammary gland tissue.
The impact of table 3 on mammary gland tissue
* * compares P<0.001 with matched group
△ △ △ compares P<0.001 with model group
△ △ compares P<0.01 with model group
△ compares P<0.05 with model group
Clinical observation report
Be divided into two groups, test group is taken drug extract prepared by technique of the present invention; Matched group is taken BUPIXIAO PIAN, and the 0.32g/ sheet is economized Huan's core pharmaceutcal corporation, Ltd by LiaoNing, China and produced, lot number: 020324.
The result of improving of curative effect index shows:
The curative effect of disease: test group, matched group clinical recovery rate are respectively 4.72%, 4.03%; Total obvious effective rate is respectively 54.33%, 48.39%.Clinical recovery rate, total obvious effective rate, total effective rate two group difference not statistically significants.Tcm syndrome total mark test group drop-out value is 11.20 ± 4.48, and the matched group drop-out value is 10.48 ± 4.62; Drop-out value two group difference not statistically significants.Lump in breast maximum transverse diameter test group decline 1.13 ± 0.74cm, matched group drop-out value 1.05 ± 0.70cm; Changing value two group difference not statistically significants.The maximum vertical footpath of lump in breast test group decline 0.87 ± 0.66cm, matched group drop-out value 0.86 ± 0.68cm; Changing value two group difference not statistically significants (ITT analysis), TT analyzes consistent with PP analysis conclusion.Therefore can prove medicine prepared by technique of the present invention, the non-pessimum check of the variation of curative effect index is all qualified.
More equal not statistically significant (P>0.05) between mammary gland ultrasound diagnosis indices medication before and after test group and matched group group.More all reduce (P<0.05), more equal not statistically significant (P>0.05) before and after the matched group medication in group after left side body of gland thickness, right side body of gland thickness test group medication with before medication.
Therefore can reach a conclusion: it is effective that the medicine that the described preparation method of the application makes is used for the treatment of cyclomastopathy (syndrome of qi stagnation and blood stasis) clinical appraisal, compare no difference of science of statistics with matched group, and non-pessimum is up to the standards.Safety indexes do not occur researcher judge relevant with trial drug extremely.Test group occurs that menstruation increases, and the untoward reaction of headache is a case each.Medicine prepared by the present invention, more convenient patient applies, carries and preserve.And can make wide in varietyly, meet the different demands of medical treatment, prophylactic.
Above-mentioned pharmacodynamics data and clinical data are the prepared pharmaceutical composition of record method in the embodiment of the present invention 20, and the prepared compositions of additive method, still effective as space is limited,, at this, do not do and enumerate.
To sum up, its curative effect of pharmaceutical composition of the present invention is pacified sheet apparently higher than breast, and its 0.3g/kg dosage is suitable with breast peace sheet 0.6g/kg dosage drug activity, illustrates by process modification and has improved drug effect, and reduced the untoward reaction odds.
The accompanying drawing explanation
Fig. 1 is rat Normal group mammary gland tissue photo
Fig. 2 is rat model group mammary gland tissue photo
Fig. 3 is that test sample 0.3g/kg dosage group rat mammary gland is organized photo
Fig. 4 is that test sample 0.6g/kg dosage group rat mammary gland is organized photo
Fig. 5 organizes photo for breast peace sheet 0.3g/kg dosage group rat mammary gland
Fig. 6 organizes photo for breast peace film 0.6g/kg dosage group rat mammary gland
Fig. 7 is for to organize photo for BUPIXIAO PIAN 1.6g/kg dosage group rat mammary gland
The specific embodiment
Embodiment 1
1) get 160 parts of Concha Ostreaes, 250 parts of the Radixs Astragali, 40 parts of Rhizoma Sparganii, 30 parts, Fructus Hordei Germinatus, 170 parts of Radix Asparagis, 70 parts of Myrrhas, 170 parts of Herba Epimedii, 170 parts of Radix Salviae Miltiorrhizaes, 40 parts of the Rhizoma Atractylodis Macrocephalaes, 170 parts of Sargassums, 40 parts of Radix Bupleuri, 40 parts of Rhizoma Curcumae, 50 parts of Endothelium Corneum Gigeriae Galli, 40 parts, Pericarpium Citri Reticulatae Viride, 40 parts of Olibanums, for following step;
2) get Concha Ostreae acid adding decocting and boil, filter, filtrate is concentrated into dry, and crushed after being dried obtains the acid extraction thing, standby;
3) get Rhizoma Sparganii, Radix Bupleuri, the Rhizoma Atractylodis Macrocephalae, Rhizoma Curcumae and soak, with extraction by steam distillation volatile oil, minute get volatile oil standby; Decoction liquor filters, and medicinal residues decoct with water filtration, merges decoction liquor, obtains the first water extract, standby;
4) get Myrrha, Herba Epimedii, Radix Salviae Miltiorrhizae, Pericarpium Citri Reticulatae Viride, Olibanum alcohol reflux, filter, reclaim ethanol to the thick paste shape, drying under reduced pressure obtains alcohol extract, standby; Medicinal residues decoct with water filtration, merge decoction liquor and obtain the second water extract, standby;
5) get the Radix Astragali, Fructus Hordei Germinatus, Radix Asparagi, Sargassum, Endothelium Corneum Gigeriae Galli and decoct with water and filter to obtain the 3rd water extract, standby;
6) first and second and three water extracts are merged, concentrating under reduced pressure, with acid extraction thing and alcohol extract co-grinding, spray into volatile oil, airtight placement after drying under reduced pressure.
Embodiment 2
1) get the crude drug of following weight portion: 130 parts of Concha Ostreaes, 210 parts of the Radixs Astragali, 20 parts of Rhizoma Sparganii, 20 parts, Fructus Hordei Germinatus, 1400 parts of Radix Asparagis, 50 parts of Myrrhas, 140 parts of Herba Epimedii, 140 parts of Radix Salviae Miltiorrhizaes, 20 parts of the Rhizoma Atractylodis Macrocephalaes, 140 parts of Sargassums, 20 parts of Radix Bupleuri, 20 parts of Rhizoma Curcumae, 30 parts of Endothelium Corneum Gigeriae Galli, 20 parts, Pericarpium Citri Reticulatae Viride, 20 parts of Olibanums;
2) the Concha Ostreae acid adding decocting of getting weight portion described in step 1 boils 1 time, and each 1 hour, filter, obtain the acid extraction thing;
3) Rhizoma Sparganii, Radix Bupleuri, the Rhizoma Atractylodis Macrocephalae, the Rhizoma Curcumae of getting weight portion described in step 1 are soaked 2 hours, extract volatile oil, minute get volatile oil standby; Medicinal residues decoct with water 1 time, and each 1 hour, filter, merge decoction liquor, obtain the first water extract;
4) get Myrrha, Herba Epimedii, Radix Salviae Miltiorrhizae, Pericarpium Citri Reticulatae Viride, the Olibanum alcohol reflux 1-3 time of weight portion described in step 1, merge extractive liquid,, reclaim ethanol to the thick paste shape, and drying under reduced pressure obtains alcohol extract; Medicinal residues decoct with water 1 time, each 1 hour, merge decoction liquor and obtain the second water extract;
5) get the Radix Astragali, Fructus Hordei Germinatus, Radix Asparagi, Sargassum, Endothelium Corneum Gigeriae Galli and decoct with water 1 time, each 1 hour, merge decoction liquor, filter to obtain the 3rd water extract;
6) first and second and three water extracts are merged to concentrating under reduced pressure, after drying under reduced pressure, with acid extraction thing and alcohol extract co-grinding, spray into volatile oil, airtight placement.
Embodiment 3
1) get the crude drug of following weight portion: 160 parts of Concha Ostreaes, 245 parts of the Radixs Astragali, 35 parts of Rhizoma Sparganii, 28 parts, Fructus Hordei Germinatus, 160 parts of Radix Asparagis, 70 parts of Myrrhas, 165 parts of Herba Epimedii, Radix Salviae Miltiorrhizae 165,35 parts of the Rhizoma Atractylodis Macrocephalaes, 165 parts of Sargassums, 35 parts of Radix Bupleuri, 35 parts of Rhizoma Curcumae, 50 parts of Endothelium Corneum Gigeriae Galli, 35 parts, Pericarpium Citri Reticulatae Viride, 40 parts of Olibanums;
2) the Concha Ostreae acid adding decocting of getting weight portion described in step 1 boils 3 times, and each 3 hours, filter, obtain the acid extraction thing;
3) Rhizoma Sparganii, Radix Bupleuri, the Rhizoma Atractylodis Macrocephalae, the Rhizoma Curcumae of getting weight portion described in step 1 are soaked 4 hours, extract volatile oil, minute get volatile oil standby; Medicinal residues decoct with water 3 times, and each 3 hours, filter, merge decoction liquor, obtain the first water extract;
4) get Myrrha, Herba Epimedii, Radix Salviae Miltiorrhizae, Pericarpium Citri Reticulatae Viride, the Olibanum alcohol reflux 3 times of weight portion described in step 1, merge extractive liquid,, reclaim ethanol to the thick paste shape, and drying under reduced pressure obtains alcohol extract; Medicinal residues decoct with water 3 times, each 3 hours, merge decoction liquor and obtain the second water extract;
5) get the Radix Astragali, Fructus Hordei Germinatus, Radix Asparagi, Sargassum, Endothelium Corneum Gigeriae Galli and decoct with water 3 times, each 3 hours, merge decoction liquor, filter to obtain the 3rd water extract;
6) first and second and three water extracts are merged to concentrating under reduced pressure, after drying under reduced pressure, with acid extraction thing and alcohol extract co-grinding, spray into volatile oil, airtight placement.
Embodiment 4
1) get the crude drug of following weight portion: 150 parts of Concha Ostreaes, 220 parts of the Radixs Astragali, 25 parts of Rhizoma Sparganii, 23 parts, Fructus Hordei Germinatus, 150 parts of Radix Asparagis, 60 parts of Myrrhas, 150 parts of Herba Epimedii, Radix Salviae Miltiorrhizae 150,28 parts of the Rhizoma Atractylodis Macrocephalaes, 150 parts of Sargassums, 25 parts of Radix Bupleuri, 25 parts of Rhizoma Curcumae, 40 parts of Endothelium Corneum Gigeriae Galli, 30 parts, Pericarpium Citri Reticulatae Viride, 30 parts of Olibanums;
2) the Concha Ostreae acid adding decocting of getting weight portion described in step 1 boils 1 time, and 3 hours, filter, filtrate is concentrated into dry, and crushed after being dried obtains the acid extraction thing;
3), after Rhizoma Sparganii, Radix Bupleuri, the Rhizoma Atractylodis Macrocephalae, the Rhizoma Curcumae of getting weight portion described in step 1 soaked 2 hours, with extraction by steam distillation volatile oil 5 hours, minute get volatile oil standby; Decoction liquor filters, and medicinal residues decoct with water 1 time, and each 3 hours, filter, merge decoction liquor, obtain the first water extract;
4) get the Myrrha, Herba Epimedii, Radix Salviae Miltiorrhizae, Pericarpium Citri Reticulatae Viride of weight portion described in step 1,70% alcohol reflux secondary for Olibanum, merge secondary raffinate, filter, reclaim ethanol to the thick paste shape, drying under reduced pressure obtains alcohol extract, standby; Medicinal residues decoct with water secondary, and each 1 hour, filter, merge decoction liquor and obtain the second water extract;
5) get the Radix Astragali, Fructus Hordei Germinatus, Radix Asparagi, Sargassum, Endothelium Corneum Gigeriae Galli and decoct with water 1 time, 3 hours, merge the secondary decoction liquor, filter to obtain the 3rd water extract;
6) first and second and three water extracts are merged to concentrating under reduced pressure, after drying under reduced pressure, with acid extraction thing and alcohol extract co-grinding, spray into volatile oil, airtight placement.
Embodiment 5
1) get the crude drug of following weight portion: 160 parts of Concha Ostreaes, 240 parts of the Radixs Astragali, 35 parts of Rhizoma Sparganii, 28 parts, Fructus Hordei Germinatus, 160 parts of Radix Asparagis, 65 parts of Myrrhas, 160 parts of Herba Epimedii, Radix Salviae Miltiorrhizae 160,32 parts of the Rhizoma Atractylodis Macrocephalaes, 160 parts of Sargassums, 35 parts of Radix Bupleuri, 35 parts of Rhizoma Curcumae, 45 parts of Endothelium Corneum Gigeriae Galli, 35 parts, Pericarpium Citri Reticulatae Viride, 35 parts of Olibanums;
2) the Concha Ostreae acid adding decocting of getting weight portion described in step 1 boils 3 times, and each 1 hour, filter, filtrate is concentrated into dry, and crushed after being dried obtains the acid extraction thing;
3), after Rhizoma Sparganii, Radix Bupleuri, the Rhizoma Atractylodis Macrocephalae, the Rhizoma Curcumae of getting weight portion described in step 1 soaked 4 hours, with extraction by steam distillation volatile oil 7 hours, minute get volatile oil standby; Decoction liquor filters, and medicinal residues decoct with water 3 times, and each 1 hour, filter, merge decoction liquor, obtain the first water extract;
4) get Myrrha, Herba Epimedii, Radix Salviae Miltiorrhizae, Pericarpium Citri Reticulatae Viride, the Olibanum 70-90% alcohol reflux secondary of weight portion described in step 1, merge secondary raffinate, filter, reclaim ethanol to the thick paste shape, drying under reduced pressure obtains alcohol extract, standby; Medicinal residues decoct with water secondary, and each 3 hours, filter, merge decoction liquor and obtain the second water extract;
5) get the Radix Astragali, Fructus Hordei Germinatus, Radix Asparagi, Sargassum, Endothelium Corneum Gigeriae Galli and decoct with water 3 times, each 1 hour, merge the secondary decoction liquor, filter to obtain the 3rd water extract;
6) the, two and three water extracts are merged to concentrating under reduced pressure, with acid extraction thing and alcohol extract co-grinding, spray into volatile oil after drying under reduced pressure, airtight placement.
Embodiment 6
1) get the crude drug of following weight portion: 157 parts of Concha Ostreaes, 235.6 parts of the Radixs Astragali, 31.4 parts of Rhizoma Sparganii, 26.2 parts, Fructus Hordei Germinatus, 157 parts of Radix Asparagis, 62.8 parts of Myrrhas, 157 parts of Herba Epimedii, 157 parts of Radix Salviae Miltiorrhizaes, 31.4 parts of the Rhizoma Atractylodis Macrocephalaes, 157 parts of Sargassums, 31.4 parts of Radix Bupleuri, 31.4 parts of Rhizoma Curcumae, 42 parts of Endothelium Corneum Gigeriae Galli, 31.4 parts, Pericarpium Citri Reticulatae Viride, 31.4 parts of Olibanums, for following step;
2) Concha Ostreae powder of getting weight portion described in step 1 is broken into coarse powder, adds 5 times of amounts and adjusts the sour water of pH value to 2-3 with glacial acetic acid, decocts secondary, and each 2 hours, filter, filtrate is concentrated into dry, after drying, pulverizes to obtain the acid extraction thing;
3) get water soaking that Rhizoma Sparganii, the Rhizoma Atractylodis Macrocephalae, Radix Bupleuri, the Rhizoma Curcumae of weight portion described in step 1 add 10 times of amounts after 3 hours, with extraction by steam distillation volatile oil 6 hours, minute get volatile oil, another device is preserved; Decoction liquor filters, and the decocting that medicinal residues add 10 times of amounts boils secondary, and each 2 hours, filter, merge decoction liquor and obtain the first water extract;
4) get Myrrha, Herba Epimedii, Radix Salviae Miltiorrhizae, Pericarpium Citri Reticulatae Viride, the 80% alcohol reflux secondary for Olibanum of weight portion described in step 1, the alcohol reflux 3 hours that adds for the first time 8 times of amounts, the alcohol reflux 2 hours that adds for the second time 6 times of amounts, merge secondary raffinate, filter, reclaim ethanol to the thick paste shape, drying under reduced pressure obtains alcohol extract; The decocting that medicinal residues add 10 times of amounts boils secondary, and each 2 hours, filter, merge decoction liquor and obtain the second water extract;
5) decocting that the Radix Astragali, Fructus Hordei Germinatus, Radix Asparagi, Sargassum, the Endothelium Corneum Gigeriae Galli of getting weight portion described in step 1 adds 10 times of amounts boils secondary, and each 2 hours, merge the secondary decoction liquor, filter to obtain the 3rd water extract, standby;
6) first and second and three water extracts are merged, being evaporated to 60 ℃ of relative densities is 1.25-1.35, after drying under reduced pressure, with acid extraction thing and alcohol extract co-grinding, sprays into volatile oil, airtight placement.
Embodiment 7
1) get 150 parts of Concha Ostreaes, 230 parts of the Radixs Astragali, 30 parts of Rhizoma Sparganii, 25 parts, Fructus Hordei Germinatus, 155 parts of Radix Asparagis, 60 parts of Myrrhas, 155 parts of Herba Epimedii, Radix Salviae Miltiorrhizae 155,30 parts of the Rhizoma Atractylodis Macrocephalaes, 155 parts of Sargassums, 30 parts of Radix Bupleuri, 30 parts of Rhizoma Curcumae, 40 parts of Endothelium Corneum Gigeriae Galli, 30 parts, Pericarpium Citri Reticulatae Viride, 35 parts of Olibanums; For following step;
2) get Concha Ostreae acid adding decocting and boil 2 times, each 1-3 hour, filter, and filtrate is concentrated into dry, and crushed after being dried obtains the acid extraction thing, standby;
3), after getting Rhizoma Sparganii, Radix Bupleuri, the Rhizoma Atractylodis Macrocephalae, Rhizoma Curcumae and soaking 2-4 hour, with extraction by steam distillation volatile oil 5-7 hour, minute get volatile oil standby; Decoction liquor filters, and medicinal residues decoct with water 2 times, and each 2 hours, filter, merge decoction liquor, obtain the first water extract, standby;
4) get Myrrha, Herba Epimedii, Radix Salviae Miltiorrhizae, Pericarpium Citri Reticulatae Viride, 80% alcohol reflux secondary for Olibanum, merge secondary raffinate, filter, reclaim ethanol to the thick paste shape, drying under reduced pressure obtains alcohol extract, standby; Medicinal residues decoct with water secondary, and each 2 hours, filter, merge decoction liquor and obtain the second water extract, standby;
5) get the Radix Astragali, Fructus Hordei Germinatus, Radix Asparagi, Sargassum, Endothelium Corneum Gigeriae Galli and decoct with water secondary, each 2 hours, merge the secondary decoction liquor, filter to obtain the 3rd water extract, standby;
6) first and second and three water extracts are merged, when being evaporated to 50-80 ℃ of relative density and being 1.25-1.35, reduce pressure after dry and acid extraction thing and alcohol extract co-grinding, spray into volatile oil, airtight placement.
Embodiment 8
1) get 157 parts of Concha Ostreaes, 235.6 parts of the Radixs Astragali, 31.4 parts of Rhizoma Sparganii, 26.2 parts, Fructus Hordei Germinatus, 157 parts of Radix Asparagis, 62.8 parts of Myrrhas, 157 parts of Herba Epimedii, 157 parts of Radix Salviae Miltiorrhizaes, 31.4 parts of the Rhizoma Atractylodis Macrocephalaes, 157 parts of Sargassums, 31.4 parts of Radix Bupleuri, 31.4 parts of Rhizoma Curcumae, 42 parts of Endothelium Corneum Gigeriae Galli, 31.4 parts, Pericarpium Citri Reticulatae Viride, 31.4 parts of Olibanums, for following step;
2) get Concha Ostreae powder and be broken into coarse powder, add 5 times of amounts and adjust the sour water of pH value to 2-3 with glacial acetic acid, decoct secondary, each 2 hours, filter, filtrate is concentrated into dry, after drying, pulverizes to such an extent that the acid extraction thing is standby;
3) get water soaking that Rhizoma Sparganii, the Rhizoma Atractylodis Macrocephalae, Radix Bupleuri, Rhizoma Curcumae add 10 times of amounts after 3 hours, with extraction by steam distillation volatile oil 6 hours, minute get volatile oil, another device is preserved; Decoction liquor filters, and the decocting that medicinal residues add 10 times of amounts boils secondary, and each 2 hours, filter, merge decoction liquor and obtain the first water extract, standby;
4) get Myrrha, Herba Epimedii, Radix Salviae Miltiorrhizae, Pericarpium Citri Reticulatae Viride, 80% alcohol reflux secondary for Olibanum, merge secondary raffinate, filter, reclaim ethanol to the thick paste shape, drying under reduced pressure obtains alcohol extract, standby; Medicinal residues decoct with water secondary, and each 2 hours, filter, merge decoction liquor and obtain the second water extract, standby;
5) get the Radix Astragali, Fructus Hordei Germinatus, Radix Asparagi, Sargassum, Endothelium Corneum Gigeriae Galli and decoct with water secondary, each 2 hours, merge the secondary decoction liquor, filter to obtain the 3rd water extract, standby;
6) first and second and three water extracts are merged, when being evaporated to 50-80 ℃ of relative density and being 1.25-1.35, after drying under reduced pressure, with acid extraction thing and alcohol extract co-grinding, spray into volatile oil, airtight placement.
Embodiment 9
1) get 157 parts of Concha Ostreaes, 235.6 parts of the Radixs Astragali, 31.4 parts of Rhizoma Sparganii, 26.2 parts, Fructus Hordei Germinatus, 157 parts of Radix Asparagis, 62.8 parts of Myrrhas, 157 parts of Herba Epimedii, 157 parts of Radix Salviae Miltiorrhizaes, 31.4 parts of the Rhizoma Atractylodis Macrocephalaes, 157 parts of Sargassums, 31.4 parts of Radix Bupleuri, 31.4 parts of Rhizoma Curcumae, 42 parts of Endothelium Corneum Gigeriae Galli, 31.4 parts, Pericarpium Citri Reticulatae Viride, 31.4 parts of Olibanums, for following step;
2) get Concha Ostreae acid adding decocting and boil 2 times, each 2 hours, filter, filtrate is concentrated into dry, and crushed after being dried obtains the acid extraction thing, standby;
3), after getting Rhizoma Sparganii, Radix Bupleuri, the Rhizoma Atractylodis Macrocephalae, Rhizoma Curcumae and soaking 3 hours, with extraction by steam distillation volatile oil 5-7 hour, minute get volatile oil standby; Decoction liquor filters, and medicinal residues decoct with water 2 times, and each 2 hours, filter, merge decoction liquor, obtain the first water extract, standby;
4) get Myrrha, Herba Epimedii, Radix Salviae Miltiorrhizae, Pericarpium Citri Reticulatae Viride, 80% alcohol reflux secondary for Olibanum, the alcohol reflux 3 hours that adds for the first time 8 times of amounts, the alcohol reflux 2 hours that adds for the second time 6 times of amounts, merge secondary raffinate, filter, reclaim ethanol to the thick paste shape, drying under reduced pressure obtains alcohol extract; The decocting that medicinal residues add 10 times of amounts boils secondary, and each 2 hours, filter, it is standby that the merging decoction liquor obtains the second water extract;
5) get the Radix Astragali, Fructus Hordei Germinatus, Radix Asparagi, Sargassum, Endothelium Corneum Gigeriae Galli and decoct with water secondary, each 2 hours, merge the secondary decoction liquor, filter to obtain the 3rd water extract, standby;
6) first and second and three water extracts are merged, when being evaporated to 60 ℃ of relative densities and being 1.25-1.35, after drying under reduced pressure, with acid extraction thing and alcohol extract co-grinding, spray into volatile oil, airtight placement.
Embodiment 10
1) get 157 parts of Concha Ostreaes, 235.6 parts of the Radixs Astragali, 31.4 parts of Rhizoma Sparganii, 26.2 parts, Fructus Hordei Germinatus, 157 parts of Radix Asparagis, 62.8 parts of Myrrhas, 157 parts of Herba Epimedii, 157 parts of Radix Salviae Miltiorrhizaes, 31.4 parts of the Rhizoma Atractylodis Macrocephalaes, 157 parts of Sargassums, 31.4 parts of Radix Bupleuri, 31.4 parts of Rhizoma Curcumae, 42 parts of Endothelium Corneum Gigeriae Galli, 31.4 parts, Pericarpium Citri Reticulatae Viride, 31.4 parts of Olibanums, for following step;
2) get Concha Ostreae powder and be broken into coarse powder, add 5 times of amounts and adjust the sour water of pH value to 2-3 with glacial acetic acid, decoct secondary, each 2 hours, filter, filtrate is concentrated into dry, after drying, pulverizes to such an extent that the acid extraction thing is standby;
3) get water soaking that Rhizoma Sparganii, the Rhizoma Atractylodis Macrocephalae, Radix Bupleuri, Rhizoma Curcumae add 10 times of amounts after 3 hours, with extraction by steam distillation volatile oil 6 hours, minute get volatile oil, another device is preserved; Decoction liquor filters, and the decocting that medicinal residues add 10 times of amounts boils secondary, and each 2 hours, filter, merge decoction liquor and obtain the first water extract, standby;
4) get Myrrha, Herba Epimedii, Radix Salviae Miltiorrhizae, Pericarpium Citri Reticulatae Viride, 80% alcohol reflux secondary for Olibanum, the alcohol reflux 3 hours that adds for the first time 8 times of amounts, the alcohol reflux 2 hours that adds for the second time 6 times of amounts, merge secondary raffinate, filter, reclaim ethanol to the thick paste shape, drying under reduced pressure obtains alcohol extract; The decocting that medicinal residues add 10 times of amounts boils secondary, and each 2 hours, filter, it is standby that the merging decoction liquor obtains the second water extract;
5) get the Radix Astragali, Fructus Hordei Germinatus, Radix Asparagi, Sargassum, Endothelium Corneum Gigeriae Galli and decoct with water secondary, each 2 hours, merge the secondary decoction liquor, filter to obtain the 3rd water extract, standby;
6) first and second and three water extracts are merged, when being evaporated to 60 ℃ of relative densities and being 1.25-1.35, after drying under reduced pressure, with acid extraction thing and alcohol extract co-grinding, spray into volatile oil, airtight placement.
Embodiment 11
1) get 157 parts of Concha Ostreaes, 235.6 parts of the Radixs Astragali, 31.4 parts of Rhizoma Sparganii, 26.2 parts, Fructus Hordei Germinatus, 157 parts of Radix Asparagis, 62.8 parts of Myrrhas, 157 parts of Herba Epimedii, 157 parts of Radix Salviae Miltiorrhizaes, 31.4 parts of the Rhizoma Atractylodis Macrocephalaes, 157 parts of Sargassums, 31.4 parts of Radix Bupleuri, 31.4 parts of Rhizoma Curcumae, 42 parts of Endothelium Corneum Gigeriae Galli, 31.4 parts, Pericarpium Citri Reticulatae Viride, 31.4 parts of Olibanums, for following step;
2) get Concha Ostreae powder and be broken into coarse powder, add 5 times of amounts and adjust the sour water of pH value to 2.5 with glacial acetic acid, decoct secondary, each 2 hours, filter, filtrate is concentrated into dry, after drying, pulverizes to such an extent that the acid extraction thing is standby;
3) get water soaking that Rhizoma Sparganii, the Rhizoma Atractylodis Macrocephalae, Radix Bupleuri, Rhizoma Curcumae add 10 times of amounts after 3 hours, with extraction by steam distillation volatile oil 6 hours, minute get volatile oil, another device is preserved; Decoction liquor filters, and the decocting that medicinal residues add 10 times of amounts boils secondary, and each 2 hours, filter, merge decoction liquor and obtain the first water extract, standby;
4) get Myrrha, Herba Epimedii, Radix Salviae Miltiorrhizae, Pericarpium Citri Reticulatae Viride, 80% alcohol reflux secondary for Olibanum, the alcohol reflux 3 hours that adds for the first time 8 times of amounts, the alcohol reflux 2 hours that adds for the second time 6 times of amounts, merge secondary raffinate, filter, reclaim ethanol to the thick paste shape, drying under reduced pressure obtains alcohol extract; The decocting that medicinal residues add 10 times of amounts boils secondary, and each 2 hours, filter, it is standby that the merging decoction liquor obtains the second water extract;
5) get the Radix Astragali, Fructus Hordei Germinatus, Radix Asparagi, Sargassum, Endothelium Corneum Gigeriae Galli and decoct with water secondary, each 2 hours, merge the secondary decoction liquor, filter to obtain the 3rd water extract, standby;
6) first and second and three water extracts are merged, being evaporated to 60 ℃ of relative densities is 1.3 o'clock, after drying under reduced pressure, with acid extraction thing and alcohol extract co-grinding, sprays into volatile oil, airtight placement.
Embodiment 12
1) get 157 parts of Concha Ostreaes, 235.6 parts of the Radixs Astragali, 31.4 parts of Rhizoma Sparganii, 26.2 parts, Fructus Hordei Germinatus, 157 parts of Radix Asparagis, 62.8 parts of Myrrhas, 157 parts of Herba Epimedii, 157 parts of Radix Salviae Miltiorrhizaes, 31.4 parts of the Rhizoma Atractylodis Macrocephalaes, 157 parts of Sargassums, 31.4 parts of Radix Bupleuri, 31.4 parts of Rhizoma Curcumae, 42 parts of Endothelium Corneum Gigeriae Galli, 31.4 parts, Pericarpium Citri Reticulatae Viride, 31.4 parts of Olibanums, for following step;
2) get Concha Ostreae powder and be broken into the phase powder, add 5 times of amounts and adjust the sour water of pH value to 2 with glacial acetic acid, decoct secondary, each 2 hours, filter, filtrate is concentrated into dry, after drying, pulverizes to such an extent that the acid extraction thing is standby;
3) get water soaking that Rhizoma Sparganii, the Rhizoma Atractylodis Macrocephalae, Radix Bupleuri, Rhizoma Curcumae add 10 times of amounts after 3 hours, with extraction by steam distillation volatile oil 6 hours, minute get volatile oil, another device is preserved; Decoction liquor filters, and the decocting that medicinal residues add 10 times of amounts boils secondary, and each 2 hours, filter, merge decoction liquor and obtain the first water extract, standby;
4) get Myrrha, Herba Epimedii, Radix Salviae Miltiorrhizae, Pericarpium Citri Reticulatae Viride, 80% alcohol reflux secondary for Olibanum, the alcohol reflux 3 hours that adds for the first time 8 times of amounts, the alcohol reflux 2 hours that adds for the second time 6 times of amounts, merge secondary raffinate, filter, reclaim ethanol to the thick paste shape, drying under reduced pressure obtains alcohol extract; The decocting that medicinal residues add 10 times of amounts boils secondary, and each 2 hours, filter, it is standby that the merging decoction liquor obtains the second water extract;
5) get the Radix Astragali, Fructus Hordei Germinatus, Radix Asparagi, Sargassum, Endothelium Corneum Gigeriae Galli and decoct with water secondary, each 2 hours, merge the secondary decoction liquor, filter to obtain the 3rd water extract, standby;
6) first and second and three water extracts are merged, being evaporated to 60 ℃ of relative densities is 1.25 o'clock, after drying under reduced pressure, with acid extraction thing and alcohol extract co-grinding, sprays into volatile oil, airtight placement.
Embodiment 13
Get any mixed extract 100g of embodiment 1-12, add the dextrin of 1.5 times of amounts, 0.5% sucrose, 1.5% microcrystalline Cellulose, make soft material with appropriate dissolve with ethanol, granulates, and 60 ℃ of forced air dryings, granulate, and granulate, obtain granule.
Embodiment 14
Get any mixed extract 100g of embodiment 1-12, add the Polyethylene Glycol of 1000g, mix homogeneously, melting, upper pill dripping machine, make drop pill.
Embodiment 15
Get any mixed extract 100g of embodiment 1-12, add 5% polyvinylpolypyrrolidone, 0.1% magnesium stearate, 50% microcrystalline Cellulose, make soft material with appropriate alcoholic solution, granulate, 60 ℃ of forced air dryings, granulate, granulate, compacting in flakes, obtains oral cavity disintegration tablet.
Embodiment 16
Get any mixed extract 0.5g of embodiment 1-12, glucose 4.5g, sodium thiosulfate 0.9g and distilled water 1ml, after the said components mix homogeneously, lyophilization, 500 of packing, obtain injectable powder.
Embodiment 17
Get any mixed extract 100g of embodiment 1-12, add equivalent starch, sucrose and magnesium stearate, granulate, and incapsulates, and obtains capsule.
Embodiment 18
Get any extract 100g of embodiment 1-12, with starch, sodium carboxymethyl cellulose, Pulvis Talci mix homogeneously, granulate, and tabletting obtains tablet.
Embodiment 19
Get any mixed extract 2g of embodiment 1-12, with syrup 4g, be dissolved in the pure water of 100ml, homogenizing, filter, through high-temperature short-time sterilization (135 ℃, 4s).Sterile filling, packing.Make oral liquid.
Embodiment 20
1) get the crude drug of following weight portion: 157 parts of Concha Ostreaes, 235.6 parts of the Radixs Astragali, 31.4 parts of Rhizoma Sparganii, 26.2 parts, Fructus Hordei Germinatus, 157 parts of Radix Asparagis, 62.8 parts of Myrrhas, 157 parts of Herba Epimedii, 157 parts of Radix Salviae Miltiorrhizaes, 31.4 parts of the Rhizoma Atractylodis Macrocephalaes, 157 parts of Sargassums, 31.4 parts of Radix Bupleuri, 31.4 parts of Rhizoma Curcumae, 42 parts of Endothelium Corneum Gigeriae Galli, 31.4 parts, Pericarpium Citri Reticulatae Viride, 31.4 parts of Olibanums;
2) Concha Ostreae powder of getting weight portion described in step 1 is broken into coarse powder, adds 5 times of amounts and adjusts the sour water of pH value to 2-3 with glacial acetic acid, decocts secondary, and each 2 hours, filter, filtrate is concentrated into dry, after drying, pulverizes to obtain the acid extraction thing;
3) get water soaking that Rhizoma Sparganii, the Rhizoma Atractylodis Macrocephalae, Radix Bupleuri, the Rhizoma Curcumae of weight portion described in step 1 add 10 times of amounts after 3 hours, with extraction by steam distillation volatile oil 6 hours, minute get volatile oil, another device is preserved; Decoction liquor filters, and the decocting that medicinal residues add 10 times of amounts boils secondary, and each 2 hours, filter, merge decoction liquor and obtain the first water extract;
4) get Myrrha, Herba Epimedii, Radix Salviae Miltiorrhizae, Pericarpium Citri Reticulatae Viride, the 80% alcohol reflux secondary for Olibanum of weight portion described in step 1, the alcohol reflux 3 hours that adds for the first time 8 times of amounts, the alcohol reflux 2 hours that adds for the second time 6 times of amounts, merge secondary raffinate, filter, reclaim ethanol to the thick paste shape, drying under reduced pressure obtains alcohol extract; The decocting that medicinal residues add 10 times of amounts boils secondary, and each 2 hours, filter, merge decoction liquor and obtain the second water extract;
5) decocting that the Radix Astragali, Fructus Hordei Germinatus, Radix Asparagi, Sargassum, the Endothelium Corneum Gigeriae Galli of getting weight portion described in step 1 adds 10 times of amounts boils secondary, and each 2 hours, merge the secondary decoction liquor, filter to obtain the 3rd water extract, standby;
6) first and second and three water extracts are merged, when being evaporated to 60 ℃ of relative densities and being 1.25-1.35 and acid extraction thing and alcohol extract combination drying pulverize, add one or more in appropriate amount of starch, cross linked polyvinyl pyrrolidone, polyvinylpyrrolidone, micropowder silica gel, granulate, spray into volatile oil, 24h is placed in sealing, incapsulates.
Embodiment 21
1) get 157 parts of Concha Ostreaes, 235.6 parts of the Radixs Astragali, 31.4 parts of Rhizoma Sparganii, 26.2 parts, Fructus Hordei Germinatus, 157 parts of Radix Asparagis, 62.8 parts of Myrrhas, 157 parts of Herba Epimedii, 157 parts of Radix Salviae Miltiorrhizaes, 31.4 parts of the Rhizoma Atractylodis Macrocephalaes, 157 parts of Sargassums, 31.4 parts of Radix Bupleuri, 31.4 parts of Rhizoma Curcumae, 42 parts of Endothelium Corneum Gigeriae Galli, 31.4 parts, Pericarpium Citri Reticulatae Viride, 31.4 parts of Olibanums, for following step;
2) get Concha Ostreae acid adding decocting and boil, filter, filtrate is concentrated into dry, and crushed after being dried obtains the acid extraction thing, standby;
3) get Rhizoma Sparganii, Radix Bupleuri, the Rhizoma Atractylodis Macrocephalae, Rhizoma Curcumae and soak, with extraction by steam distillation volatile oil, minute get volatile oil standby; Decoction liquor filters, and medicinal residues decoct with water filtration, merges decoction liquor, obtains the first water extract, standby;
4) get Myrrha, Herba Epimedii, Radix Salviae Miltiorrhizae, Pericarpium Citri Reticulatae Viride, Olibanum alcohol reflux, filter, reclaim ethanol to the thick paste shape, drying under reduced pressure obtains alcohol extract, standby; Medicinal residues decoct with water filtration, merge decoction liquor and obtain the second water extract, standby;
5) get the Radix Astragali, Fructus Hordei Germinatus, Radix Asparagi, Sargassum, Endothelium Corneum Gigeriae Galli and decoct with water and filter to obtain the 3rd water extract, standby;
6) first and second and three water extracts are merged, concentrating under reduced pressure and acid extraction thing and alcohol extract co-grinding, add appropriate amount of auxiliary materials as one or more in starch, cross linked polyvinyl pyrrolidone, polyvinylpyrrolidone, micropowder silica gel, granulate, spray into volatile oil, sealing is placed, and incapsulates.
Embodiment 22
1) get the crude drug of following weight portion: 157 parts of Concha Ostreaes, 235.6 parts of the Radixs Astragali, 31.4 parts of Rhizoma Sparganii, 26.2 parts, Fructus Hordei Germinatus, 157 parts of Radix Asparagis, 62.8 parts of Myrrhas, 157 parts of Herba Epimedii, 157 parts of Radix Salviae Miltiorrhizaes, 31.4 parts of the Rhizoma Atractylodis Macrocephalaes, 157 parts of Sargassums, 31.4 parts of Radix Bupleuri, 31.4 parts of Rhizoma Curcumae, 42 parts of Endothelium Corneum Gigeriae Galli, 31.4 parts, Pericarpium Citri Reticulatae Viride, 31.4 parts of Olibanums;
2) Concha Ostreae powder of getting weight portion described in step 1 is broken into coarse powder, adds 5 times of amounts and adjusts the sour water of pH value to 2-3 with glacial acetic acid, decocts secondary, and each 2 hours, filter, filtrate is concentrated into dry, after drying, pulverizes to obtain the acid extraction thing;
3) get water soaking that Rhizoma Sparganii, the Rhizoma Atractylodis Macrocephalae, Radix Bupleuri, the Rhizoma Curcumae of weight portion described in step 1 add 10 times of amounts after 3 hours, with extraction by steam distillation volatile oil 6 hours, minute get volatile oil, another device is preserved; Decoction liquor filters, and the decocting that medicinal residues add 10 times of amounts boils secondary, and each 2 hours, filter, merge decoction liquor and obtain the first water extract;
4) get Myrrha, Herba Epimedii, Radix Salviae Miltiorrhizae, Pericarpium Citri Reticulatae Viride, the 80% alcohol reflux secondary for Olibanum of weight portion described in step 1, the alcohol reflux 3 hours that adds for the first time 8 times of amounts, the alcohol reflux 2 hours that adds for the second time 6 times of amounts, merge secondary raffinate, filter, reclaim ethanol to the thick paste shape, drying under reduced pressure obtains alcohol extract; The decocting that medicinal residues add 10 times of amounts boils secondary, and each 2 hours, filter, merge decoction liquor and obtain the second water extract;
5) decocting that the Radix Astragali, Fructus Hordei Germinatus, Radix Asparagi, Sargassum, the Endothelium Corneum Gigeriae Galli of getting weight portion described in step 1 adds 10 times of amounts boils secondary, and each 2 hours, merge the secondary decoction liquor, filter to obtain the 3rd water extract, standby;
6) first and second and three water extracts are merged, pulverize with acid extraction thing and alcohol extract combination drying when being evaporated to 60 ℃ of relative densities and being 1.25-1.35, add appropriate amount of auxiliary materials, granulate, spray into volatile oil, sealing placement, the soft capsule of packing into.
Claims (6)
1. a preparation method for the treatment of the Chinese medicine composition of nodules of the breast is characterized in that preparation method is as follows:
1) get the crude drug of following weight portion: Concha Ostreae 130-160 part, Radix Astragali 210-250 part, Rhizoma Sparganii 20-40 part, Fructus Hordei Germinatus 20-30 part, Radix Asparagi 140-170 part, Myrrha 50-70 part, Herba Epimedii 140-170 part, Radix Salviae Miltiorrhizae 140-170 part, Rhizoma Atractylodis Macrocephalae 20-40 part, Sargassum 140-170 part, Radix Bupleuri 20-40 part, Rhizoma Curcumae 20-40 part, Endothelium Corneum Gigeriae Galli 30-50 part, Pericarpium Citri Reticulatae Viride 20-40 part, Olibanum 20-40 part;
The Concha Ostreae of 2) getting weight portion described in step 1 adds acid extraction, obtains the acid extraction thing;
3) get Rhizoma Sparganii, Radix Bupleuri, the Rhizoma Atractylodis Macrocephalae, the Rhizoma Curcumae of weight portion described in step 1, mixed extraction volatile oil, the medicinal residues extracting in water, obtain the first water extract;
4) get Myrrha, Herba Epimedii, Radix Salviae Miltiorrhizae, Pericarpium Citri Reticulatae Viride, the Olibanum ethanol extraction of weight portion described in step 1, obtain alcohol extract; The medicinal residues extracting in water obtains the second water extract;
5) get the Radix Astragali, Fructus Hordei Germinatus, Radix Asparagi, Sargassum, Endothelium Corneum Gigeriae Galli extracting in water and obtain the 3rd water extract;
6) above-mentioned first and second merged and concentrate with three water extracts, after the concentrate drying under reduced pressure, with acid extraction thing and alcohol extract co-grinding, spray into volatile oil, sealing is placed.
2. the preparation method of Chinese medicine composition as claimed in claim 1 is characterized in that preparation method is as follows:
1) get the crude drug of following weight portion: Concha Ostreae 140-160 part, Radix Astragali 215-245 part, Rhizoma Sparganii 25-35 part, Fructus Hordei Germinatus 23-28 part, Radix Asparagi 150-160 part, Myrrha 55-70 part, Herba Epimedii 145-165 part, Radix Salviae Miltiorrhizae 145-165 part, Rhizoma Atractylodis Macrocephalae 25-35 part, Sargassum 145-165 part, Radix Bupleuri 25-35 part, Rhizoma Curcumae 25-35 part, Endothelium Corneum Gigeriae Galli 35-50 part, Pericarpium Citri Reticulatae Viride 25-35 part, Olibanum 25-40 part;
2) the Concha Ostreae acid adding decocting of getting weight portion described in step 1 boils 1-3 time, and each 1-3 hour, filter, and obtains the acid extraction thing;
3) Rhizoma Sparganii, Radix Bupleuri, the Rhizoma Atractylodis Macrocephalae, the Rhizoma Curcumae of getting weight portion described in step 1 are soaked 2-4 hour, extract volatile oil, minute get volatile oil standby; Medicinal residues decoct with water 1-3 time, and each 1-3 hour, filter, and merges decoction liquor, obtains the first water extract;
4) get Myrrha, Herba Epimedii, Radix Salviae Miltiorrhizae, Pericarpium Citri Reticulatae Viride, the Olibanum alcohol reflux 1-3 time of weight portion described in step 1, merge extractive liquid,, reclaim ethanol to the thick paste shape, and drying under reduced pressure obtains alcohol extract; Medicinal residues decoct with water 1-3 time, and each 1-3 hour merges decoction liquor and obtains the second water extract;
5) Radix Astragali, Fructus Hordei Germinatus, Radix Asparagi, Sargassum, the Endothelium Corneum Gigeriae Galli of getting weight portion described in step 1 decoct with water 1-3 time, and each 1-3 hour, merge decoction liquor, filters to obtain the 3rd water extract;
6) first and second and three water extracts are merged to concentrating under reduced pressure, after the concentrate drying under reduced pressure, with acid extraction thing and alcohol extract co-grinding, spray into volatile oil, sealing is placed.
3. the preparation method of Chinese medicine composition as claimed in claim 1 is characterized in that preparation method is as follows:
1) get the crude drug of following weight portion: Concha Ostreae 150-160 part, Radix Astragali 220-240 part, Rhizoma Sparganii 25-35 part, Fructus Hordei Germinatus 23-28 part, Radix Asparagi 150-160 part, Myrrha 60-65 part, Herba Epimedii 150-160 part, Radix Salviae Miltiorrhizae 150-160 part, Rhizoma Atractylodis Macrocephalae 28-32 part, Sargassum 150-160 part, Radix Bupleuri 25-35 part, Rhizoma Curcumae 25-35 part, Endothelium Corneum Gigeriae Galli 40-45 part, Pericarpium Citri Reticulatae Viride 30-35 part, Olibanum 30-35 part;
2) the Concha Ostreae acid adding decocting of getting weight portion described in step 1 boils 1-3 time, and each 1-3 hour, filter, and filtrate is concentrated into dry, and crushed after being dried obtains the acid extraction thing;
3), after Rhizoma Sparganii, Radix Bupleuri, the Rhizoma Atractylodis Macrocephalae, the Rhizoma Curcumae of getting weight portion described in step 1 soaked 2-4 hour, with extraction by steam distillation volatile oil 5-7 hour, minute get volatile oil standby; Decoction liquor filters, and medicinal residues decoct with water 1-3 time, and each 1-3 hour, filter, and merges decoction liquor, obtains the first water extract;
4) get Myrrha, Herba Epimedii, Radix Salviae Miltiorrhizae, Pericarpium Citri Reticulatae Viride, the Olibanum 70-90% alcohol reflux secondary of weight portion described in step 1, merge secondary raffinate, filter, reclaim ethanol to the thick paste shape, drying under reduced pressure obtains alcohol extract, standby; Medicinal residues decoct with water secondary, and each 1-3 hour, filter, and merge decoction liquor and obtain the second water extract;
5) Radix Astragali, Fructus Hordei Germinatus, Radix Asparagi, Sargassum, the Endothelium Corneum Gigeriae Galli of getting weight portion described in step 1 decoct with water 1-3 time, and each 1-3 hour, merge the secondary decoction liquor, filters to obtain the 3rd water extract;
6) first and second and three water extracts are merged to concentrating under reduced pressure, after the concentrate drying under reduced pressure, with acid extraction thing and alcohol extract co-grinding, spray into volatile oil, sealing is placed.
4. the preparation method of Chinese medicine composition as claimed in claim 1 is characterized in that preparation method is as follows:
1) get the crude drug of following weight portion: 157 parts of Concha Ostreaes, 235.6 parts of the Radixs Astragali, 31.4 parts of Rhizoma Sparganii, 26.2 parts, Fructus Hordei Germinatus, 157 parts of Radix Asparagis, 62.8 parts of Myrrhas, 157 parts of Herba Epimedii, 157 parts of Radix Salviae Miltiorrhizaes, 31.4 parts of the Rhizoma Atractylodis Macrocephalaes, 157 parts of Sargassums, 31.4 parts of Radix Bupleuri, 31.4 parts of Rhizoma Curcumae, 42 parts of Endothelium Corneum Gigeriae Galli, 31.4 parts, Pericarpium Citri Reticulatae Viride, 31.4 parts of Olibanums, for following step;
2) Concha Ostreae powder of getting weight portion described in step 1 is broken into coarse powder, adds 5 times of amounts and adjusts the sour water of pH value to 2-3 with glacial acetic acid, decocts secondary, and each 2 hours, filter, filtrate is concentrated into dry, after drying, pulverizes to obtain the acid extraction thing;
3) get water soaking that Rhizoma Sparganii, the Rhizoma Atractylodis Macrocephalae, Radix Bupleuri, the Rhizoma Curcumae of weight portion described in step 1 add 10 times of amounts after 3 hours,
With extraction by steam distillation volatile oil 6 hours, minute get volatile oil, another device is preserved; Decoction liquor filters, and the decocting that medicinal residues add 10 times of amounts boils secondary, and each 2 hours, filter, merge decoction liquor and obtain the first water extract;
4) get Myrrha, Herba Epimedii, Radix Salviae Miltiorrhizae, Pericarpium Citri Reticulatae Viride, the 80% alcohol reflux secondary for Olibanum of weight portion described in step 1, the alcohol reflux 3 hours that adds for the first time 8 times of amounts, the alcohol reflux 2 hours that adds for the second time 6 times of amounts, merge secondary raffinate, filter, reclaim ethanol to the thick paste shape, drying under reduced pressure obtains alcohol extract; The decocting that medicinal residues add 10 times of amounts boils secondary, and each 2 hours, filter, merge decoction liquor and obtain the second water extract;
5) decocting that the Radix Astragali, Fructus Hordei Germinatus, Radix Asparagi, Sargassum, the Endothelium Corneum Gigeriae Galli of getting weight portion described in step 1 adds 10 times of amounts boils secondary, and each 2 hours, merge the secondary decoction liquor, filter to obtain the 3rd water extract, standby;
6) first and second and three water extracts are merged, when being evaporated to 60 ℃ of relative densities and being 1.25-1.35, after drying under reduced pressure, with acid extraction thing and alcohol extract co-grinding, spray into volatile oil, sealing is placed.
5. according to the preparation method of the described Chinese medicine composition of claim 1-4, it is characterized in that adding pharmaceutically acceptable carrier to make following preparation this pharmaceutical composition: capsule, pill, granule, tablet, suspensoid, microcapsule.
6. as the preparation method of the described pharmaceutical composition of claim 1-4, it is characterized in that its formulation method is: first and second and three water extracts are merged, concentrating under reduced pressure, after drying under reduced pressure with acid extraction thing and alcohol extract co-grinding, add one or more in starch, crospolyvinylpyrrolidone, polyvinylpyrrolidone, micropowder silica gel, granulate, spray into volatile oil, sealing is placed, and incapsulates.
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| 乳安合剂的制备与质量标准研究;谭建伟等;《中国药房》;20071130;第18卷(第33期);2588-2590 * |
| 从牡蛎壳中提取生物糖蛋白的分析研究;尹德胜等;《广州化工》;20091231;第37卷(第9期);143-144 * |
| 尹德胜等.从牡蛎壳中提取生物糖蛋白的分析研究.《广州化工》.2009,第37卷(第9期),143-144. |
| 谭建伟等.乳安合剂的制备与质量标准研究.《中国药房》.2007,第18卷(第33期),2588-2590. |
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