CN102579869B - Preparation method of traditional Tibetan medicine composition for treating liver diseases - Google Patents
Preparation method of traditional Tibetan medicine composition for treating liver diseases Download PDFInfo
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Abstract
The invention relates to a preparation method of a traditional Tibetan medicine composition for treating liver diseases, which comprises the following steps: extracting and including volatile oil, extracting with ethanol, pulverizing the medicinal materials into fine powder, forming the preparation and the like. Compared with the traditional preparation, the medicine application compliance of the patient can be obviously enhanced. The pharmaceutical preparation prepared by the method provided by the invention can implement high absorption speed, quick effect taking and high bioavailability on the premise of reserving the drug effect of the original preparation; the effective ingredient can reach to the focus position centrally; and the pharmaceutical preparation has favorable curative effect.
Description
Technical field
The present invention relates to a kind of preparation method of Tibetan medicinal composition, particularly a kind of preparation method that is used for the treatment of the Tibetan medicinal composition of hepatopathy, belong to the Tibetan medicinal preparation field.
Background technology
Liver is the metabolism center of human body, is one of important organ of sustaining life, the health of its functional status substantial connection human body, and liver cell is damaged, and the function of liver suffers damage, and may cause that the series of health is not suitable with symptom.Hepatitis belongs to the traditional Chinese medical science " hepatopathy " category, and hepatopathy is many by the poison of experiencing the epidemic disease turbid damp; Or eating and drinking without temperance, impairing the spleen and stomach, so that essential substances from water and cereals dysfunction of the spleen in transportation and transformation, the turbid damp internal resistance, hot and suffocating heat-transformation and make damp and hot mixedly mutually, taste are stopped up resistance, and depression of liver-QI can not catharsis; Or, by internal injury caused by excess of seven emotions, liver is lost transport; Or stagnated QI transforming into fire, stagnation in liver meridian; Or deficiency of YIN-blood, liver-yang is partially high, and retention of damp-heat in the interior, and the accumulation of cold in liver meridian forms this disease; Or the urgent bile of heat leaks; Or depression of liver-QI, with the passing of time hinder network, the blood stasis retardance, cause bile excretion not smooth, and bile leaks, and overflowing in skin is jaundice.The right rib distending pain of clinical main manifestations, according to by, inappetence, myasthenia of limbs, vomiting, headache, dizzy, tinnitus, conjunctival congestion, irritability, whole body jaundice, liver enlargement etc.According to statistics, the number that hbs antigen is carried in the whole world surpasses 2.8 hundred million, and China is hepatitis big country, and in population of China, 8-10% being arranged at present is hepatitis B virus carriers, and still has a considerable amount of newly-increased patients every year.
The smooth capsule of liver is that gold is scolded the exclusive product of Tibetan medicine limited company, records in Chinese patent medicine provincial standard rising national standard part, standard number: WS-10927 (ZD-0927)-2002.The smooth capsule preparations of liver is to be made by the medical material of following weight proportion: tophus 20.1g, Concretio Silicea Bambusae 20.1g, Flos Carthami 40.0g, Stigma Croci 8.0g, Herba meconopsis integrifoliae 59.6g, tangut dragonhead 40.1g, Corydalis impatiens (Pall.) Fisch. 40.1g, Mumiyah-asil 40.1g, Flos Caryophylli 20.1g, artificial Calculus Bovis 4.0g, Indian Herba Swertiae bimaculatae 20.1g, Herpetospermum caudigerum Wall. 12.0g, Radix Aucklandiae Fructus Aristolochiae 12.0g, Parmelia saxatilis Ach. 4.0g, Moschus 1.6g, Vermilion 1.7g.
The smooth capsule of liver is due to respond well, and considered patient's physiology, pathological characteristic, through clinical verification, evident in efficacy.Yet, the simple physical processing that prior art all adopts the raw medicinal material pulverizing, mixes about the preparation method of the smooth medicine of liver, the raw material the effective elements of the medicine discharges slowly, badly influence absorbing of effective ingredient, need badly and introduce modern preparation method, Fast Stripping, onset are provided, absorb the smooth preparation of better liver.
Summary of the invention
The present invention is directed to the deficiencies in the prior art, a kind of preparation method for the treatment of the Tibetan medicinal composition preparation of hepatopathy is provided.
Technical scheme of the present invention is as follows:
A kind of preparation method for the treatment of the Tibetan medicinal composition preparation of hepatopathy, the raw material medicines in portions by weight of described pharmaceutical composition consists of: tophus 10-30 part, Concretio Silicea Bambusae 10-30 part, Flos Carthami 20-60 part, Stigma Croci 4-10 part, Herba meconopsis integrifoliae 25-75 part, tangut dragonhead 15-50 part, Corydalis impatiens (Pall.) Fisch. 15-50 part, Mumiyah-asil 15-50 part, Flos Caryophylli 10-30 part, artificial Calculus Bovis 2-5 part, Indian Herba Swertiae bimaculatae 10-30 part, Herpetospermum caudigerum Wall. 5-15 part, Parmelia saxatilis Ach. 2-5 part, artificial Moschus 1-3 part; Comprise the following steps:
(1) get Flos Caryophylli by the crude drug composition and ratio, add water 4-10 times weight, adopt steam distillation, extract volatile oil 3-6h, collect volatile oil, medicinal liquid filters, and obtains extracting solution A ' and medicinal residues A;
The volatile oil that collection is obtained adds in the beta cyclodextrin saturated aqueous solution of percent weight in volume 3-4%, the envelope-bulk to weight ratio of volatile oil and beta cyclodextrin is 1ml: 3-5g, under stirring condition, keep 40 ℃-60 ℃ of temperature, stir 3～4h ,-4 ℃ of-4 ℃ of cold preservations are spent the night, sucking filtration, precipitation, 40 ℃ of-60 ℃ of vacuum dryings, obtain volatile oil clathrate compound;
(2) get tangut dragonhead by the crude drug composition and ratio, Flos Carthami, Herba meconopsis integrifoliae, Corydalis impatiens (Pall.) Fisch., Indian Herba Swertiae bimaculatae, Herpetospermum caudigerum Wall., Parmelia saxatilis Ach. is totally 7 flavor medical materials, with the medicinal residues A after step (1) is extracted volatile oil, mix, add the alcoholic solution B of volumetric concentration 30%～100% to extract 2-3 time, temperature 50 C-100 ℃, the amount that at every turn adds alcoholic solution B is described 7 flavor medical materials and medicinal residues A gross weight 8-10 times, extract 2-3h, filter, with the extracting solution A ' after step (1) extraction volatile oil, merge, concentrating under reduced pressure, be concentrated into the fluid extract that under medicinal liquid that under 25 ℃ of conditions, relative density is 1.06-1.12 or 60 ℃ of conditions, relative density is 1.20-1.40, perhaps,
Get tangut dragonhead by the crude drug composition and ratio, Flos Carthami, Herba meconopsis integrifoliae, Corydalis impatiens (Pall.) Fisch., Indian Herba Swertiae bimaculatae, Herpetospermum caudigerum Wall., Parmelia saxatilis Ach. is totally 7 flavor medical materials, mix, be ground into the 0.5mm-2mm fine powder, with the medicinal residues A after Flos Caryophylli is extracted volatile oil, mix, the alcoholic solution B that adds volumetric concentration 30%～100%, soak 6-12h, with alcoholic solution B percolation, extract, institute's consumption is described 7 flavor medical materials and medicinal residues A gross weight 10-30 times, collect the percolation medicinal liquid, with the extracting solution A ' after Flos Caryophylli extraction volatile oil, merge, temperature is lower than under 60 ℃ of conditions, concentrating under reduced pressure, be concentrated into the fluid extract that under medicinal liquid that under 25 ℃ of conditions, relative density is 1.06-1.12 or 60 ℃ of conditions, relative density is 1.20-1.40, perhaps,
Get tangut dragonhead by the crude drug composition and ratio, Flos Carthami, Herba meconopsis integrifoliae, Corydalis impatiens (Pall.) Fisch., Indian Herba Swertiae bimaculatae, Herpetospermum caudigerum Wall., Parmelia saxatilis Ach. is totally 7 flavor medical materials, with the medicinal residues A after step (1) is extracted volatile oil, mix, add water extraction 2-3 time, temperature 50 C-100 ℃, the amount that at every turn adds water is described 7 flavor medical materials and medicinal residues A gross weight 8-10 times, extract 2-3h, filter, with the extracting solution A ' after step (1) extraction volatile oil, merge, concentrating under reduced pressure, be concentrated into the fluid extract that under medicinal liquid that under 25 ℃ of conditions, relative density is 1.06-1.12 or 60 ℃ of conditions, relative density is 1.20-1.40,
(3) get the fluid extract that under 60 ℃ of conditions of step (2) gained, relative density is 1.20-1.40, drying, obtain ethanol extraction C; Perhaps,
Get the medicinal liquid that under 25 ℃ of conditions of step (2) gained, relative density is 1.06-1.12, filter, macroporous resin adsorption 2～12h by 0.2～1 times of medicinal liquid weight, then use the water elution of 2～8 times of amounts of macroporous resin volume, use successively again the ethanol elution of the variable concentrations of 2～8 times of macroporous resin volumes, eluting is respectively 10% ethanol by the volumetric concentration of ethanol, 30% ethanol, 50% ethanol, 70% ethanol, 95% ethanol elution, collect respectively eluent, merge standby, eluent concentrating under reduced pressure after merging reclaims ethanol, collection is concentrated into the fluid extract of relative density 1.20-1.40 under 60 ℃ of conditions, dry, obtain purification by macroporous resin extract D,
(4) get tophus, Concretio Silicea Bambusae, Stigma Croci, Mumiyah-asil, artificial Calculus Bovis, artificial Moschus by the crude drug composition and ratio, totally 6 flavor medical materials, be ground into 1-200 μ m, obtains the medical material fine powder; Perhaps,
Get tophus, Concretio Silicea Bambusae, Stigma Croci, Mumiyah-asil, artificial Calculus Bovis, artificial Moschus by the crude drug composition and ratio, totally 6 the flavor medical materials, the alcoholic solution B that adds volumetric concentration 30%～100%, soak 6-12h, with alcoholic solution B percolation, extracts, institute's consumption is 10-30 times of described 6 flavor medical material gross weights, collect the percolation medicinal liquid, temperature is lower than under 60 ℃ of conditions, concentrating under reduced pressure, drying, obtain extract E; Perhaps,
Get tophus, Concretio Silicea Bambusae, Stigma Croci, Mumiyah-asil, artificial Calculus Bovis, artificial Moschus by the crude drug composition and ratio, totally 6 the flavor medical materials, add the alcoholic solution B of volumetric concentration 30%～100% to extract 2-3 time, temperature 50 C-100 ℃, the amount that at every turn adds alcoholic solution B is 8-10 times of described 6 flavor medical material gross weights, extracts 2-3h, filter, the medicinal liquid concentrating under reduced pressure, drying, obtain extract F;
(5) the medical material fine powder that the ethanol extraction C that volatile oil clathrate compound above-mentioned steps (1) made, step (3) make or purification by macroporous resin extract D, step (4) make or extract E or extract F mix, add conventional adjuvant, according to common process, be prepared into pharmaceutically acceptable any dosage form.
The preferred HPD600 of macroporous resin, LSA-21, LSA-40, DM130 type for adsorbing in above-mentioned steps (3).
Preferred according to the present invention, the raw material medicines in portions by weight of described pharmaceutical composition consists of: tophus 15-20 part, Concretio Silicea Bambusae 15-20 part; Flos Carthami 42-47 part, Stigma Croci 4-7 part, Herba meconopsis integrifoliae 50-55 part; tangut dragonhead 30-37 part, Corydalis impatiens (Pall.) Fisch. 30-37 part, Mumiyah-asil 30-39 part; Flos Caryophylli 10-18 part; artificial Calculus Bovis 2-3.5 part, Indian Herba Swertiae bimaculatae 15-18 part, Herpetospermum caudigerum Wall. 5-11 part; Parmelia saxatilis Ach. 2-3.5 part, artificial Moschus 1-1.5 part.
Further preferred, the raw material medicines in portions by weight of described pharmaceutical composition consists of: 17.6 parts of tophuss, 17.6 parts of Concretio Silicea Bambusaes; 43.7 parts, Flos Carthami, 7 parts of Stigma Crocis, 52 parts of Herba meconopsis integrifoliae; 35 parts of tangut dragonheads, 35 parts of Corydalis impatiens (Pall.) Fisch.s, 38.2 parts of Mumiyah-asil; 17.6 parts of Flos Caryophyllis; 3.5 parts of artificial Calculus Boviss, 17.6 parts of Indian Herba Swertiae bimaculataes, 10.5 parts of Herpetospermum caudigerum Wall.s; 3.5 parts of Parmelia saxatilis Ach., 1.4 parts of artificial Moschuss.
Preferred according to the present invention, the preparation method of the Tibetan medicinal composition capsule of the present invention's treatment hepatopathy comprises the following steps:
(1) get Flos Caryophylli by the crude drug composition and ratio, add 6 times of weight of water, adopt steam distillation, extract volatile oil 4h, collect volatile oil, obtain volatile oil, medicinal liquid filters, and obtains extracting solution A ' and medicinal residues A;
The volatile oil that collection is obtained adds in the beta cyclodextrin saturated aqueous solution of percent weight in volume 4%, the envelope-bulk to weight ratio of volatile oil and beta cyclodextrin is 1ml: 4g, under stirring condition, keep temperature 50 C, stir 4h ,-4 ℃ of cold preservations are spent the night, sucking filtration, precipitation, 5 ℃ of vacuum dryings, obtain volatile oil clathrate compound;
(2) get tangut dragonhead by the crude drug composition and ratio, Flos Carthami, Herba meconopsis integrifoliae, Corydalis impatiens (Pall.) Fisch., Indian Herba Swertiae bimaculatae, Herpetospermum caudigerum Wall., Parmelia saxatilis Ach. is totally 7 flavor medical materials, mix, be ground into 200 μ m fine powders, with the medicinal residues A after Flos Caryophylli is extracted volatile oil, mix, the alcoholic solution B that adds volumetric concentration 50%, soak 8h, with alcoholic solution B percolation, extract, institute's consumption is described 7 flavor medical materials and medicinal residues A gross weight 25 times, collect the percolation medicinal liquid, with the extracting solution A ' after Flos Caryophylli extraction volatile oil, merge, temperature is lower than under 60 ℃ of conditions, concentrating under reduced pressure, be concentrated into the medicinal liquid that under 25 ℃ of conditions, relative density is 1.10,
(3) get the medicinal liquid that under 25 ℃ of conditions of step (2) gained, relative density is 1.10, filter, HPD600 type macroporous resin adsorption 6h by 1/3 times of medicinal liquid weight, then use the water elution of 5 times of amounts of HPD600 type macroporous resin volume, use successively again the ethanol elution of the variable concentrations of 5 times of amounts of HPD600 type macroporous resin volume, eluting is respectively 10% ethanol by the volumetric concentration of ethanol, 30% ethanol, 50% ethanol, 70% ethanol, 95% ethanol elution, collect respectively eluent, merge, eluent concentrating under reduced pressure after merging reclaims ethanol, collection is concentrated into the fluid extract of relative density 1.20 under 60 ℃ of conditions, dry, obtain purification by macroporous resin extract D,
(4): by the crude drug composition and ratio, get tophus, Concretio Silicea Bambusae, Stigma Croci, Mumiyah-asil, artificial Calculus Bovis, artificial Moschus, totally 6 flavor medical materials, be ground into 50 μ m fine powders, adds the alcoholic solution B of volumetric concentration 80%, soak 12h, with alcoholic solution B percolation, extract, institute's consumption is 30 times of described 6 flavor medical material gross weights, collects the percolation medicinal liquid, temperature is lower than under 60 ℃ of conditions, concentrating under reduced pressure, drying, obtain extract E;
(5): the extract E that the purification by macroporous resin extract D that the volatile oil clathrate compound that above-mentioned steps (1) is made, step (3) make, step (4) make mixes, and adds conventional adjuvant, according to common process, is prepared into capsule.
The pass of weight portion of the present invention and parts by volume is g/ml or kg/l.
The present invention has following advantage:
1, characteristics of the present invention are to take the plant composition as material base, take drug activity as guidance, take into full account character, the clinical disease needs of ingredient, and the physiological conditions of medication object etc., adopt new extraction preparation method, be prepared from, compare with conventional formulation, pharmaceutical composition prepared by method of the present invention is under the prerequisite that retains former preparation drug effect, can realize the effective ingredient Fast Stripping, absorb, concentrate and arrive lesions position, improved availability.Specifically see the test example data declaration.
2, the volatile oil component of the present invention to the prescription medical material, carried out extracting protection, adopts the beta cyclodextrin clathrate process effectively to guarantee the stable of volatile oil active ingredient.Specifically see the test example data declaration.
3, the preparation method that the percolation adopted in the present invention extracts, can effectively protect thermally labile component.
The preparation method of the micronizing that 4, in the present invention, tophus, Concretio Silicea Bambusae, Stigma Croci, Mumiyah-asil, artificial Calculus Bovis, artificial Moschus etc. adopt, can realize fully absorbing the Fast Stripping of active ingredient.Specifically see the test example data declaration.
The preparation method of the purification by macroporous resin active ingredient 5, adopted in the present invention, can realize effective enrichment of effective ingredient, improves administration concentration, makes active ingredient be convenient to concentrate fast and arrive lesions position.Specifically see the test example data declaration.
6, the pharmaceutical composition that prepared by the present invention, having overcome prior art is crude drug and pulverizes and to be used as medicine, be not suitable for the shortcoming of modern formulation, adopt the pharmaceutical composition of modern technologies gained to can be used for the various modern dosage forms such as capsule, granule, oral liquid, drop pill, dispersible tablet.
The specific embodiment
Following embodiment and experimental example are for further illustrating but being not limited to the present invention.The smooth compositions of the liver of using in experimental example is the pharmaceutical composition of the treatment hepatopathy for preparing of the inventive method.
The raw material medicines in portions by weight proportioning of embodiment 1-5 pharmaceutical composition is as follows:
17.6 parts of tophuss, 17.6 parts of Concretio Silicea Bambusaes, 43.7 parts, Flos Carthami, 7 parts of Stigma Crocis, 52 parts of Herba meconopsis integrifoliae, 35 parts of tangut dragonheads, 35 parts of Corydalis impatiens (Pall.) Fisch.s, 38.2 parts of Mumiyah-asil, 17.6 parts of Flos Caryophyllis, 3.5 parts of artificial Calculus Boviss, 17.6 parts of Indian Herba Swertiae bimaculataes, 10.5 parts of Herpetospermum caudigerum Wall.s, 3.5 parts of Parmelia saxatilis Ach., 1.4 parts of artificial Moschuss.
The smooth capsule of former commercially available liver of use is that gold is scolded Tibetan medicine Pharmaceutical limited company product as a comparison.
The smooth pharmaceutical composition of experimental example 1 liver used is the pharmaceutical composition that embodiment 1-5 prepares.
The DM130 model resin Anhui Samsung resin Science and Technology Ltd. used in embodiment and experimental example is on sale; The precious grace chemical industry of HPD600, YWD-01 model resin Cangzhou company limited is on sale; X-5, NKA, ADS-F8, LS-300, D101 model resin Chemical Plant of Nankai Univ. are on sale; LSA-21LSA-40 model resin Xi'an Lanxiao Sci-Tech Co., Ltd. is on sale.
Embodiment 1, a kind of preparation for the treatment of the medicament composition capsule of hepatopathy
(1) get Flos Caryophylli by the crude drug composition and ratio, add 6 times of weight of water, adopt steam distillation, extract volatile oil 4h, collect volatile oil, obtain volatile oil, medicinal liquid filters, and obtains extracting solution A ' and medicinal residues A;
The volatile oil that collection is obtained adds in the beta cyclodextrin saturated aqueous solution of percent weight in volume 4%, the envelope-bulk to weight ratio of volatile oil and beta cyclodextrin is 1ml: 4g, under stirring condition, keep temperature 50 C, stir 4h ,-4 ℃ of cold preservations are spent the night, sucking filtration, precipitation, 5 ℃ of vacuum dryings, obtain volatile oil clathrate compound;
(2) get tangut dragonhead by the crude drug composition and ratio, Flos Carthami, Herba meconopsis integrifoliae, Corydalis impatiens (Pall.) Fisch., Indian Herba Swertiae bimaculatae, Herpetospermum caudigerum Wall., Parmelia saxatilis Ach. is totally 7 flavor medical materials, mix, be ground into 200 μ m fine powders, with the medicinal residues A after Flos Caryophylli is extracted volatile oil, mix, the alcoholic solution B that adds volumetric concentration 50%, soak 8h, with alcoholic solution B percolation, extract, institute's consumption is described 7 flavor medical materials and medicinal residues A gross weight 25 times, collect the percolation medicinal liquid, with the extracting solution A ' after Flos Caryophylli extraction volatile oil, merge, temperature is lower than under 60 ℃ of conditions, concentrating under reduced pressure, be concentrated into the medicinal liquid that under 25 ℃ of conditions, relative density is 1.10,
(3) get the medicinal liquid that under 25 ℃ of conditions of step (2) gained, relative density is 1.10, filter, HPD600 type macroporous resin adsorption 6h by 1/3 times of medicinal liquid weight, then use the water elution of 5 times of amounts of HPD600 type macroporous resin volume, use successively again the ethanol elution of the variable concentrations of 5 times of amounts of HPD600 type macroporous resin volume, eluting is respectively 10% ethanol by the volumetric concentration of ethanol, 30% ethanol, 50% ethanol, 70% ethanol, 95% ethanol elution, collect respectively eluent, merge, eluent concentrating under reduced pressure after merging is reclaimed to ethanol, collection is concentrated into the fluid extract of relative density 1.3 under 60 ℃ of conditions, dry, obtain purification by macroporous resin extract D,
(4) get tophus, Concretio Silicea Bambusae, Stigma Croci, Mumiyah-asil, artificial Calculus Bovis, artificial Moschus by the crude drug composition and ratio, totally 6 flavor medical materials, be ground into 50 μ m fine powders, adds the alcoholic solution B of volumetric concentration 80%, soak 12h, with alcoholic solution B percolation, extract, institute's consumption is 30 times of described 6 flavor medical material gross weights, collects the percolation medicinal liquid, temperature is lower than under 60 ℃ of conditions, concentrating under reduced pressure, drying, obtain extract E;
(5) the extract E that the purification by macroporous resin extract D that volatile oil clathrate compound above-mentioned steps (1) made, step (3) make, step (4) make mixes, and adds conventional adjuvant, according to common process, is prepared into capsule.
Embodiment 2, a kind of preparation for the treatment of the medicament composition granule agent of hepatopathy
(1) get Flos Caryophylli by the crude drug composition and ratio, add 8 times of weight of water, adopt steam distillation, extract volatile oil 6h, collect volatile oil, obtain volatile oil, medicinal liquid filters, and obtains extracting solution A ' and medicinal residues A;
The volatile oil that collection is obtained adds in the beta cyclodextrin saturated aqueous solution of percent weight in volume 3%, the envelope-bulk to weight ratio of volatile oil and beta cyclodextrin is 1ml: 5g, under stirring condition, keep temperature 60 C, stir 4h ,-4 ℃ of cold preservations are spent the night, sucking filtration, precipitation, 40 ℃ of vacuum dryings, obtain volatile oil clathrate compound;
(2) get tangut dragonhead, Flos Carthami, Herba meconopsis integrifoliae, Corydalis impatiens (Pall.) Fisch., Indian Herba Swertiae bimaculatae, Herpetospermum caudigerum Wall., Parmelia saxatilis Ach. totally 7 flavor medical materials by the crude drug composition and ratio, with the medicinal residues A after step (1) is extracted volatile oil, mix, add the alcoholic solution B of volumetric concentration 80% to extract 3 times, 80 ℃ of temperature, the amount that at every turn adds alcoholic solution B is described 7 flavor medical materials and medicinal residues A gross weight 8 times, extract 3h, filter, with the extracting solution A ' after step (1) extraction volatile oil, merge, concentrating under reduced pressure, be concentrated into the fluid extract that under 60 ℃ of conditions, relative density is 1.40;
(3) get the fluid extract that under 60 ℃ of conditions of step (2) gained, relative density is 1.40, drying, obtain ethanol extraction C;
(4) get tophus, Concretio Silicea Bambusae, Stigma Croci, Mumiyah-asil, artificial Calculus Bovis, artificial Moschus by the crude drug composition and ratio, totally 6 flavor medical materials, be ground into the 0.5mm fine powder, adds the alcoholic solution B of volumetric concentration 80%, soak 8h, with alcoholic solution B percolation, extract, institute's consumption is 30 times of described 6 flavor medical material gross weights, collects the percolation medicinal liquid, temperature is lower than under 60 ℃ of conditions, concentrating under reduced pressure, drying, obtain extract E;
(5) the extract E that the ethanol extraction C that volatile oil clathrate compound above-mentioned steps (1) made, step (3) make, step (4) make mixes, and adds conventional adjuvant, according to common process, is prepared into granule.Embodiment 3, a kind of preparation for the treatment of the medicinal composition tablets of hepatopathy
(1) get Flos Caryophylli by the crude drug composition and ratio, add 5 times of weight of water, adopt steam distillation, extract volatile oil 3h, collect volatile oil, obtain volatile oil, medicinal liquid filters, and obtains extracting solution A ' and medicinal residues A;
The volatile oil that collection is obtained adds in the beta cyclodextrin saturated aqueous solution of percent weight in volume 3%, the envelope-bulk to weight ratio of volatile oil and beta cyclodextrin is 1ml: 4g, under stirring condition, keep temperature 60 C, stir 4h, 4 ℃ of cold preservations are spent the night, sucking filtration, precipitation, 60 ℃ of vacuum dryings, obtain volatile oil clathrate compound;
(2) get tangut dragonhead, Flos Carthami, Herba meconopsis integrifoliae, Corydalis impatiens (Pall.) Fisch., Indian Herba Swertiae bimaculatae, Herpetospermum caudigerum Wall., Parmelia saxatilis Ach. totally 7 flavor medical materials by the crude drug composition and ratio, with the medicinal residues A after step (1) is extracted volatile oil, mix, add the water reflux, extract, 3 times,, the amount that at every turn adds water is described 7 flavor medical materials and medicinal residues A gross weight 10 times, extracts 2h, filter, with the extracting solution A ' after step (1) extraction volatile oil, merge, concentrating under reduced pressure, be concentrated into the medicinal liquid that under 25 ℃ of conditions, relative density is 1.10;
(3) get the medicinal liquid that under 25 ℃ of conditions of step (2) gained, relative density is 1.10, filter, LSA-21 type macroporous resin adsorption 8h by 1/6 times of medicinal liquid weight, then use the water elution of 8 times of amounts of LSA-21 type macroporous resin volume, use successively again the ethanol elution of the variable concentrations of 8 times of LSA-21 type macroporous resin volumes, eluting is respectively 10% ethanol by the volumetric concentration of ethanol, 30% ethanol, 50% ethanol, 70% ethanol, 95% ethanol elution, collect respectively eluent, merge standby, eluent concentrating under reduced pressure after merging is reclaimed to ethanol, collection is concentrated into the fluid extract of relative density 1.40 under 60 ℃ of conditions, dry, obtain purification by macroporous resin extract D,
(4) get tophus, Concretio Silicea Bambusae, Stigma Croci, Mumiyah-asil, artificial Calculus Bovis, artificial Moschus by the crude drug composition and ratio, totally 6 flavor medical materials, be ground into 50 μ m, obtains the medical material fine powder;
(5) the medical material fine powder that the purification by macroporous resin extract D that volatile oil clathrate compound above-mentioned steps (1) made, step (3) make, step (4) make mixes, and adds conventional adjuvant, according to common process, is prepared into tablet.
Embodiment 4, a kind of preparation for the treatment of the pharmaceutical composition pill of hepatopathy
(1) get Flos Caryophylli by the crude drug composition and ratio, add 6 times of weight of water, adopt steam distillation, extract volatile oil 4h, collect volatile oil, obtain volatile oil, medicinal liquid filters, and obtains extracting solution A ' and medicinal residues A;
The volatile oil that collection is obtained adds in the beta cyclodextrin saturated aqueous solution of percent weight in volume 4%, the envelope-bulk to weight ratio of volatile oil and beta cyclodextrin is 1ml: 4g, under stirring condition, keep temperature 50 C, stir 4h ,-4 ℃ of cold preservations are spent the night, sucking filtration, precipitation, 50 ℃ of vacuum dryings, obtain volatile oil clathrate compound;
(2) get tangut dragonhead, Flos Carthami, Herba meconopsis integrifoliae, Corydalis impatiens (Pall.) Fisch., Indian Herba Swertiae bimaculatae, Herpetospermum caudigerum Wall., Parmelia saxatilis Ach. totally 7 flavor medical materials by the crude drug composition and ratio, with the medicinal residues A after step (1) is extracted volatile oil, mix, the alcoholic solution B reflux, extract, 3 times that adds volumetric concentration 60%, the amount that at every turn adds 60% alcoholic solution B is described 7 flavor medical materials and medicinal residues A gross weight 10 times, extract 2h, filter, with the extracting solution A ' after step (1) extraction volatile oil, merge, concentrating under reduced pressure, the medicinal liquid that under concentrated 25 ℃ of conditions, relative density is 1.10;
(3) get the medicinal liquid that under 25 ℃ of conditions of step (2) gained, relative density is 1.10, filter, DM130 type macroporous resin adsorption 6h by 1/3 times of weight, then use the water elution of 8 times of amounts of DM-130 type macroporous resin volume, use successively again the ethanol elution of the variable concentrations of 8 times of DM130 type macroporous resin volumes, eluting is respectively 10% ethanol by the volumetric concentration of ethanol, 30% ethanol, 50% ethanol, 70% ethanol, 95% ethanol elution, collect respectively eluent, merge standby, eluent concentrating under reduced pressure after merging is reclaimed to ethanol, collection is concentrated into the fluid extract of relative density 1.20-1.40 under 60 ℃ of conditions, dry, the different concentration ethanol extract D after purification by macroporous resin,
(4) get tophus, Concretio Silicea Bambusae, Stigma Croci, Mumiyah-asil, artificial Calculus Bovis, artificial Moschus by the crude drug composition and ratio; totally 6 flavor medical materials, be ground into the 1.4mm fine powder, adds the alcoholic solution B of volumetric concentration 90%; soak 12h; with alcoholic solution B percolation, extract, institute's consumption is 30 times of described 6 flavor medical material gross weights, collects the percolation medicinal liquid; temperature is lower than under 60 ℃ of conditions; concentrating under reduced pressure, drying, obtain extract E.
(5) the extract E that the purification by macroporous resin extract D that volatile oil clathrate compound above-mentioned steps (1) made, step (3) make, step (4) make mixes, and adds conventional adjuvant, according to common process, is prepared into pill.
Embodiment 5, a kind of preparation for the treatment of the medicament composition dropping pills of hepatopathy
(1) get Flos Caryophylli by the crude drug composition and ratio, add 6 times of weight of water, adopt steam distillation, extract volatile oil 4h, collect volatile oil, obtain volatile oil, medicinal liquid filters, and obtains extracting solution A ' and medicinal residues A;
The volatile oil that collection is obtained adds in the beta cyclodextrin saturated aqueous solution of percent weight in volume 4%, the envelope-bulk to weight ratio of volatile oil and beta cyclodextrin is 1ml: 4g, under stirring condition, keep temperature 50 C, stir 4h ,-4 ℃ of cold preservations are spent the night, sucking filtration, precipitation, 50 ℃ of vacuum dryings, obtain volatile oil clathrate compound;
(2) get tangut dragonhead, Flos Carthami, Herba meconopsis integrifoliae, Corydalis impatiens (Pall.) Fisch., Indian Herba Swertiae bimaculatae, Herpetospermum caudigerum Wall., Parmelia saxatilis Ach. totally 7 flavor medical materials by the crude drug composition and ratio, with the medicinal residues A after step (1) is extracted volatile oil, mix, the alcoholic solution B reflux, extract, 3 times that adds volumetric concentration 60%, the amount that at every turn adds 60% alcoholic solution B is described 7 flavor medical materials and medicinal residues A gross weight 10 times, extract 2h, filter, with the extracting solution A ' after step (1) extraction volatile oil, merge, concentrating under reduced pressure, the fluid extract that under concentrated 60 ℃ of conditions, relative density is 1.3;
(3) get the fluid extract that under 60 ℃ of conditions of step (2) gained, relative density is 1.3, drying, obtain ethanol extraction C;
(4) get tophus, Concretio Silicea Bambusae, Stigma Croci, Mumiyah-asil, artificial Calculus Bovis, artificial Moschus by the crude drug composition and ratio; totally 6 the flavor medical materials; the alcoholic solution B that adds volumetric concentration 80%, add the alcoholic solution B of volumetric concentration 80% to extract 2-3 time, temperature 60 C; the amount that at every turn adds alcoholic solution B is 10 times of described 6 flavor medical material gross weights; extract 3h, filter the medicinal liquid concentrating under reduced pressure; drying, obtain extract F.
(5) the extract F that the different ethanol extraction C that volatile oil clathrate compound above-mentioned steps (1) made, step (3) make, step (4) make mixes, and adds conventional adjuvant, according to common process, is prepared into drop pill.
Experimental example 1, take anti-HBV effect as target, the pharmacological action that utilizes Duck hepatitis B model to carry out the smooth pharmaceutical composition of liver is observed.
The animal model preparation: male 1 age in days sheldrake, body weight 40-50g, through lower limb shin arteries and veins injection duck DHBV-DNA strong positive serum, 0.2ml/ only, raises to 2 week age as duck hepatitis B experimental animal model.
Test method: 140 of congenital infection DHBV ducks are divided into 7 groups, 20 every group at random: positive controls, virus control group, the smooth compositions 1-5 of liver.The smooth pharmaceutical composition of the liver of administration group, dosage is 100mg/kg/d, virus control group starch solution, the smooth capsule of liver for positive controls, dosage is 100mg/kg/d; Gavaging every day 1 time, 10 days is a course for the treatment of.Respectively with medication before, medication 10d external jugular vein gets blood, separation of serum-20 ℃ preservation is to be checked.Get above-mentioned Sanguis Anas domestica please, every batch with the time point film, with P labelling DHBV-DNA probe, and asks dot blot hybridization as Sanguis Anas domestica, autoradiography diaphragm speckle is surveyed OD value (490nm) on microplate reader, calculating serum DHBV-DNA density.The results are shown in Table 1.
The inhibitory action of the smooth pharmaceutical composition of table 1 body liver to DHBV-DNA
(annotating: with comparison before the medication of this group, * P<0.01)
Result shows, during in body, anti-dhbv dna is tested, the smooth pharmaceutical composition 1-5 of liver all can significantly reduce DHBV infected duck serum DHBV-DNA level, and be better than the smooth capsule matched group of liver, the anti-hepatitis B effect of the smooth pharmaceutical composition of prompting liver is better than the smooth capsule preparations of former liver, and the smooth pharmaceutical composition 1 effect optimum of liver.
Experimental example 2, stability test
Take Flos Caryophylli volatile oil as index, investigate volatile oil beta cyclodextrin inclusion technique advantage.
Press the method for embodiment 1 and extract volatile oil, and enclose, prepare the smooth composition capsule of liver simultaneously; Preparation method by the smooth capsule of former liver prepares the smooth capsule of liver; Identical conditions transfers and sets to 0,1,2,3,6 month, detect volatile oil content, the results are shown in Table 2.
The investigation result of table 2 beta cyclodextrin enclose to volatile oil stability
Result shows, after Flos Caryophylli volatile oil use beta cyclodextrin enclose of the present invention, can improve the stability of volatile oil in preparation.
Experimental example 3, Dissolution Rate Testing
The dissolution of the active ingredient such as S-A Hydroxysafflor yellow A, crocin I and glycosides II, muscone, eugenol, the bitter glycosides of Indian Herba Swertiae bimaculatae of take is index, carries out the advantage of the smooth pharmaceutical composition of liver and investigates.The results are shown in Table 3.
The smooth pharmaceutical composition dissolution of table 3 liver result
Result shows, the dissolution of the active ingredient such as the smooth pharmaceutical composition 1-5 of liver S-A Hydroxysafflor yellow A, crocin I and glycosides II, muscone, eugenol, the bitter glycosides of Indian Herba Swertiae bimaculatae all is better than the smooth capsule matched group of liver.
Experimental example 4: craft screening test
The content of the bitter glycosides of total flavones and Indian Herba Swertiae bimaculatae of take is index, investigates the impact of different model resin on the smooth compositions effective ingredient of liver enriching and purifying.The results are shown in Table 4, table 5.
Table 4 different model Resin sieving selection result
Result shows, the HPD600 macroporous adsorbent resin is all the highest to total flavones and the bitter glycosides absorption of Indian Herba Swertiae bimaculatae, and dead adsorption losses minimum.
Table 5 macroporous resin enrichment purification effective ingredient result
| Technique | General flavone content (mg/g) | S-A Hydroxysafflor yellow A (mg/g) | The bitter glycosides (mg/g) of Indian Herba Swertiae bimaculatae |
| Before the HPD600 purification | 35.6 | 1.5 | 0.21 |
| After the HPD600 purification | 400.8 | 21.5 | 2.53 |
Result shows, after purification by macroporous resin, effective ingredient has obtained effective enrichment, improves effective ingredient concentration.
Claims (1)
1. a preparation method for the treatment of the Tibetan medicinal composition preparation of hepatopathy, the raw material medicines in portions by weight of described pharmaceutical composition consists of: 17.6 parts of tophuss, 17.6 parts of Concretio Silicea Bambusaes, 43.7 parts, Flos Carthami, 7 parts of Stigma Crocis, 52 parts of Herba meconopsis integrifoliae, 35 parts of tangut dragonheads, 35 parts of Corydalis impatiens (Pall.) Fisch.s, 38.2 parts of Mumiyah-asil, 17.6 parts of Flos Caryophyllis, 3.5 parts of artificial Calculus Boviss, 17.6 parts of Indian Herba Swertiae bimaculataes, 10.5 parts of Herpetospermum caudigerum Wall.s, 3.5 parts of Parmelia saxatilis Ach., 1.4 parts of artificial Moschuss; It is characterized in that, comprise the following steps:
(1) get Flos Caryophylli by the crude drug composition and ratio, add 6 times of weight of water, adopt steam distillation, extract volatile oil 4h, collect volatile oil, obtain volatile oil, medicinal liquid filters, and obtains extracting solution A ' and medicinal residues A;
The volatile oil that collection is obtained adds in the beta cyclodextrin saturated aqueous solution of percent weight in volume 4%, the envelope-bulk to weight ratio of volatile oil and beta cyclodextrin is 1ml:4g, under stirring condition, keep temperature 50 C, stir 4h ,-4 ℃ of cold preservations are spent the night, sucking filtration, precipitation, 5 ℃ of vacuum dryings, obtain volatile oil clathrate compound;
(2) get tangut dragonhead by the crude drug composition and ratio, Flos Carthami, Herba meconopsis integrifoliae, Corydalis impatiens (Pall.) Fisch., Indian Herba Swertiae bimaculatae, Herpetospermum caudigerum Wall., Parmelia saxatilis Ach. is totally 7 flavor medical materials, mix, be ground into 200 μ m fine powders, with the medicinal residues A after Flos Caryophylli is extracted volatile oil, mix, the alcoholic solution B that adds volumetric concentration 50%, soak 8h, with alcoholic solution B percolation, extract, institute's consumption is described 7 flavor medical materials and medicinal residues A gross weight 25 times, collect the percolation medicinal liquid, with the extracting solution A ' after Flos Caryophylli extraction volatile oil, merge, temperature is lower than under 60 ℃ of conditions, concentrating under reduced pressure, be concentrated into the medicinal liquid that under 25 ℃ of conditions, relative density is 1.10,
(3) get the medicinal liquid that under 25 ℃ of conditions of step (2) gained, relative density is 1.10, filter, HPD600 type macroporous resin adsorption 6h by 1/3 times of medicinal liquid weight, then use the water elution of 5 times of amounts of HPD600 type macroporous resin volume, use successively again the ethanol elution of the variable concentrations of 5 times of amounts of HPD600 type macroporous resin volume, eluting is respectively 10% ethanol by the volumetric concentration of ethanol, 30% ethanol, 50% ethanol, 70% ethanol, 95% ethanol elution, collect respectively eluent, merge, eluent concentrating under reduced pressure after merging is reclaimed to ethanol, collection is concentrated into the fluid extract of relative density 1.3 under 60 ℃ of conditions, dry, obtain purification by macroporous resin extract D,
(4) get tophus, Concretio Silicea Bambusae, Stigma Croci, Mumiyah-asil, artificial Calculus Bovis, artificial Moschus by the crude drug composition and ratio, totally 6 flavor medical materials, be ground into 50 μ m fine powders, adds the alcoholic solution B of volumetric concentration 80%, soak 12h, with alcoholic solution B percolation, extract, institute's consumption is 30 times of described 6 flavor medical material gross weights, collects the percolation medicinal liquid, temperature is lower than under 60 ℃ of conditions, concentrating under reduced pressure, drying, obtain extract E;
(5) the extract E that the purification by macroporous resin extract D that volatile oil clathrate compound above-mentioned steps (1) made, step (3) make, step (4) make mixes, and adds conventional adjuvant, according to common process, is prepared into capsule.
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