CN102688277A - Pharmaceutical composition and preparation for eliminating dampness and dredging obstruction as well as preparation and application for same - Google Patents
Pharmaceutical composition and preparation for eliminating dampness and dredging obstruction as well as preparation and application for same Download PDFInfo
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Abstract
The invention discloses a pharmaceutical composition and a preparation for eliminating dampness and dredging obstruction as well as a preparation and an application for the same. The pharmaceutical composition is prepared from raw materials in parts by weight: 10-20 parts by weight of volatile oil inclusion compound, and 85-95 parts by weight of ethanol extract. According to the invention, preparation process is optimized, volatile oil has small possibility of volatilizing after being included by beta-cyclodextrin, thus enhancing medicine stability, and enabling the administration quantity of the prescription to be more accurate; and by using the optimized extraction process, the volatile oil is furthest extracted, and medicinal material resource and social cost are furthest saved.
Description
Technical field
The present invention relates to a kind of pharmaceutical composition, preparation and preparation thereof and application, particularly a kind of pharmaceutical composition, preparation and preparation thereof and application of the blood stasis dispelling that is used to dehumidify.
Background technology
Rheumatic arthritis, rheumatoid arthritis, osteoarthritis are commonly encountered diseases, frequently-occurring diseases clinically, and Therapeutic Method is a lot of, but effect differs.
Five tastes manna dipping lotion is recorded in Chinese patent medicine provincial standard rising national drug standards part, standard numbering: WS-11383 (ZD-1383)-2002.Consist of: Cacumen et folium sabinae przewalskii 200g, Cacumen Myricariae Germanicae 200g, Herba Ephedrae 200g, Rhododendron 200g, Artemisia sieversiana Willd. 200g.Function cures mainly and is clearing away heat and expelling wind, the effect of dehumidifying blood stasis dispelling.Be used for the redness and swelling of joints burning pain due to the rheumatism pathogenic heat numbness resistance meridians, joint stuffiness; Rheumatic arthritis, rheumatoid arthritis, osteoarthritis are seen above-mentioned patient.Five tastes manna dipping lotion is owing to respond well, and is evident in efficacy through clinical verification, has no side effect, and enjoys the patient to favor clinically.Former technology is: with Cacumen et folium sabinae przewalskii 200g, Cacumen Myricariae Germanicae 200g, Herba Ephedrae 200g, Rhododendron 200g, Artemisia sieversiana Willd. 200g, extract volatile oil with vapor distillation, and subsequent use; Medicinal residues mix with Herba Ephedrae, add distillers yeast, barley wine is an amount of, and reuse 50% alcohol reflux is 3 times after the fermentation process, 4 hours for the first time; Second and third time each 2 hours, merge extractive liquid, filters, and filtrate recycling ethanol also is concentrated into an amount of; Add above-mentioned volatile oil and sodium benzoate, add water to 1000ml, left standstill below 4 ℃ 48 hours, filter; Fill, sterilization promptly gets.
Five tastes manna medicinal-bathing particle is recorded in Chinese patent medicine provincial standard rising national drug standards part, standard numbering: WS-11385 (ZD-1385)-2002.Consist of: Juniperus oxycedrus 1000g, Rhododendron 1000g, Artemisia sieversiana Willd. 1000g, Herba Ephedrae 1000g, Cacumen Myricariae Germanicae 1000g.Function cures mainly and is: relieving the exterior syndrome by diaphoresis, anti-inflammatory analgetic, flat yellow fluid, promoting blood circulation to remove obstruction in the collateral.Be used for various dermatosiss and rheumatism, rheumatoid arthritis, gout, hemiplegia, women's puerperal disease.Disease such as sprain for soft group.Former technology is: the above five tastes, and get Herba Ephedrae 500g and be ground into fine powder, subsequent use; Four flavors such as residue Herba Ephedrae and all the other Artemisia sieversiana Willd. are ground into coarse powder, extract volatile oil with steam distillation, and volatile oil is subsequent use, and medicinal liquid filters; Filtrate for later use, medicinal residues decocte with water 1 hour filters, and filtrating merges with above-mentioned filtrating; Being evaporated to relative density is the clear paste of 1.28～1.30 (50 ℃), with above-mentioned fine powder mixing, processes granule, drying; Add above-mentioned volatile oil, mixing, treat that volatile oil is blotted by granule after, promptly get.
Five tastes manna dipping lotion in the market and granule all are that volatile oil is added in the middle of the last preparation; But volatile oil can not be directly water-soluble; When having a bath, can only swim in the surface of water; Can be because the temperature of the water when having a bath to be higher, most of volatile oil has vapored away this moment, can have influence on the curative effect of medicine like this; Bottled lotion is generally heavier, and the patient carries very inconvenient, and granule is not because volatile oil has enclose, and volatile oil just than being easier to volatilization, so also can influence the curative effect of medicine when granule is placed.
Summary of the invention
To the deficiency of prior art, the present invention provides a kind of pharmaceutical composition of blood stasis dispelling and preparation method thereof that dehumidifies that is used to; The present invention also provides the pharmaceutical preparation and the method for preparing of said composition.Further the present invention also provides the application of said composition and preparation.
Technical scheme of the present invention is following:
A kind of pharmaceutical composition of the blood stasis dispelling that is used to dehumidify, process by the raw material of following weight portion:
Volatile oil clathrate compound 10-20 weight portion, ethanol extraction 85-95 weight portion;
Described volatile oil clathrate compound makes according to following method: with Cacumen et folium sabinae przewalskii 150-250 weight portion, Cacumen Myricariae Germanicae 150-250 weight portion, Rhododendron 150-250 weight portion, Artemisia sieversiana Willd. 150-250 weight portion; Be cut into pieces, add medical material gross weight 4-9 water doubly, extract volatile oil with vapor distillation; Extraction time 3-5 hour; Get volatile oil and medicinal residues, collect volatile oil, subsequent use; Precision takes by weighing beta-schardinger dextrin-, adds distilled water and is made into the solution that contains beta-schardinger dextrin-mass percent 5%-7%, stirs, and 60 ℃ of-70 ℃ of heating in water bath make dissolving; Be cooled to 50 ℃-55 ℃, under the stirring condition, add the equal-volume mixture of volatile oil and dehydrated alcohol, make volatile oil: beta-schardinger dextrin-=1ml:4g; Sealing is stirred 3-5h ,-4 ℃ of-4 ℃ of cold preservation 12-24h, sucking filtration under 50 ℃ of-55 ℃ of conditions; Deposition, 50 ℃ of-55 ℃ of vacuum dryings are pulverized, and get volatile oil clathrate compound;
Described ethanol extraction makes according to following method: the medicinal residues after volatile oil extracts mix with 150-250 weight portion Herba Ephedrae, add medicinal residues and the total medical material amount of Herba Ephedrae the 0.25-0.3wt% distillers yeast, spray into the barley wine that 35～56 of 2-3wt% spends and ferment, after the fermentation process; The 6-10 of the total medical material amount of reuse medicinal residues and Herba Ephedrae volumetric concentration 40-60% ethanol doubly, 80 ℃ are extracted 2-4 time, 3-5 hour for the first time; Each 1-3 of second and third time hour; It is 1.33 thick paste that merge extractive liquid,, filtrate decompression are concentrated into 50 ℃ of relative densities, 70-90 ℃ vacuum drying 3-5 hour; Pulverize, get ethanol extraction.
Preferred according to the present invention, a kind of pharmaceutical composition of the blood stasis dispelling that is used to dehumidify, process by the raw material of following weight portion:
Volatile oil clathrate compound 15 weight portions, ethanol extraction 91 weight portions;
Described volatile oil clathrate compound makes according to following method: with Cacumen et folium sabinae przewalskii 200 weight portions, Cacumen Myricariae Germanicae 200 weight portions, Rhododendron 200 weight portions, Artemisia sieversiana Willd. 200 weight portions; Be cut into pieces, add the water of 6 times of medical material gross weights, extract volatile oil with vapor distillation; 4 hours extraction times; Get volatile oil and medicinal residues, collect volatile oil, subsequent use; Precision takes by weighing beta-schardinger dextrin-, adds distilled water and is made into the solution that contains beta-schardinger dextrin-mass percent 5%, stirs, and 60 ℃ of-70 ℃ of heating in water bath make dissolving; Be cooled to 50 ℃-55 ℃, under the stirring condition, add the equal-volume mixture of volatile oil and dehydrated alcohol, make volatile oil: beta-schardinger dextrin-=1ml:4g; Sealing is stirred 4h ,-4 ℃ of cold preservation 12h, sucking filtration under 50 ℃ of conditions; Deposition, 50 ℃ of vacuum dryings are pulverized, and get volatile oil clathrate compound;
Described ethanol extraction makes according to following method: the medicinal residues after volatile oil extracts mix with 200 weight portion Herba Ephedraes, add medicinal residues and the total medical material amount of Herba Ephedrae the 0.25wt% distillers yeast, spray into 38～40 of 2wt% and spend barley wines and ferment, after the fermentation process; 8 times volumetric concentration 50% ethanol of the total medical material amount of reuse medicinal residues and Herba Ephedrae, 80 ℃ are extracted 3 times, 4 hours for the first time; Second and third time each 2 hours; It is 1.33 thick paste that merge extractive liquid,, filtrate decompression are concentrated into 50 ℃ of relative densities, 80 ℃ of vacuum dryings 4 hours; Pulverize, get ethanol extraction.
The unit of above weight portion and parts by volume is a grams per milliliter.
Supplementary material of the present invention is commercial product.
A kind of drug combination preparation of the blood stasis dispelling that is used to dehumidify is that the pharmaceutical composition by above-mentioned a kind of blood stasis dispelling that is used to dehumidify adds conventional adjuvant, processes effervescent granule according to common process; Said adjuvant comprises one or more of solvent, disintegrating agent, antiseptic, binding agent, lubricant.
Preferred according to the present invention, a kind of pharmaceutical composition effervescent granule of the blood stasis dispelling that is used to dehumidify is processed by the raw material of following weight portion: volatile oil clathrate compound 15g, ethanol extraction 91g, sodium bicarbonate 55g, citric acid 45g, microcrystalline Cellulose 94g;
Described volatile oil clathrate compound makes according to following method: with Cacumen et folium sabinae przewalskii 200g, Cacumen Myricariae Germanicae 200g, Rhododendron 200g, Artemisia sieversiana Willd. 200g; Be cut into pieces, add the water of 6 times of medical material gross weights, extract volatile oil with vapor distillation; 4 hours extraction times; Get volatile oil and medicinal residues, collect volatile oil, subsequent use; Precision takes by weighing beta-schardinger dextrin-, adds distilled water and is made into the solution that contains beta-schardinger dextrin-mass percent 5%, stirs, and 60 ℃ of-70 ℃ of heating in water bath make dissolving; Be cooled to 50 ℃-55 ℃, under the stirring condition, add the equal-volume mixture of volatile oil and dehydrated alcohol, make volatile oil: beta-schardinger dextrin-=1ml:4g; Sealing is stirred 4h ,-4 ℃ of cold preservation 12h, sucking filtration under 50 ℃ of conditions; Deposition, 50 ℃ of vacuum dryings are pulverized, and get volatile oil clathrate compound;
Described ethanol extraction makes according to following method: the medicinal residues after volatile oil extracts mix with the 200g Herba Ephedrae, add medicinal residues and the total medical material amount of Herba Ephedrae the 0.25wt% distillers yeast, spray into 38～40 of 2wt% and spend barley wines and ferment, after the fermentation process; 8 times volumetric concentration 50% ethanol of the total medical material amount of reuse medicinal residues and Herba Ephedrae, 80 ℃ are extracted 3 times, 4 hours for the first time; Second and third time each 2 hours; It is 1.33 thick paste that merge extractive liquid,, filtrate decompression are concentrated into 50 ℃ of relative densities, 80 ℃ of vacuum dryings 4 hours; Pulverize, get ethanol extraction.
A kind of preparation of drug combination method of the blood stasis dispelling that is used to dehumidify, step is following:
(1) with Cacumen et folium sabinae przewalskii 150-250 weight portion, Cacumen Myricariae Germanicae 150-250 weight portion, Rhododendron 150-250 weight portion, Artemisia sieversiana Willd. 150-250 weight portion; Be cut into pieces, add medical material gross weight 4-9 water doubly, extract volatile oil with vapor distillation; Extraction time 3-5 hour; Get volatile oil and medicinal residues, collect volatile oil, subsequent use; Precision takes by weighing beta-schardinger dextrin-, adds distilled water and is made into the solution that contains beta-schardinger dextrin-mass percent 5%-7%, stirs, and 60 ℃ of-70 ℃ of heating in water bath make dissolving; Be cooled to 50 ℃-55 ℃, under the stirring condition, add the equal-volume mixture of volatile oil and dehydrated alcohol, make volatile oil: beta cyclodextrin=1ml:4g; Sealing is stirred 3-5h ,-4 ℃ of-4 ℃ of cold preservation 12-24h, sucking filtration under 50 ℃ of-55 ℃ of conditions; Deposition, 50 ℃ of-55 ℃ of vacuum dryings are pulverized, and get volatile oil clathrate compound;
(2) medicinal residues after volatile oil extracts mix with 150-250 weight portion Herba Ephedrae, add medicinal residues and the total medical material amount of Herba Ephedrae the 0.25-0.3wt% distillers yeast, spray into 35～56 of 2-3wt% and spend barley wines and ferment, after the fermentation process; The 6-10 of the total medical material amount of reuse medicinal residues and Herba Ephedrae volumetric concentration 40-60% ethanol doubly, 80 ℃ are extracted 2-4 time, 3-5 hour for the first time; Each 1-3 of second and third time hour; It is 1.33 thick paste that merge extractive liquid,, filtrate decompression are concentrated into 50 ℃ of relative densities, 70-90 ℃ vacuum drying 3-5 hour; Pulverize, get ethanol extraction;
(3) ethanol extraction that volatile oil clathrate compound that step (1) is made and step (2) make mixes, and promptly gets.
Preferred according to the present invention, a kind of preparation of drug combination method of the blood stasis dispelling that is used to dehumidify, step is following:
(1) with Cacumen et folium sabinae przewalskii 200 weight portions, Cacumen Myricariae Germanicae 200 weight portions, Rhododendron 200 weight portions, Artemisia sieversiana Willd. 200 weight portions, is cut into pieces, adds the water of 6 times of medical material gross weights; Extract volatile oil with vapor distillation, 4 hours extraction times, get volatile oil and medicinal residues; Collect volatile oil, subsequent use; Precision takes by weighing beta-schardinger dextrin-, adds distilled water and is made into the solution that contains beta-schardinger dextrin-mass percent 5%, stirs, and 60 ℃ of-70 ℃ of heating in water bath make dissolving; Be cooled to 50 ℃-55 ℃, under the stirring condition, add the equal-volume mixture of volatile oil and dehydrated alcohol, make volatile oil: beta cyclodextrin=1ml:4g; Sealing is stirred 4h ,-4 ℃ of cold preservation 12h, sucking filtration under 50 ℃ of conditions; Deposition, 50 ℃ of vacuum dryings are pulverized, and get volatile oil clathrate compound;
(2) medicinal residues after volatile oil extracts mix with 200 weight portion Herba Ephedraes, add medicinal residues and the total medical material amount of Herba Ephedrae the 0.25wt% distillers yeast, spray into 38～40 of 2wt% and spend barley wines and ferment, after the fermentation process; 8 times volumetric concentration 50% ethanol of the total medical material amount of reuse medicinal residues and Herba Ephedrae, 80 ℃ are extracted 3 times, 4 hours for the first time; Second and third time each 2 hours, merge extractive liquid,, it is 1.33 thick paste that filtrate decompression is concentrated into 50 ℃ of relative densities; 80 ℃ of vacuum dryings 4 hours are pulverized, ethanol extraction;
(3) ethanol extraction that volatile oil clathrate compound that step (1) is made and step (2) make mixes, and promptly gets.
Preferred according to the present invention, a kind of method for preparing of pharmaceutical composition effervescent granule of the blood stasis dispelling that is used to dehumidify, step is following:
(1) with Cacumen et folium sabinae przewalskii 200g, Cacumen Myricariae Germanicae 200g, Rhododendron 200g, Artemisia sieversiana Willd. 200g, be cut into pieces, add the water of 6 times of medical material gross weights, extract volatile oil with vapor distillation, 4 hours extraction times, get volatile oil and medicinal residues, collect volatile oil, subsequent use; Precision takes by weighing beta-schardinger dextrin-, adds distilled water and is made into the solution that contains beta-schardinger dextrin-mass percent 5%, stirs, and 60 ℃ of-70 ℃ of heating in water bath make dissolving; Be cooled to 50 ℃-55 ℃, under the stirring condition, add the equal-volume mixture of volatile oil and dehydrated alcohol, make volatile oil: beta-schardinger dextrin-=1ml:4g; Sealing is stirred 4h ,-4 ℃ of cold preservation 12h, sucking filtration under 50 ℃ of conditions; Deposition, 50 ℃ of vacuum dryings are pulverized, and get volatile oil clathrate compound;
(2) medicinal residues after volatile oil extracts mix with the 200g Herba Ephedrae, add medicinal residues and the total medical material amount of Herba Ephedrae the 0.25wt% distillers yeast, spray into 38～40 of 2wt% and spend barley wines and ferment, after the fermentation process; 8 times volumetric concentration 50% ethanol of the total medical material amount of reuse medicinal residues and Herba Ephedrae, 80 ℃ are extracted 3 times, 4 hours for the first time; Second and third time each 2 hours, merge extractive liquid,, it is 1.33 thick paste that filtrate decompression is concentrated into 50 ℃ of relative densities; 80 ℃ of vacuum dryings 4 hours are pulverized, ethanol extraction;
(3) ethanol extraction that volatile oil clathrate compound that step (1) is made and step (2) make mixes, and adds sodium bicarbonate, citric acid, and dehydrated alcohol is done wetting agent, mixing, and 16 orders are granulated, 50 ℃ of dryings 2 hours, 18 order granulate, pack promptly gets.
A kind of pharmaceutical composition of the blood stasis dispelling that is used for dehumidifying is in the application of preparation treatment rheumatism, rheumatoid arthritis, gout.
Technical characterstic of the present invention:
1, the clathrate process that does not have volatile oil in the former technology of five tastes manna dipping lotion, and former extraction process only embodies vapor distillation extraction volatile oil; The extracted amount of concrete amount of water, extraction time and volatile oil is not all write exactly; Adopt beta-cyclodextrin inclusion compound among the present invention; Optimize three critical technical parameters of volatile oil and beta-schardinger dextrin-usage ratio, mixing time, whipping temp, also optimized simultaneously amount of water in the volatile oil extraction process, extraction time critical technical parameter.
2, in the former extraction process of five tastes manna dipping lotion, concentration of alcohol, alcohol adding amount, extraction time, extraction time are not all carried out process optimization test, the invention reside in the extraction process, above-mentioned factor is optimized, and optimizes optimum extraction process.
3, feed intake with volatile oil clathrate compound and ethanol extraction mixing, add conventional adjuvant, process that clinical use is convenient, onset effervescent granule faster.
The present invention compared with prior art, beneficial effect is following:
1, volatile oil of the present invention should not volatilize volatile oil through behind the beta-cyclodextrin inclusion compound, has increased stability of drug, also makes the prescription inventory more accurate simultaneously; Extraction process with after optimizing not only extracts volatile oil to greatest extent, and has practiced thrift herb resource and social cost to greatest extent.
2, compare with conventional formulation, the pharmaceutical preparation of the method preparation of invention is under the prerequisite that keeps former preparation drug effect, and effervescent granule uses convenient and onset is faster, also can use this compositions to process different preparations according to clinical needs simultaneously.
The specific embodiment
Following embodiment and experimental example are used to further specify but are not limited to the present invention.
The pharmaceutical composition of embodiment 1, a kind of blood stasis dispelling that is used to dehumidify, process by the raw material of following weight portion:
Volatile oil clathrate compound 15g, ethanol extraction 91g;
Be prepared from according to following method:
(1) with Cacumen et folium sabinae przewalskii 200g, Cacumen Myricariae Germanicae 200g, Rhododendron 200g, Artemisia sieversiana Willd. 200g, be cut into pieces, add the water of 6 times of medical material gross weights, extract volatile oil with vapor distillation, 4 hours extraction times, get volatile oil and medicinal residues, collect volatile oil, subsequent use; Precision takes by weighing beta-schardinger dextrin-, adds distilled water and is made into the solution that contains beta-schardinger dextrin-mass percent 5%, stirs, and 60 ℃ of-70 ℃ of heating in water bath make dissolving; Be cooled to 50 ℃-55 ℃, under the stirring condition, add the equal-volume mixture of volatile oil and dehydrated alcohol, make volatile oil: beta-schardinger dextrin-=1ml:4g; Sealing is stirred 4h ,-4 ℃ of cold preservation 12h, sucking filtration under 50 ℃ of conditions; Deposition, 50 ℃ of vacuum dryings are pulverized, and get volatile oil clathrate compound;
(2) medicinal residues after volatile oil extracts mix with the 200g Herba Ephedrae, add medicinal residues and the total medical material amount of Herba Ephedrae the 0.25wt% distillers yeast, spray into 38～40 of 2wt% and spend barley wines and ferment, after the fermentation process; 8 times volumetric concentration 50% ethanol of the total medical material amount of reuse medicinal residues and Herba Ephedrae, 80 ℃ are extracted 3 times, 4 hours for the first time; Second and third time each 2 hours, merge extractive liquid,, it is 1.33 thick paste that filtrate decompression is concentrated into 50 ℃ of relative densities; 80 ℃ of vacuum dryings 4 hours are pulverized, ethanol extraction;
(3) ethanol extraction that volatile oil clathrate compound that step (1) is made and step (2) make mixes, and promptly gets.
The pharmaceutical composition effervescent granule of embodiment 2, a kind of blood stasis dispelling that is used to dehumidify, process by the raw material of following weight portion:
Volatile oil clathrate compound 15g, ethanol extraction 91g, sodium bicarbonate 55g, citric acid 45g, microcrystalline Cellulose 94g.
Be prepared from according to following method:
(1) with Cacumen et folium sabinae przewalskii 200g, Cacumen Myricariae Germanicae 200g, Rhododendron 200g, Artemisia sieversiana Willd. 200g, be cut into pieces, add the water of 6 times of medical material gross weights, extract volatile oil with vapor distillation, 4 hours extraction times, get volatile oil and medicinal residues, collect volatile oil, subsequent use; Precision takes by weighing beta-schardinger dextrin-, adds distilled water and is made into the solution that contains beta-schardinger dextrin-mass percent 5%, stirs, and 60 ℃ of-70 ℃ of heating in water bath make dissolving; Be cooled to 50 ℃-55 ℃, under the stirring condition, add the equal-volume mixture of volatile oil and dehydrated alcohol, make volatile oil: beta-schardinger dextrin-=1ml:4g; Sealing is stirred 4h, 4 ℃ of cold preservation 12h, sucking filtration under 50 ℃ of conditions; Deposition, 50 ℃ of vacuum dryings are pulverized, and get volatile oil clathrate compound;
(2) medicinal residues after volatile oil extracts mix with the 200g Herba Ephedrae, add medicinal residues and the total medical material amount of Herba Ephedrae the 0.25wt% distillers yeast, spray into 38～40 of 2wt% and spend barley wines and ferment, after the fermentation process; 8 times volumetric concentration 50% ethanol of the total medical material amount of reuse medicinal residues and Herba Ephedrae, 80 ℃ are extracted 3 times, 4 hours for the first time; Second and third time each 2 hours, merge extractive liquid,, it is 1.33 thick paste that filtrate decompression is concentrated into 50 ℃ of relative densities; 80 ℃ of vacuum dryings 4 hours are pulverized, ethanol extraction;
(3) ethanol extraction that volatile oil clathrate compound that step (1) is made and step (2) make mixes, and adds sodium bicarbonate, citric acid, microcrystalline Cellulose, and dehydrated alcohol is done wetting agent, mixing, and 16 orders are granulated, 50 ℃ of dryings 2 hours, pack promptly gets.
Experimental example 1, the experiment of volatile oil extraction process
The former technology of five tastes manna dipping lotion only embodies vapor distillation and extracts volatile oil, and the extracted amount of concrete amount of water, extraction time and volatile oil is not all write exactly,, in process optimization process of the present invention, above-mentioned factor is investigated for this reason.
1, vapor distillation extracts the investigation of amount of water in the volatile oil:
Investigation method:, make an experiment to 4 times of amount of water, 6 times, 8 times three gradients; Take by weighing medical material according to prescription, the water that adds 4 times, 6 times, 8 times amounts respectively extracts, 4 hours extraction times, extract 80 ℃ of temperature, and observe and receive oil mass: the result sees table 1.
The investigation of table 1 amount of water
| Medical material amount (g) | Amount of water (ml) | Receive oil mass (ml) |
| 200 | 800 | 0.5 |
| 200 | 1200 | 0.85 |
| 200 | 1600 | 0.86 |
The result shows: add the water of 4 times of weight, the volatile oil extracted amount is lower, add 6 times of weight water extraction volatile oil amount with add 8 times of weight the few of difference of water, from energy savings with practice thrift cost consideration, preferably add the water of 6 times of weight.
2, vapor distillation extracts the investigation of extraction time in the volatile oil:
Investigation method:,, make an experiment to 2 hours extraction times, 4 hours, 6 hours three gradients according to document and knowhow; Take by weighing medical material according to prescription, the water that adds 8 times of amounts extracts, and extracts respectively 2 hours, 4 hours, 6 hours, extracts 80 ℃ of temperature, and observe and receive oil mass: the result sees table 2.
The investigation of table 2 extraction time
| Medical material amount (g) | Extraction time (min) | Receive oil mass (ml) |
| 200 | 120 | 0.5 |
| 200 | 240 | 0.85 |
| 200 | 360 | 0.86 |
The result shows: extracted 2 hours, the volatile oil extracted amount is lower, extracts the amount and the few of difference of amount of extracting 6 hours volatile oil of 4 hours volatile oil, from saving time and practicing thrift cost consideration, preferably extracts 4 hours.
To sum up experimental result shows, adds the water of 4 times of weight, and the volatile oil extracted amount is lower, add 6 times of weight water extraction volatile oil amount with add 8 times of weight the few of difference of water; The amount of volatile oil is along with the increase of time, and the volatilization oil mass increases gradually, but when extraction time reaches 4 hours; The volatilization oil mass is extracted basically and is finished, and from energy savings and saving cost consideration, preferably adds the water of 6 times of weight; Extracted 4 hours continuously, add the water distillation and collect volatile oil, the volatile oil yield is: 0.46%.
Experimental example 2, inclusion essential oil technological experiment
Do not have inclusion essential oil technology in the former technology of five tastes manna dipping lotion; The invention has the advantages that and adopt the beta cyclodextrin enclose; The accuracy and the stability of volatile oil consumption have been improved; Major influence factors is volatile oil and beta-schardinger dextrin-usage ratio, mixing time, whipping temp in volatile oil beta-cyclodextrin inclusion compound,, in process optimization process of the present invention, above-mentioned factor is investigated for this reason.
1, the investigation of volatile oil and beta-cyclodextrin inclusion compound ratio
The investigation method: to volatile oil and beta-cyclodextrin inclusion compound ratio be set at 1ml:2g, 1ml:4g, three gradients of 1ml:6g are investigated, and are that index is investigated with the inclusion rate, the result sees table 3.
The investigation of table 3 volatile oil and beta-cyclodextrin inclusion compound ratio
| Volatilization oil mass (ml) | Enclose ratio (ml:g) | Inclusion rate (%) |
| 1 | 1：2 | 72 |
| 1 | 1：4 | 85 |
| 1 | 1：6 | 86 |
The result shows: the ratio enclose of 1:2, and inclusion rate is lower; 1:4 and 1:8 enclose see there is not notable difference from inclusion rate, with reference to the few more good more principle of supplementary product consumption, so select for use 1:4 to carry out enclose.
2, the investigation of mixing time in the clathrate process
The investigation method: the mixing time to volatile oil and beta-cyclodextrin inclusion compound is investigated, and is set at 2 hours, 4 hours, 6 hours three gradients are investigated, and are that index is investigated with the inclusion rate, and the result sees table 4.
The investigation of table 4 volatile oil and beta-cyclodextrin inclusion compound mixing time
| Volatilization oil mass (ml) | Mixing time (h) | Inclusion rate (%) |
| 1 | 2 | 75 |
| 1 | 4 | 86 |
| 1 | 6 | 86 |
The result shows: mixing time is in the time of 2 hours, and inclusion rate is lower, stirs 4 hours and 6 hours, sees there is not notable difference from inclusion rate, with reference to saving time the principle of cost, carries out enclose in 4 hours so select for use.
3, the investigation of whipping temp in the clathrate process
The investigation method: because volatile oil can at high temperature lose, so the temperature of volatile oil and beta-cyclodextrin inclusion compound is investigated, being set at 30 ℃, 50 ℃, 70 ℃ three gradients and investigating, is that index is investigated with the inclusion rate, and the result sees table 5.
The investigation of table 5 volatile oil and beta-cyclodextrin inclusion compound whipping temp
| Volatilization oil mass (ml) | Whipping temp (℃) | Inclusion rate (%) |
| 1 | 30 | 60 |
| 1 | 50 | 86 |
| 1 | 70 | 70 |
The result shows: when the enclose whipping temp was 30 ℃, because temperature is lower, inclusion rate was also very low; Enclose fully is during 70 ℃ of enclose of temperature, because temperature is too high; Caused the volatilization loss of volatile oil, inclusion rate is also very low, so select 50 ℃ for use as the enclose temperature.
To sum up the result shows: in five tastes manna dipping lotion dipping lotion new technology, the optimum of optimization is: volatile oil and beta-cyclodextrin inclusion compound ratio are 1ml:4g, and under 50 ℃, stir 4 hours.
The investigation of experimental example 3, volatile oil process beta-cyclodextrin inclusion compound rear stability
The investigation method: according to the clathrate process of optimizing with inclusion essential oil after, carry out the extraction of volatile oil according to the method for distilling of volatile oil, be index with the oil-collecting ratio, investigate the stability of volatile oil: the result sees table 6.
The investigation of table 6 enclose rear stability
| Clathrate (g) | Oil-collecting ratio (%) |
| 50 | 92 |
| 50 | 93 |
| 50 | 94 |
The result shows: three results' oil-collecting ratio, more stable, almost free of losses (＜10%) has good stability.
Experimental example 4, ethanol extraction technological experiment
The former technology of five tastes manna dipping lotion is write medical material exactly and is added 50% alcohol reflux 3 times; Decocted 4 hours for the first time, second and third time each 2 hours is extracted out for what guarantee that effective ingredient tries one's best; Take into account production cost simultaneously, the present invention further optimizes original working condition.
Adopt single factor to investigate method, respectively concentration of alcohol, alcohol adding amount, extraction time, extraction time are investigated, optimize optimum extraction process; According to the result that each factor is investigated respectively, draw optimised process and be: add 50% ethanol of 8 times of amounts, 80 ℃ of refluxed are extracted 3 times, decoct 4 hours second and third time each 2 hours for the first time.
1, the investigation of concentration of alcohol in the extraction process:
Investigation method: the character of considering each medical material chemical analysis in the prescription; Decision adopts ethanol to extract; And concentration of alcohol investigated; Adopt 30% ethanol, 50% ethanol, three gradients of 80% ethanol to make an experiment, serve as to investigate index with dried cream yield and Determination of Ephedrine Hydrochloride: the result sees table 7.
The investigation of table 7 concentration of alcohol
| Medical material amount (g) | Concentration of alcohol | Dried cream yield | Content (mg/ml) |
| 200 | 30% | 12% | 0.08 |
| 200 | 50% | 9.2% | 0.12 |
| 200 | 80% | 9.1% | 0.13 |
The result shows: adopt 30% ethanol extraction, impurity is more, and content is undesirable; Adopt 50% ethanol to extract dried cream yield and Determination of Ephedrine Hydrochloride all meets the requirements, 80% ethanol extraction and 50% ethanol extraction difference are little, consider production safety and production cost, so preferred 50% ethanol extracts.
2, the investigation of alcohol adding amount in the extraction process:
The investigation method: 50% alcoholic acid alcohol adding amount is investigated, adopted three gradients of 6 times, 8 times, 10 times amounts to make an experiment, serve as to investigate index with dried cream yield and Determination of Ephedrine Hydrochloride: the result sees table 8.
The investigation of table 8 alcohol adding amount
| Medical material amount (g) | Alcohol adding amount (ml) | Dried cream yield | Content (mg/ml) |
| 200 | 1200 | 8% | 0.1 |
| 200 | 1600 | 9.2% | 0.13 |
| 200 | 2000 | 9.4% | 0.14 |
The result shows: 50% ethanol that adds 6 times of weight; The dried cream yield and the Determination of Ephedrine Hydrochloride of extract are all lower; 50% ethanol that adds 8 times of weight; The few of difference of 50% ethanol of dried cream yield and Determination of Ephedrine Hydrochloride and adding 10 times of weight from energy savings and saving cost consideration, preferably adds 50% ethanol of 8 times of weight.
3, the investigation of extraction time in the extraction process:
The investigation method: adopt 3 times, 5 times, 8 times three gradients to make an experiment to extraction time, with 8 times of amount 50% ethanol, extracted 3 hours, serve as to investigate index with dried cream yield and Determination of Ephedrine Hydrochloride: the result sees table 9.
The investigation of table 9 extraction time
| Medical material amount (g) | Extraction time | Dried cream yield | Content (mg/ml) |
| 200 | 3 | 9.1% | 0.12 |
| 200 | 5 | 9.2% | 0.13 |
| 200 | 8 | 9.4% | 0.14 |
The result shows: extract 3 times, 5 times, 8 times, the dried cream yield of extract and all few of difference of Determination of Ephedrine Hydrochloride from energy savings and saving cost consideration, are preferably extracted 3 times.
4, the investigation of extraction time in the extraction process:
Investigation method: investigate 2 hours for the first time respectively, second and third time each 1 hour; 4 hours for the first time, second and third time each 2 hours; 6 hours for the first time, second and third time 3 hours; This three extraction time gradient make an experiment, with 8 times the amount 50% ethanol, extracts 3 times, with dried cream yield and Determination of Ephedrine Hydrochloride serve as the investigation index: the result sees table 10.
The investigation of table 10 extraction time
| Medical material amount (g) | Extraction time (h) | Dried cream yield | Content (mg/ml) |
| 200 | 2，1，1 | 8.6% | 0.07 |
| 200 | 4，2，2 | 9.2% | 0.12 |
| 200 | 6，3，3 | 9.4% | 0.13 |
The result shows: extracted 2 hours for the first time, and two, three extractions 1 hour, dried cream rate and Determination of Ephedrine Hydrochloride are all lower, and other 2 condition difference are little, from energy savings and saving cost consideration, are preferably 4 hours for the first time, second and third time 2 hours.
Experimental example 5, the experiment of effervescence granular preparation prescription screening
The principal element that influences effervescent formulation has the selection of the proportioning of soda acid amount, wetting agent, the consumption of lubricant, investigates in the face of these influence factors down.
The investigation method of soda acid amount proportioning: take by weighing raw material according to the prescription ratio, the soda acid ratio is carried out according to 55:45,50:50, three ratios of 45:55, and serve as to investigate index with the effervescent time: the result sees table 11.
The investigation of table 11 soda acid amount proportioning
| The soda acid proportioning | The effervescent time (min) |
| 55：45 | 5 |
| 50：50 | 3 |
| 45：55 | 1 |
The result shows: during soda acid ratio 45:55, the effervescent time is the shortest, dissolve the rapidest, so preferred citric acid 45g, the sodium bicarbonate 55g of using.
The screening of different filleies and consumption thereof
This extract is handled through the ethanol precipitate with ethanol, and viscosity ratio is bigger, for this reason, has investigated the influence of different filleies to material viscosity.According to prescription proportioning weighing material in the table 12, mix homogeneously is granulated with an amount of dehydrated alcohol, drying, and granulate is investigated the granule character.
The investigation of different filleies of table 12 and consumption thereof
| Prescription | Extract (g) | Volatile oil clathrate compound (g) | Dextrin (g) | Microcrystalline Cellulose | Starch (g) |
| Prescription 1 | 45.5 | 7.5 | 74 | ? | ? |
| Prescription 2 | 45.5 | 7.5 | 94 | ? | ? |
| Prescription 3 | 45.5 | 7.5 | 114 | ? | ? |
| Prescription 4 | 45.5 | 7.5 | ? | 74 | ? |
| Prescription 5 | 45.5 | 7.5 | ? | 94 | ? |
| Prescription 6 | 45.5 | 7.5 | ? | 114 | ? |
| Prescription 7 | 45.5 | 7.5 | ? | ? | 74 |
| Prescription 8 | 45.5 | 7.5 | ? | ? | 94 |
| Prescription 9 | 45.5 | 7.5 | ? | ? | 114 |
The result shows that select for use the dextrin filler to granulate, grain forming property is poor, is prone to the moisture absorption, and dissolving is comparatively slow in water; Select for use starch to granulate as filler, shaping particles property is poor, the difficulty of granulating, and therefore two adjuvants should not be as filler.When selecting for use microcrystalline Cellulose to granulate, when consumption is 74g, the glutinous moisture absorption that is prone to of granule, when selecting 94g for use, the granule that makes is moderate, and therefore the unsuitable moisture absorption selects for use microcrystalline Cellulose as filler, and consumption is 94g.
The screening of dehydrated alcohol consumption
Proportioning according to prescription 5 takes by weighing material, and mix homogeneously is got 4 parts altogether, adds dehydrated alcohol according to table 13 and granulates, and serve as to investigate index with granule effervescent time and character: the result sees table 13.
The selection of table 13 wetting agent consumption
| Amount of ethanol (%) | The effervescent time (min) | Character |
| 5% | 0.5 | Loose |
| 8% | 1 | Loose slightly |
[0129]
| 11% | 1.5 | Moderate |
| 13% | 3.5 | More glutinous |
The result shows: when adding the dehydrated alcohol of total medicated powder weight 5%, loose particles is when selecting the dehydrated alcohol of total medicated powder weight 13% for use; Can be more glutinous, and the effervescent time is longer, selects 8%～11% for use; The granule that makes is moderate, so the dehydrated alcohol consumption is 8%～11% of total medicated powder weight.
Experimental example 6, the clinical experiment of five tastes manna dipping lotion for treatment rheumatoid arthritis
One, case is included standard in
(1) diagnosis of rheumatoid arthritis standard
1. adopt American Rheumatism Association's diagnostic criteria in 1987 at present usually:
(1) morning, deadlock continued to 1 hour (every day), continued at least 6 weeks;
(2) swollen joint more than 3 or 3 is arranged, continued at least 6 weeks;
(3) wrist, metacarpophalangeal joints or PIP are swollen, continue at least 6 weeks;
(4) symmetry swollen joint continued at least 6 weeks;
(5) the hands X-ray film changes;
(6) subcutaneous nodule is arranged;
(7) rheumatoid factor positive (titre>1:32).
More than possess more than 4 or 4 in 7 and can be diagnosed as rheumatoid arthritis
2. joint standards of grading
The I level: daily routines are not limited
II level: have the joint motion of moderate strength limited, but can satisfy the daily routines needs
The III level: there is tangible limitation of activity in the joint, and the patient can not be engaged in most of occupations or can not well take care of number one
The IV level: LOM or compelled bed maybe can only be sitting on the wheelchair
3.X line by stages
The I phase: normal or joint end osteoporosis
The II phase: joint end osteoporosis, idol have joint subchondral cyst appearance to destroy or bone erosion changes
The III phase: capsule property destruction under the tangible articular cartilage, the joint space is narrow, the subluxation of joint deformity
The IV phase: except II, III phase change, and fibroid or bony ankylosis are arranged.
(2) exclusion standard
1. do not meet the above-mentioned standard of including in
2. merge serious disease persons such as the heart, brain, liver, kidney and hemopoietic system
3. gestation or women breast-feeding their children, psychotic etc.
Two, testing program
MethodsThe cases enrolled successively is divided into two groups at random according to being admitted to hospital: embodiment group 60 examples, and matched group 60 examples, GP TH all obtains the patient and family members agree, two groups sex, age, the course of disease, state of an illness difference not statistically significant.Respectively at observation corresponding index before and after the patient treatment.
Three, therapeutic regimen:
Advise patient's teetotalism during the treatment, suitably reduce heat and take in.The embodiment group gives the effervescent granule novel formulation of embodiment 2, washout.Matched group gives five tastes manna lotion, washout.The contained crude drug amount of 150g effervescent granule is equivalent to the contained crude drug amount of 250ml five tastes manna lotion.Water temperature is regulated according to patient's physical condition and disease.Originally bathing, water temperature generally transfer to 38 ℃～40C, time l0～15 minute, and l course of treatment is 7 days; Water temperature can rise to about 43c by patient's physical condition gradually in the bathing the 3rd～6 day. in the time lengthening to 25 minute; Be adjusted to bathing standard originally from the 7th day water temperature and time.The hot a heatable brick bed that must crouch after each the bath perspired 5～l0 minute.Continuously with 4 courses of treatment.
Four, observation index
1. health giving quality observation
(1) cardinal symptom: arthralgia, arthroncus, joint joint stuffiness, stiff and relevant performance in morning
(2) mainly relevant sign: articular pain number, arthroncus number, function of joint, the average grip of both hands, stiff time in morning, the horizontal vision synopsis of pain 10cm method
(3) physico-chemical examination: joint X inspection, erythrocyte sedimentation rate (ESR).
2. safety indexes
(1) general health check-up item inspection
(2) hematuria routine examination
(3) hepatic and renal function inspection
(4) observe the untoward reaction that possibly occur
Observe These parameters before and after the treatment.
Five, therapeutic evaluation standard
1. cure: clinical symptoms (pain, swelling deadlock in morning, function limitation etc.) and positive sign disappear, and it is normal that each joint movement function recovers, and takes care of oneself, and erythrocyte sedimentation rate is reduced to normally, follow up a case by regular visits to not recurrence more than 1 year.
2. produce effects: clinical symptom relief, weight increase, each joint movement function partly recover normal .x line to be taken the photograph sheet and shows that soft tissue swelling disappears, and osteoporosis and bone destruction are stable, do not have recurrence and increase the weight of more than 5 months through following up a case by regular visits to.
3. take a turn for the better: pain and swelling alleviates, and each joint movement function makes moderate progress, and erythrocyte sedimentation rate obviously changes.
4. invalid: after treating for 1 course of treatment, each arthralgia does not have improvement.
Six, result of the test
Embodiment treats the rheumatoid arthritis clinical observation result
χ
2Check is compared * P with former preparation<0.05.
The above results shows: matched group 60 routine patients, cure 11 examples, and cure rate is 18.3%; Produce effects 19 examples, obvious effective rate are 31.7%; Effective 13 examples, effective percentage are 21.7%; Invalid 17 examples, inefficiency are 28.3%; Total effective rate is 71.7%.Implement 1 example group 60 routine patients, cure 15 examples, cure rate is 25%; Produce effects 24 examples, obvious effective rate are 40%; Effective 12 examples, effective percentage are 20%; Invalid 9 examples, inefficiency are 15%; Total effective rate is 85.0%.Through χ
2Check is compared with matched group, and the effervescent granule novel formulation total effective rate of embodiment 2 significantly is superior to former preparation (P<0.05).The effervescent granule novel formulation treatment rheumatoid arthritis effect of prompting embodiment 2 is superior to former preparation.
In addition, two groups of patients do not see tangible untoward reaction in the medication process, and the patients with hepatic renal function detects index all in normal range before and after the medication.
Claims (7)
1. the pharmaceutical composition of the blood stasis dispelling that is used to dehumidify is characterized in that, is processed by the raw material of following weight portion:
Volatile oil clathrate compound 10-20 weight portion, ethanol extraction 85-95 weight portion;
Described volatile oil clathrate compound makes according to following method: with Cacumen et folium sabinae przewalskii 150-250 weight portion, Cacumen Myricariae Germanicae 150-250 weight portion, Rhododendron 150-250 weight portion, Artemisia sieversiana Willd. 150-250 weight portion; Be cut into pieces, add medical material gross weight 4-9 water doubly, extract volatile oil with vapor distillation; Extraction time 3-5 hour; Get volatile oil and medicinal residues, collect volatile oil, subsequent use; Precision takes by weighing beta-schardinger dextrin-, adds distilled water and is made into the solution that contains beta-schardinger dextrin-mass percent 5%-7%, stirs, and 60 ℃ of-70 ℃ of heating in water bath make dissolving; Be cooled to 50 ℃-55 ℃, under the stirring condition, add the equal-volume mixture of volatile oil and dehydrated alcohol, make volatile oil: beta-schardinger dextrin-=1ml:4g; Sealing is stirred 3-5h ,-4 ℃ of-4 ℃ of cold preservation 12-24h, sucking filtration under 50 ℃ of-55 ℃ of conditions; Deposition, 50 ℃ of-55 ℃ of vacuum dryings are pulverized, and get volatile oil clathrate compound;
Described ethanol extraction makes according to following method: the medicinal residues after volatile oil extracts mix with 150-250 weight portion Herba Ephedrae, add medicinal residues and the total medical material amount of Herba Ephedrae the 0.25-0.3wt% distillers yeast, spray into the barley wine that 35～56 of 2-3wt% spends and ferment, after the fermentation process; The 6-10 of the total medical material amount of reuse medicinal residues and Herba Ephedrae volumetric concentration 40-60% ethanol doubly, 80 ℃ are extracted 2-4 time, 3-5 hour for the first time; Each 1-3 of second and third time hour; It is 1.33 thick paste that merge extractive liquid,, filtrate decompression are concentrated into 50 ℃ of relative densities, 70-90 ℃ vacuum drying 3-5 hour; Pulverize, get ethanol extraction.
2. the pharmaceutical composition of a kind of blood stasis dispelling that is used to dehumidify as claimed in claim 1 is characterized in that, is processed by the raw material of following weight portion:
Volatile oil clathrate compound 15 weight portions, ethanol extraction 91 weight portions;
Described volatile oil clathrate compound makes according to following method: with Cacumen et folium sabinae przewalskii 200 weight portions, Cacumen Myricariae Germanicae 200 weight portions, Rhododendron 200 weight portions, Artemisia sieversiana Willd. 200 weight portions; Be cut into pieces, add the water of 6 times of medical material gross weights, extract volatile oil with vapor distillation; 4 hours extraction times; Get volatile oil and medicinal residues, collect volatile oil, subsequent use; Precision takes by weighing beta-schardinger dextrin-, adds distilled water and is made into the solution that contains beta-schardinger dextrin-mass percent 5%, stirs, and 60 ℃ of-70 ℃ of heating in water bath make dissolving; Be cooled to 50 ℃-55 ℃, under the stirring condition, add the equal-volume mixture of volatile oil and dehydrated alcohol, make volatile oil: beta-schardinger dextrin-=1ml:4g; Sealing is stirred 4h ,-4 ℃ of cold preservation 12h, sucking filtration under 50 ℃ of conditions; Deposition, 50 ℃ of vacuum dryings are pulverized, and get volatile oil clathrate compound;
Described ethanol extraction makes according to following method: the medicinal residues after volatile oil extracts mix with 200 weight portion Herba Ephedraes, add medicinal residues and the total medical material amount of Herba Ephedrae the 0.25wt% distillers yeast, spray into 38～40 of 2wt% and spend barley wines and ferment, after the fermentation process; 8 times volumetric concentration 50% ethanol of the total medical material amount of reuse medicinal residues and Herba Ephedrae, 80 ℃ are extracted 3 times, 4 hours for the first time; Second and third time each 2 hours; It is 1.33 thick paste that merge extractive liquid,, filtrate decompression are concentrated into 50 ℃ of relative densities, 80 ℃ of vacuum dryings 4 hours; Pulverize, get ethanol extraction.
3. the drug combination preparation of the blood stasis dispelling that is used to dehumidify is characterized in that it being to add conventional adjuvant by claim 1 or 2 a kind of be used to dehumidify pharmaceutical composition of blood stasis dispelling, processes effervescent granule according to common process; Said adjuvant comprises one or more of solvent, disintegrating agent, antiseptic, binding agent, lubricant.
4. the drug combination preparation of a kind of blood stasis dispelling that is used to dehumidify as claimed in claim 3; It is characterized in that described effervescent granule, process: volatile oil clathrate compound 15g, ethanol extraction 91g, sodium bicarbonate 55g, citric acid 45g, microcrystalline Cellulose 94g by the raw material of following weight portion;
Described volatile oil clathrate compound makes according to following method: with Cacumen et folium sabinae przewalskii 200g, Cacumen Myricariae Germanicae 200g, Rhododendron 200g, Artemisia sieversiana Willd. 200g; Be cut into pieces, add the water of 6 times of medical material gross weights, extract volatile oil with vapor distillation; 4 hours extraction times; Get volatile oil and medicinal residues, collect volatile oil, subsequent use; Precision takes by weighing beta-schardinger dextrin-, adds distilled water and is made into the solution that contains beta-schardinger dextrin-mass percent 5%, stirs, and 60 ℃ of-70 ℃ of heating in water bath make dissolving; Be cooled to 50 ℃-55 ℃, under the stirring condition, add the equal-volume mixture of volatile oil and dehydrated alcohol, make volatile oil: beta-schardinger dextrin-=1ml:4g; Sealing is stirred 4h ,-4 ℃ of cold preservation 12h, sucking filtration under 50 ℃ of conditions; Deposition, 50 ℃ of vacuum dryings are pulverized, and get volatile oil clathrate compound;
Described ethanol extraction makes according to following method: the medicinal residues after volatile oil extracts mix with the 200g Herba Ephedrae, add medicinal residues and the total medical material amount of Herba Ephedrae the 0.25wt% distillers yeast, spray into 38～40 of 2wt% and spend barley wines and ferment, after the fermentation process; 8 times volumetric concentration 50% ethanol of the total medical material amount of reuse medicinal residues and Herba Ephedrae, 80 ℃ are extracted 3 times, 4 hours for the first time; Second and third time each 2 hours; It is 1.33 thick paste that merge extractive liquid,, filtrate decompression are concentrated into 50 ℃ of relative densities, 80 ℃ of vacuum dryings 4 hours; Pulverize, get ethanol extraction.
5. according to claim 1 or claim 2 a kind of preparation of drug combination method of blood stasis dispelling that is used to dehumidify is characterized in that step is following:
(1) with Cacumen et folium sabinae przewalskii 150-250 weight portion, Cacumen Myricariae Germanicae 150-250 weight portion, Rhododendron 150-250 weight portion, Artemisia sieversiana Willd. 150-250 weight portion; Be cut into pieces, add medical material gross weight 4-9 water doubly, extract volatile oil with vapor distillation; Extraction time 3-5 hour; Get volatile oil and medicinal residues, collect volatile oil, subsequent use; Precision takes by weighing beta-schardinger dextrin-, adds distilled water and is made into the solution that contains beta-schardinger dextrin-mass percent 5%-7%, stirs, and 60 ℃ of-70 ℃ of heating in water bath make dissolving; Be cooled to 50 ℃-55 ℃, under the stirring condition, add the equal-volume mixture of volatile oil and dehydrated alcohol, make volatile oil: beta-schardinger dextrin-=1ml:4g; Sealing is stirred 3-5h ,-4 ℃ of-4 ℃ of cold preservation 12-24h, sucking filtration under 50 ℃ of-55 ℃ of conditions; Deposition, 50 ℃ of-55 ℃ of vacuum dryings are pulverized, and get volatile oil clathrate compound;
(2) medicinal residues after volatile oil extracts mix with 150-250 weight portion Herba Ephedrae, add medicinal residues and the total medical material amount of Herba Ephedrae the 0.25-0.3wt% distillers yeast, spray into 35～56 of 2-3wt% and spend barley wines and ferment, after the fermentation process; The 6-10 of the total medical material amount of reuse medicinal residues and Herba Ephedrae volumetric concentration 40-60% ethanol doubly, 80 ℃ are extracted 2-4 time, 3-5 hour for the first time; Each 1-3 of second and third time hour; It is 1.33 thick paste that merge extractive liquid,, filtrate decompression are concentrated into 50 ℃ of relative densities, 70-90 ℃ vacuum drying 3-5 hour; Pulverize, get ethanol extraction;
(3) ethanol extraction that volatile oil clathrate compound that step (1) is made and step (2) make mixes, and promptly gets.
6. the preparation of drug combination method of a kind of blood stasis dispelling that is used to dehumidify as claimed in claim 5 is characterized in that step is following:
(1) with Cacumen et folium sabinae przewalskii 200 weight portions, Cacumen Myricariae Germanicae 200 weight portions, Rhododendron 200 weight portions, Artemisia sieversiana Willd. 200 weight portions, is cut into pieces, adds the water of 6 times of medical material gross weights; Extract volatile oil with vapor distillation, 4 hours extraction times, get volatile oil and medicinal residues; Collect volatile oil, subsequent use; Precision takes by weighing beta-schardinger dextrin-, adds distilled water and is made into the solution that contains beta-schardinger dextrin-mass percent 5%, stirs, and 60 ℃ of-70 ℃ of heating in water bath make dissolving; Be cooled to 50 ℃-55 ℃, under the stirring condition, add the equal-volume mixture of volatile oil and dehydrated alcohol, make volatile oil: beta-schardinger dextrin-=1ml:4g; Sealing is stirred 4h ,-4 ℃ of cold preservation 12h, sucking filtration under 50 ℃ of conditions; Deposition, 50 ℃ of vacuum dryings are pulverized, and get volatile oil clathrate compound;
(2) medicinal residues after volatile oil extracts mix with 200 weight portion Herba Ephedraes, add medicinal residues and the total medical material amount of Herba Ephedrae the 0.25wt% distillers yeast, spray into 38～40 of 2wt% and spend barley wines and ferment, after the fermentation process; 8 times volumetric concentration 50% ethanol of the total medical material amount of reuse medicinal residues and Herba Ephedrae, 80 ℃ are extracted 3 times, 4 hours for the first time; Second and third time each 2 hours, merge extractive liquid,, it is 1.33 thick paste that filtrate decompression is concentrated into 50 ℃ of relative densities; 80 ℃ of vacuum dryings 4 hours are pulverized, ethanol extraction;
(3) ethanol extraction that volatile oil clathrate compound that step (1) is made and step (2) make mixes, and promptly gets.
7. the drug combination preparation of a kind of blood stasis dispelling that is used to dehumidify as claimed in claim 4 is characterized in that the method for preparing of described effervescent granule, and step is following:
(1) with Cacumen et folium sabinae przewalskii 200g, Cacumen Myricariae Germanicae 200g, Rhododendron 200g, Artemisia sieversiana Willd. 200g, be cut into pieces, add the water of 6 times of medical material gross weights, extract volatile oil with vapor distillation, 4 hours extraction times, get volatile oil and medicinal residues, collect volatile oil, subsequent use; Precision takes by weighing beta-schardinger dextrin-, adds distilled water and is made into the solution that contains beta-schardinger dextrin-mass percent 5%, stirs, and 60 ℃ of-70 ℃ of heating in water bath make dissolving; Be cooled to 50 ℃-55 ℃, under the stirring condition, add the equal-volume mixture of volatile oil and dehydrated alcohol, make volatile oil: beta-schardinger dextrin-=1ml:4g; Sealing is stirred 4h ,-4 ℃ of cold preservation 12h, sucking filtration under 50 ℃ of conditions; Deposition, 50 ℃ of vacuum dryings are pulverized, and get volatile oil clathrate compound;
(2) medicinal residues after volatile oil extracts mix with the 200g Herba Ephedrae, add medicinal residues and the total medical material amount of Herba Ephedrae the 0.25wt% distillers yeast, spray into 38～40 of 2wt% and spend barley wines and ferment, after the fermentation process; 8 times volumetric concentration 50% ethanol of the total medical material amount of reuse medicinal residues and Herba Ephedrae, 80 ℃ are extracted 3 times, 4 hours for the first time; Second and third time each 2 hours, merge extractive liquid,, it is 1.33 thick paste that filtrate decompression is concentrated into 50 ℃ of relative densities; 80 ℃ of vacuum dryings 4 hours are pulverized, ethanol extraction;
(3) ethanol extraction that volatile oil clathrate compound that step (1) is made and step (2) make mixes, and adds sodium bicarbonate, citric acid, and dehydrated alcohol is done wetting agent, mixing, and 16 orders are granulated, 50 ℃ of dryings 2 hours, 18 order granulate, pack promptly gets.
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| CN1733025A (en) * | 2005-08-23 | 2006-02-15 | 甘肃省药物研究所 | Pharmaceutical composition for treating rheumatic and rheumatoid diseases and its preparation process |
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| 《中成药地方标准上升国家标准》 20021231 WS-11385(ZD-1385)-2002 五味甘露药浴颗粒 , * |
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