Summary of the invention
The object of the invention is to for the deficiencies in the prior art, provide a kind of Chinese medicine composition root pain flat new preparation method, thereby improve its curative effect, improve its stability.
In order to solve the problems of the technologies described above, the present invention adopts following technical scheme:
A preparation method for Chinese medicine composition, in weight portion, the crude drug of described Chinese medicine composition consists of:
The Radix Paeoniae Alba 100~300, Radix Puerariae 25~75, Dan Semen Persicae 25~75, Flos Carthami 25~75, processed with vinegar Olibanum 25~75, processed with vinegar Myrrha 25~75, Radix Dipsaci 45~105, boiling hot Rhizoma Cibotii 45~105, Herba Lycopodii 45~105, Radix Achyranthis Bidentatae 25~75, Radix Rehmanniae 25~75, Radix Glycyrrhizae 15~35
Described preparation method comprises the steps:
(1) according to described weight portion, prepare crude drug;
(2) get Olibanum, Myrrha extraction volatile oil, medicinal residues are standby; Volatile oil carries out enclose with beta-schardinger dextrin-, obtains volatile oil clathrate compound;
(3) ethanol water hot reflux that the medicinal residues that step 2 obtains are 60~80% with other raw material medicinal alcohol concentration expressed in percentage by volumes is extracted, and alcohol extract reclaims ethanol, measures relative density and be 1.2 extractum while being concentrated into 80 ℃, obtains alcohol extract; Medicinal residues are standby;
(4) step 3 obtains medicinal residues water hot reflux is extracted, and measures relative density and be 1.2 extractum when aqueous extract is concentrated into 80 ℃, the described alcohol extract that adds step 2 to obtain, and mix homogeneously, obtains total extract;
(5) get the described total extract that step 4 obtains, the described volatile oil clathrate compound that adds acceptable adjuvant pharmaceutically and step 2 to obtain, makes acceptable preparation clinically.
Preferably, the crude drug of described Chinese medicine composition consists of:
The Radix Paeoniae Alba 200, Radix Puerariae 50, Dan Semen Persicae 50, Flos Carthami 50, processed with vinegar Olibanum 50, processed with vinegar Myrrha 50, Radix Dipsaci 75, boiling hot Rhizoma Cibotii 75, Herba Lycopodii 75, Radix Achyranthis Bidentatae 50, Radix Rehmanniae 50, Radix Glycyrrhizae 25.
In aforesaid preparation method, preferred, in step 2, Olibanum, Myrrha extraction by steam distillation volatile oil.
Preferably, in step 2, described volatile oil adds anhydrous alcohol solution, with beta-cyclodextrin inclusion compound;
Wherein, the weight of beta-schardinger dextrin-be volatile oil volume 4~8 times, be preferably 6 times.
Preferably, in step 3, the ethanol water that the medicinal residues that step 2 obtains are 60~80% with other crude drug by the ethanol concentration expressed in percentage by volume of 8~10 times of medical material weight soaks 1 hour, and then heating and refluxing extraction twice, each 1.5 hours; Preferred, the concentration expressed in percentage by volume of ethanol is 70%.
Preferably, in step 4,6~12 times of medical material weight for the medicinal residues that step 3 obtains, are preferably the water heating and refluxing extraction twice of 8 times, each 1~2 hour.
Preferably, the described preparation of acceptable is clinically selected from granule, tablet, capsule, oral liquid or syrup; Granule more preferably.
Preferred embodiment the invention provides the preparation method of the flat granule of a kind of Chinese medicine composition root pain as one, in weight portion, the crude drug of the described flat granule of pain consists of:
The Radix Paeoniae Alba 200, Radix Puerariae 50, Dan Semen Persicae 50, Flos Carthami 50, processed with vinegar Olibanum 50, processed with vinegar Myrrha 50, Radix Dipsaci 75, boiling hot Rhizoma Cibotii 75, Herba Lycopodii 75, Radix Achyranthis Bidentatae 50, Radix Rehmanniae 50, Radix Glycyrrhizae 25,
Described preparation method comprises the steps:
(1) according to described weight portion, prepare crude drug;
(2) get Olibanum, Myrrha, extraction by steam distillation volatile oil is to complete, and medicinal residues are standby; Volatile oil adds anhydrous alcohol solution, and taking weight is the beta-schardinger dextrin-of 4~8 times of volatile oil volumes, adds the water of 16~20 times of beta-schardinger dextrin-weight, and mix homogeneously, obtains beta-schardinger dextrin-aqueous solution; Under 150 revs/min of rotating speeds, slowly to described beta-schardinger dextrin-aqueous solution, add volatile oil ethanol, after adding, continue to stir 0.5 hour, cold preservation 12 hours, filters, and will filter to obtain thing oven drying at low temperature at 45 ℃, obtains the volatile oil clathrate compound of white loose;
(3) ethanol water that the medicinal residues that step 2 obtains are 70% with other crude drug by the ethanol concentration expressed in percentage by volume of 8~10 times of medical material weight soaks 1 hour, then hot reflux is extracted twice, each 1.5 hours, merge alcohol extract, reclaim ethanol, while being evaporated to 80 ℃, measure relative density and be 1.2 extractum, obtain alcohol extract; Medicinal residues are standby;
(4) twice of 6~12 times of hydro-thermal reflux, extract, of medical material weight of the medicinal residues that step 3 obtains, each 1~2 hour, filter, merge twice filtrate, add the aqueous solution after the distillation that step 2 obtains, standing, filter, when filtrate is concentrated into 80 ℃, measure relative density and be 1.2 extractum, the described alcohol extract that adds step 2 to obtain, mix homogeneously, obtains total extract;
(5) get the described total extract that step 4 obtains, add pharmaceutically acceptable adjuvant, spray granulation, the described volatile oil clathrate compound obtaining with step 2 is mixed homogeneously, and obtains.
The Chinese medicine composition that provides aforesaid preparation method to prepare is provided another object of the present invention.
The present invention also has a goal of the invention to be to provide the application of aforesaid Chinese medicine composition in the medicine of takeing on neck pain, limitation of activity, upper limb numbness due to wind-cold channel blocking network.
Pharmaceutically acceptable adjuvant of the present invention, comprise (1) diluent, such as starch, Icing Sugar, dextrin, lactose, pregelatinized Starch, microcrystalline cellulose, inorganic calcium salt (as calcium sulfate, calcium hydrogen phosphate, medicinal calcium carbonate etc.), mannitol etc., vegetable oil, Polyethylene Glycol etc.; (2) binding agent, such as distilled water, ethanol, starch slurry, sodium carboxymethyl cellulose, hydroxypropyl cellulose, methylcellulose and ethyl cellulose, hypromellose etc.; (3) disintegrating agent, such as dried starch, carboxymethyl starch sodium, low-substituted hydroxypropyl cellulose, crospolyvinylpyrrolidone, cross-linking sodium carboxymethyl cellulose etc.; (4) lubricant, such as magnesium stearate, micropowder silica gel, Pulvis Talci, hydrogenated vegetable oil, polyethylene glycols, magnesium laurylsulfate etc.(5) correctives, as sucrose, steviosin etc.
Useful technique effect of the present invention is: improved the extracting method of medical material, each effective constituents can be extracted more completely.Assay result shows, the flat granule of root pain that preparation method of the present invention prepares, and volatile oil content is 0.021ml/8g, paeoniflorin content is 31.26mg/8g.And the flat granule of root prepared by the method that pharmacopeia is recorded pain does not detect volatile oil, the content of peoniflorin is less than 27mg/8g.The more important thing is, pharmacological evaluation proves, the Chinese medicine composition that the method for the invention prepares is obviously better than the of the prior art flat granule of pain in the effect that improves microcirculation, ease pain.Illustrate that preparation method of the present invention has significantly improved the flat curative effect of Chinese medicine composition root pain.
The specific embodiment
Referring to specific embodiment, the present invention is described.It will be appreciated by those skilled in the art that these embodiment are only for the present invention is described, the scope that it does not limit the present invention in any way.
Experimental technique in following embodiment, if no special instructions, is conventional method.In following embodiment, medicinal raw material used, reagent material etc., if no special instructions, be commercially available purchase product.
embodiment 1a kind of flat granule of pain
Crude drug prescription is:
Radix Paeoniae Alba 200g, Radix Puerariae 50g, Dan Semen Persicae 50g, Flos Carthami 50g, processed with vinegar Olibanum 50g, processed with vinegar Myrrha 50g, Radix Dipsaci 75g, boiling hot Rhizoma Cibotii 75g, Herba Lycopodii 75g, Radix Achyranthis Bidentatae 50g, Radix Rehmanniae 50g, Radix Glycyrrhizae 25g
Preparation by the following method:
(1) according to prescription, prepare ingredients.
(2) get Olibanum, Myrrha adds 1kg water (10 times of amounts), with extraction by steam distillation volatile oil 5 hours, the another device of aqueous solution after distillation was collected, medicinal residues are standby; Volatile oil adds appropriate anhydrous alcohol solution, and taking weight is the beta-schardinger dextrin-of 6 times of volatile oil volumes, adds the water of 20 times of beta-schardinger dextrin-weight, and mix homogeneously, obtains beta-schardinger dextrin-aqueous solution; Under 150 revs/min of rotating speeds, slowly to described beta-schardinger dextrin-aqueous solution, add volatile oil ethanol, after adding, continue to stir 0.5 hour, cold preservation 12 hours, filters, and will filter to obtain thing oven drying at low temperature at 45 ℃, obtains the volatile oil clathrate compound of white loose.
(3) it is that 70% ethanol water 6.4kg (medical material weight 8 times) soaks 1 hour that the medicinal residues that step 2 obtains add ethanol concentration expressed in percentage by volume with other ten tastes medical materials, hot reflux is extracted 2 times, each 1.5 hours, filter, merging filtrate, filtrate recycling ethanol, measures relative density and is 1.2 extractum while being evaporated to 80 ℃, obtain alcohol extract, medicinal residues are standby.
(4) medicinal residues that step 3 obtains add water 6.4kg (medical material weight 8 times), reflux, extract, 2 times, each 1.5 hours, filter, merge the aqueous solution after the distillation that twice filtrate and step 2 obtain, standing, filter, when filtrate decompression is concentrated into 80 ℃, measure relative density and be 1.2 extractum, the alcohol extract that adds step 3 to obtain, mix homogeneously, obtains total extract.
(5) get the total extract that step 4 obtains, add dextrin and the steviosin 3.3g of 400g, mix, spray-drying process, the volatile oil clathrate compound that adds step 2 to obtain, obtains 650g, pack, every bag of 8g, makes 80 bags altogether.
Consumption usage: boiled water is taken after mixing it with water.One time 1 bag, 2 times on the one.One after each meal.Or follow the doctor's advice.
embodiment 2a kind of flat granule of pain
Crude drug prescription:
Radix Paeoniae Alba 100g, Radix Puerariae 25g, Dan Semen Persicae 25g, Flos Carthami 25g, processed with vinegar Olibanum 25g, processed with vinegar Myrrha 25g, Radix Dipsaci 45g, boiling hot Rhizoma Cibotii 45g, Herba Lycopodii 45g, Radix Achyranthis Bidentatae 25g, Radix Rehmanniae 25g, Radix Glycyrrhizae 15g
Preparation by the following method:
(1) according to prescription, prepare ingredients.
(2) get Olibanum, Myrrha adds 0.5kg water (10 times of amounts), with extraction by steam distillation volatile oil 5 hours, the another device of aqueous solution after distillation was collected, medicinal residues are standby; Volatile oil adds appropriate anhydrous alcohol solution, and taking weight is the beta-schardinger dextrin-of 4 times of volatile oil volumes, adds the water of 16 times of beta-schardinger dextrin-weight, and mix homogeneously, obtains beta-schardinger dextrin-aqueous solution; Under 150 revs/min of rotating speeds, slowly to described beta-schardinger dextrin-aqueous solution, add volatile oil ethanol, after adding, continue to stir 0.5 hour, cold preservation 12 hours, filters, and will filter to obtain thing oven drying at low temperature at 45 ℃, obtains the volatile oil clathrate compound of white loose.
(3) it is that 60% ethanol water 4.25kg (medical material weight 10 times) soaks 1 hour that the medicinal residues that step 2 obtains add ethanol concentration expressed in percentage by volume with other ten tastes medical materials, hot reflux is extracted twice, each 1.5 hours, filter, merging filtrate, filtrate recycling ethanol, measures relative density and is 1.2 extractum while being evaporated to 80 ℃, obtain alcohol extract; Medicinal residues are standby.
(4) medicinal residues that step 3 obtains add water 4.25kg (medical material weight 10 times), reflux, extract, 2 times, each 1.5 hours, filter, merge the aqueous solution after the distillation that twice filtrate and step 2 obtain, standing, filter, when filtrate decompression is concentrated into 80 ℃, measure relative density and be 1.2 extractum, the alcohol extract that adds step 3 to obtain, mix homogeneously, obtains total extract.
(5) get the total extract that step 4 obtains, add 200g dextrin and 1.6g steviosin, mix, spray-drying process, the volatile oil clathrate compound that adds step 2 to obtain, obtains 325g, pack, every bag of 8g, makes 40 bags altogether.
Consumption usage: boiled water is taken after mixing it with water.One time 1 bag, 2 times on the one.One after each meal.Or follow the doctor's advice.
embodiment 3a kind of pain plain film
Crude drug prescription:
Radix Paeoniae Alba 300g, Radix Puerariae 75g, Dan Semen Persicae 75g, Flos Carthami 75g, processed with vinegar Olibanum 75g, processed with vinegar Myrrha 75g, Radix Dipsaci 105g, boiling hot Rhizoma Cibotii 105g, Herba Lycopodii 105g, Radix Achyranthis Bidentatae 75g, Radix Rehmanniae 75g, Radix Glycyrrhizae 35g
Preparation by the following method:
(1) according to prescription, prepare ingredients.
(2) get Olibanum, Myrrha adds 1.5kg water (10 times of amounts), with extraction by steam distillation volatile oil 5 hours, the another device of aqueous solution after distillation was collected; Volatile oil adds appropriate anhydrous alcohol solution, and taking weight is the beta-schardinger dextrin-of 8 times of volatile oil volumes, adds the water of 20 times of beta-schardinger dextrin-weight, and mix homogeneously, obtains beta-schardinger dextrin-aqueous solution; Under 150 revs/min of rotating speeds, slowly to described beta-schardinger dextrin-aqueous solution, add volatile oil ethanol, after adding, continue to stir 0.5 hour, cold preservation 12 hours, filters, and will filter to obtain thing oven drying at low temperature at 45 ℃, obtains the volatile oil clathrate compound of white loose.
(3) it is that 70% ethanol water 9.4kg (medical material weight 8 times) soaks 1 hour that the medicinal residues that step 2 obtains add ethanol concentration expressed in percentage by volume with other ten tastes medical materials, hot reflux is extracted twice, each 2 hours, filter, merging filtrate, filtrate recycling ethanol, measures relative density and is 1.2 extractum while being evaporated to 80 ℃, obtain alcohol extract, medicinal residues are standby.
(4) medicinal residues that step 3 obtains add water 9.4kg (medical material weight 8 times), reflux, extract, 2 times, each 2 hours, filter, merge the aqueous solution after the distillation that twice filtrate and step 2 obtain, standing, filter, when filtrate decompression is concentrated into 80 ℃, measure relative density and be 1.2 extractum, the alcohol extract that adds step 3 to obtain, mix homogeneously, obtains total extract.
(5) get the total extract that step 4 obtains, add the dextrin of 150g, mix, granulation, dry, the volatile oil clathrate compound that adds step 2 to obtain, mixes, tabletting, every 0.5g, makes 1000 altogether.
Consumption usage: oral, one time 5,3 times on the one; One after each meal or follow the doctor's advice.
embodiment 4a kind of 'Gentongping ' capsule
Crude drug prescription:
Radix Paeoniae Alba 300g, Radix Puerariae 75g, Dan Semen Persicae 25g, Flos Carthami 25g, processed with vinegar Olibanum 50g, processed with vinegar Myrrha 50g, Radix Dipsaci 50g, boiling hot Rhizoma Cibotii 50g, Herba Lycopodii 75g, Radix Achyranthis Bidentatae 75g, Radix Rehmanniae 75g, Radix Glycyrrhizae 25g
Preparation by the following method:
(1) according to prescription, prepare ingredients.
(2) get Olibanum, Myrrha adds 1.0kg water (10 times of amounts), with extraction by steam distillation volatile oil 5 hours, the another device of aqueous solution after distillation was collected, medicinal residues are standby; Volatile oil adds appropriate anhydrous alcohol solution, and taking weight is the beta-schardinger dextrin-of 5 times of volatile oil volumes, adds the water of 18 times of beta-schardinger dextrin-weight, and mix homogeneously, obtains beta-schardinger dextrin-aqueous solution; Under 150 revs/min of rotating speeds, slowly to described beta-schardinger dextrin-aqueous solution, add volatile oil ethanol, after adding, continue to stir 0.5 hour, cold preservation 12 hours, filters, and will filter to obtain thing oven drying at low temperature at 45 ℃, obtains the volatile oil clathrate compound of white loose.
(3) it is that 80% ethanol water 8.75kg (medical material weight 10 times) soaks 1 hour that the medicinal residues that step 2 obtains add ethanol concentration expressed in percentage by volume with other ten tastes medical materials, hot reflux is extracted twice, each 2 hours, filter, merging filtrate, filtrate recycling ethanol, measures relative density and is 1.2 extractum while being evaporated to 80 ℃, obtain alcohol extract, medicinal residues are standby.
(4) medicinal residues that step 3 obtains add water 8.75kg (medical material weight 10 times), reflux, extract, 2 times, each 2 hours, filter, merge the aqueous solution after the distillation that twice filtrate and step 2 obtain, standing, filter, when filtrate decompression is concentrated into 80 ℃, measure relative density and be 1.2 extractum, the alcohol extract that adds step 3 to obtain, mix homogeneously, obtains total extract.
(5) get the total extract that step 4 obtains, add the starch of 100g, mix, granulation, dry, the volatile oil clathrate compound that adds step 2 to obtain, mixes, encapsulated, and 0.5g/ capsule makes 750 capsules altogether.
Consumption usage: oral, one time 5,3 times on the one; One after each meal or follow the doctor's advice.
embodiment 5a kind of flat oral liquid of pain
Crude drug prescription:
Radix Paeoniae Alba 150g, Radix Puerariae 30g, Dan Semen Persicae 30g, Flos Carthami 30g, processed with vinegar Olibanum 45g, processed with vinegar Myrrha 45g, Radix Dipsaci 60g, boiling hot Rhizoma Cibotii 60g, Herba Lycopodii 60g, Radix Achyranthis Bidentatae 30g, Radix Rehmanniae 30g, Radix Glycyrrhizae 20g
Preparation by the following method:
(1) according to prescription, prepare ingredients.
(2) get Olibanum, Myrrha adds 0.9kg water (10 times of amounts), with extraction by steam distillation volatile oil 5 hours, the another device of aqueous solution after distillation was collected, medicinal residues are standby; Taking weight is the beta-schardinger dextrin-of 7 times of volatile oil volumes, adds the water of 17 times of beta-schardinger dextrin-weight, and mix homogeneously, obtains beta-schardinger dextrin-aqueous solution; Under 150 revs/min of rotating speeds, slowly to described beta-schardinger dextrin-aqueous solution, add volatile oil ethanol, after adding, continue to stir 0.5 hour, cold preservation 12 hours, filters, and will filter to obtain thing oven drying at low temperature at 45 ℃, obtains the volatile oil clathrate compound of white loose.
(3) it is that 75% ethanol water 4.72kg (medical material weight 8 times) soaks 1 hour that the medicinal residues that step 2 obtains add ethanol concentration expressed in percentage by volume with other medical materials, hot reflux is extracted 2 times, each 1.5 hours, filter, merging filtrate, filtrate recycling ethanol, measures relative density and is 1.2 extractum while being evaporated to 80 ℃, obtain alcohol extract, medicinal residues are standby.
(4) medicinal residues that step 3 obtains add water 4.72kg (medical material weight 8 times), reflux, extract, 2 times, each 1.5 hours, filter, merge the aqueous solution after the distillation that twice filtrate and step 2 obtain, standing, filter, when filtrate decompression is concentrated into 80 ℃, measure relative density and be 1.2 extractum, the alcohol extract that adds step 3 to obtain, mix homogeneously, obtains total extract.
(5) get the total extract that step 4 obtains, add dextrin and the 270g sucrose of 270g, mix, granulation, dry, the volatile oil clathrate compound that adds step 2 to obtain, obtains 750g, pack, every bag of 12g, restricts 60 bags altogether.
Consumption usage: boiled water is taken after mixing it with water.One time 1 bag, 2 times on the one.One after each meal.Or follow the doctor's advice.
embodiment 6a kind of flat granule of pain
Crude drug prescription is:
Radix Paeoniae Alba 200g, Radix Puerariae 50g, Dan Semen Persicae 50g, Flos Carthami 50g, processed with vinegar Olibanum 50g, processed with vinegar Myrrha 50g, Radix Dipsaci 75g, boiling hot Rhizoma Cibotii 75g, Herba Lycopodii 75g, Radix Achyranthis Bidentatae 50g, Radix Rehmanniae 50g, Radix Glycyrrhizae 25g
Preparation by the following method:
(1) according to prescription, prepare ingredients.
(2) get Olibanum, Myrrha adds 1.0kg water (10 times of amounts), with extraction by steam distillation volatile oil 5 hours, the another device of aqueous solution after distillation was collected, medicinal residues are standby; Volatile oil adds appropriate anhydrous alcohol solution, and taking weight is the beta-schardinger dextrin-of 6 times of volatile oil volumes, adds the water of 20 times of beta-schardinger dextrin-weight, and mix homogeneously, obtains beta-schardinger dextrin-aqueous solution; Under 150 revs/min of rotating speeds, slowly to described beta-schardinger dextrin-aqueous solution, add volatile oil ethanol, after adding, continue to stir 0.5 hour, cold preservation 12 hours, filters, and will filter to obtain thing oven drying at low temperature at 45 ℃, obtains the volatile oil clathrate compound of white loose.
(3) it is that 70% ethanol water 8kg (medical material weight 10 times) soaks 1 hour that the medicinal residues that step 2 obtains add ethanol concentration expressed in percentage by volume with other ten tastes medical materials, hot reflux is extracted 3 times, each 1.5 hours, filter, merging filtrate, filtrate recycling ethanol, measures relative density and is 1.2 extractum while being evaporated to 80 ℃, obtain alcohol extract, medicinal residues are standby.
(4) medicinal residues that step 3 obtains add water 8kg (medical material weight 10 times), reflux, extract, 3 times, each 1.5 hours, filter, merge the aqueous solution after the distillation that twice filtrate and step 2 obtain, standing, filter, when filtrate decompression is concentrated into 80 ℃, measure relative density and be 1.2 extractum, the alcohol extract that adds step 3 to obtain, mix homogeneously, obtains total extract.
(5) get the total extract that step 4 obtains, add 400g dextrin and 3.3g steviosin, mix, granulation, dry, the volatile oil clathrate compound that adds step 2 to obtain, obtains 650g altogether, pack, every bag of 8g, restricts 80 bags altogether.
Consumption usage: boiled water is taken after mixing it with water.One time 1 bag, 2 times on the one.One after each meal.Or follow the doctor's advice.
comparative example 1a kind of medicament composition granule
Crude drug prescription:
Radix Paeoniae Alba 200g, Radix Puerariae 50g, Dan Semen Persicae 50g, Flos Carthami 50g, processed with vinegar Olibanum 50g, processed with vinegar Myrrha 50g, Radix Dipsaci 75g, boiling hot Rhizoma Cibotii 75g, Herba Lycopodii 75g, Radix Achyranthis Bidentatae 50g, Radix Rehmanniae 50g, Radix Glycyrrhizae 25g
Above 12 tastes, add 8 times of water gagings and decoct three times, 1.5 hours for the first time, second and third time each 1 hour, decocting liquid filtered, and filtrate merges, be evaporated in right amount, add 450g dextrin and 3.3g steviosin, mix, dry, pulverize into fine powder, granulation, dry, make 650g, pack, every bag of 8g, obtains approximately 80 bags altogether.
comparative example 2a kind of medicament composition granule
Crude drug prescription:
Radix Paeoniae Alba 200g, Radix Puerariae 50g, Dan Semen Persicae 50g, Flos Carthami 50g, processed with vinegar Olibanum 50g, processed with vinegar Myrrha 50g, Radix Dipsaci 75g, boiling hot Rhizoma Cibotii 75g, Herba Lycopodii 75g, Radix Achyranthis Bidentatae 50g, Radix Rehmanniae 50g, Radix Glycyrrhizae 25g
(1) above 12 tastes, add 70% ethanol 6.4kg (8 times of medical material weight) and soak 1 hour, and hot reflux is extracted 2 times, each 1.5 hours, filter merging filtrate, filtrate recycling ethanol, while being evaporated to 80 ℃, measure relative density and be 1.2 extractum, obtain alcohol extract, medicinal residues are standby.
(2) medicinal residues that step 2 obtains add water 6.4kg (8 times of medical material weight), reflux, extract, 2 times, each 1.5 hours, filter, merge twice filtrate, standing, filter, when filtrate decompression is concentrated into 80 ℃, measure relative density and be 1.2 extractum, the alcohol extract that adds step 1 to obtain, mix homogeneously, obtains total extract.
(3) get the total extract that step 2 obtains, add the appropriate dextrin of 400g and steviosin 3.3g, mix, granulation, dry, make 650g, pack, every bag of 8g, makes approximately 80 bags altogether.
comparative example 3a kind of medicament composition granule
Radix Paeoniae Alba 200g, Radix Puerariae 50g, Dan Semen Persicae 50g, Flos Carthami 50g, Olibanum (processed with vinegar) 50g, Myrrha (processed with vinegar) 50g, Radix Dipsaci 75g, Rhizoma Cibotii (scalding) 75g, Herba Lycopodii 75g, Radix Achyranthis Bidentatae 50g, Radix Rehmanniae 50g, Radix Glycyrrhizae 25g
(1) get Olibanum, Myrrha adds 10 times of water, with extraction by steam distillation volatile oil 5 hours, the another device of aqueous solution after distillation was collected, medicinal residues are standby; Volatile oil adds appropriate anhydrous alcohol solution, and taking weight is the beta-schardinger dextrin-of 6 times of volatile oil volumes, adds the water of 20 times of beta-schardinger dextrin-weight, and mix homogeneously, obtains beta-schardinger dextrin-aqueous solution; Under 150 revs/min of rotating speeds, slowly to described beta-schardinger dextrin-aqueous solution, add volatile oil ethanol, after adding, continue to stir 0.5 hour, cold preservation 12 hours, filters, and will filter to obtain thing oven drying at low temperature at 45 ℃, obtains the volatile oil clathrate compound of white loose.
(2) medicinal residues and other flavour of a drug add 8 times of amounts of water, and reflux, extract, 2 times each 1.5 hours, filters, merge the aqueous solution after twice filtrate and above-mentioned distillation, standing, filter, when being concentrated into 80 ℃, filtrate decompression measures relative density and is 1.2 extractum, add 400g dextrin and steviosin 3.3g, mix, dry, be ground into fine powder, granulation, the volatile oil clathrate compound that adds step 1 to obtain, dry, make 650g, pack, every bag of 8g, makes approximately 80 bags altogether.
experimental example 1volatile oil content testing
By the assay method of < < Chinese Pharmacopoeia > > appendix X D first method, the sample of embodiment 1 and comparative example 1~3 preparation is carried out the mensuration of volatile oil content, the results are shown in Table 1.
Table 1 volatile oil content testing
Group |
Embodiment 1 |
Comparative example 1 |
Comparative example 2 |
Comparative example 3 |
Volatile oil content (ml/8g) |
0.021 |
Do not detect |
Do not detect |
0.020 |
Conclusion: water or with alcohol extraction only, in Chinese medicine composition, can't detect volatile oil, the main effective ingredient of Olibanum, Myrrha cannot play a role in pharmaceutical composition.
experimental example 2the mensuration of paeoniflorin content
Adopt with the following method, the flat granule of root pain that embodiment 1 is prepared, the pharmaceutical composition that comparative example 1~3 prepares carry out the mensuration of paeoniflorin content.
The assay method of peoniflorin:
Chromatographic condition: take octadecylsilane chemically bonded silica as filler; Isopropyl alcohol-methanol-acetic acid-the water (1:23:1:75) of take is mobile phase; Detection wavelength is 230nm.
The preparation of reference substance solution: get peoniflorin reference substance appropriate, accurately weighed, add methanol and make every 1ml containing the solution of 50 μ g, obtain.
The preparation of need testing solution: get the sample under content uniformity item, porphyrize, gets about 1g, accurately weighed, to put in tool plug conical flask, precision adds methanol 25ml, close plug, weighed weight, reflux 2 hours, let cool, more weighed weight, with methanol, supply the weight of less loss, shake up, filter, get subsequent filtrate, obtain.
Algoscopy is accurate reference substance solution and each 10 μ l of need testing solution of drawing respectively, and injection liquid chromatography, measures, and obtains.
Fig. 1 is shown in by the HPLC collection of illustrative plates of reference substance, and Fig. 2-5 are shown in respectively by the HPLC collection of illustrative plates of embodiment 1 and comparative example 1-3.
Measurement result is in Table 2.
Table 2 paeoniflorin content measurement result
Group |
Embodiment 1 |
Comparative example 1 |
Comparative example 2 |
Comparative example 3 |
Paeoniflorin content (mg/8g) |
31.26 |
25.37 |
30.02 |
25.78 |
Conclusion: adopt preparation method of the present invention, in the Chinese medicine composition making, the content of peoniflorin obviously improves.The Radix Paeoniae Alba is the monarch drug in prescription, and the raising of effective component of paeonia lactiflora content in preparation will strengthen the flat drug effect of root pain.
experimental example 3the impact of Chinese medicine composition of the present invention on the experiment of cervical spondylosis of vertebral artery rabbit thrombosis
1. given the test agent
The root that embodiment 1 prepares is flat granule bitterly, is mixed with the solution of 486mg/ml with distilled water
2. reference substance
The pharmaceutical composition that comparative example 1~3 prepares, is mixed with the solution of 486mg/ml with distilled water
3. test method
Get totally 48 of the large ear white rabbit of New Zealand, weight 2.5kg~3.0kg, male and female dual-purpose, be divided at random 6 groups, be labeled as respectively test group (the flat granule of root pain that embodiment 1 prepares, 2.4g/kg, being equivalent to crude drug amount is 2.88g), contrast 1 group of (pharmaceutical composition that comparative example 1 prepares, it is 2.88g that 2.4g/kg is equivalent to crude drug amount), 2 groups of (pharmaceutical compositions that comparative example 2 prepares of comparative example, it is 2.88g that 2.4g/kg is equivalent to crude drug amount), 3 groups of (pharmaceutical compositions that comparative example 3 prepares of comparative example, it is 2.88g that 2.4g/kg is equivalent to crude drug amount), model group and blank group, every group each 8.Except blank group, remaining animal feeding is after 1 week, with abdomen position, be fixed in laboratory table, its cervical region is stretched, cut off rabbit left side cervical region hair, exposed area is 2 * 2cm skin approximately, with iodine disinfection pelt place, to get sclerosing agent XIAOZHILING ZHUSHEYE 10ml (0.04g/mL) and inject in c3~c5 transverse process of cervical vertebra side, rabbit left side, the duplicate injection time is the 2nd week and the 4th week, make rabbit vertebral artery form aseptic inflammation and scar tissue around, with this, cause the model of vertebral artery pressurized.Before choosing respectively arranged on left and right sides tremulous pulse flow velocity and basilar artery flow velocity and modeling, corresponding velocity ratio, if be less than 10cm/s person, is considered as modeling success.After modeling success, start administration.Test group gives 2.4g/kg with 1~3 group of contrast, and model group gives equal-volume normal saline, disregards for blank group.Successive administration 28 days, after last administration 24 hours, by carotid artery, get blood, carry out the mensuration that hemorheology is relevant.
Index detects: get whole blood 1ml Implanted Silicon sebific duct, cyclization after eliminating bubble, put into after external thrombus instrument, start instrument, after 15min, take out silica gel tube, by vernier caliper measurement thrombosis length, electronic balance weighing wet weight of thrombus, thrombosis is put in 60 ℃ of people's drying baker, after 15min, taken out, weigh the dry weight of thrombosis.The results are shown in Table 3.
The impact of the flat granule of table 3 pain on the experiment of cervical spondylosis of vertebral artery rabbit thrombosis
Note: with model group comparison, * P<0.05, * * P<0.01; With the comparison of blank group,
▲ ▲p<0.01.
Result:
(1) with the comparison of blank group, thrombosis length, wet weight of thrombus and the dry weight of model group all extremely significantly increases, and modeling success is described.
(2) with model group comparison, thrombosis length, wet weight of thrombus and the dry weight of test group and each contrast groups all significantly or extremely significantly reduces (P<0.05, P<0.01), wherein the decline of every detection index of test group is more obvious.The big or small sequence of each group effect is: test group > contrasts 3 groups of > and contrasts 2 groups of > and contrast 1 group.
Conclusion:
Patients with Cervical Spondylopathy blood is in high viscous state, thereby causes microcirculation dysfunction.This experiment is by measuring relatively administration Rabbits Before And After model thrombosis, shown that the flat granule of root pain that preparation method of the present invention prepares is better than compositions prepared by prior art in the effect improving aspect microcirculation disturbance.The improvement of preparation method is described, has improved the flat pharmacological action of root pain.
experimental example 4: analgesic activity is investigated.
1. given the test agent
The root that embodiment 1 prepares is flat granule bitterly, is mixed with the solution of 720mg/ml with distilled water
2. reference substance
The pharmaceutical composition that comparative example 1~3 prepares, is mixed with the solution of 720mg/ml with distilled water
3. test method
Test method 1: get 60 of healthy male mices, be divided at random 5 groups: test group (the flat granule of root pain that embodiment 1 prepares, 3.24g/kg, be equivalent to crude drug 3.89g), contrast 1 group of (pharmaceutical composition that comparative example 1 prepares, 3.24g/kg, be equivalent to crude drug 3.89g), 2 groups of (pharmaceutical compositions that comparative example 2 prepares of comparative example, 3.24g/kg, be equivalent to crude drug 3.89g), 3 groups of (pharmaceutical compositions that comparative example 3 prepares of comparative example, 3.24g/kg, be equivalent to crude drug 3.89g) and normal saline group (1.0ml/ only), gastric infusion, every day 1 time, successive administration 3d.After last 1 administration 1h, each ip in mice 0.9% glacial acetic acid solution 0.1mL10g
-1, then observe writhing response in mice 20min, and record the writhing number of times of mice.The results are shown in Table 4.
The impact of the flat granule of table 4 pain on glacial acetic acid induced mice writhing response
Note: *: compare P<0.05 with normal saline group,
▲ ▲: compare P<0.05 with 1 group of contrast,
▲ ▲ ▲: compare p<0.01 with 1 group of contrast.
Result:
1), with the comparison of normal saline group, test group and each contrast groups can reduce mouse writhing number of times in 20min.1 group of comparison of test group and contrast, has utmost point significant difference (P<0.01).
2) the tested medicine process that contrasts 3 groups detects, and also contain volatile oil, but its analgesic effect is weaker than test group: 1 group of comparison of test group and contrast, has utmost point significant difference (P<0.01); Contrast 3 groups and 1 group of comparison of contrast, there is significant difference (P<0.05).
Conclusion:
Although the Chinese medicine composition of preparing with art methods and the method for the invention has analgesic activity.But the analgesic activity of the flat granule of root prepared by the method for the invention pain is obviously better than compositions prepared by art methods, be also better than the pharmaceutical composition that simple improvement Olibanum, Myrrha extracting method obtain.The enhancing that the tested medicine analgesic effect of test group is described is not to be derived from merely volatile oil, but the improvement of each extraction step of the present invention and the synthesis result of optimization.
In a word, by above-mentioned pharmacological evaluation, prove, root prepared by preparation method of the present invention is bitterly flat, in the effect that improves microcirculation, ease pain, is obviously better than existing preparation.Illustrate that preparation method of the present invention significantly strengthens the flat pharmacological action of root pain.
Specific description of embodiments of the present invention above does not limit the present invention, and those skilled in the art can make according to the present invention various changes or distortion, only otherwise depart from spirit of the present invention, all should belong to the scope of claims of the present invention.