CN103006972A - Tongjingning granule and preparation thereof - Google Patents
Tongjingning granule and preparation thereof Download PDFInfo
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- CN103006972A CN103006972A CN2012105907730A CN201210590773A CN103006972A CN 103006972 A CN103006972 A CN 103006972A CN 2012105907730 A CN2012105907730 A CN 2012105907730A CN 201210590773 A CN201210590773 A CN 201210590773A CN 103006972 A CN103006972 A CN 103006972A
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Abstract
The invention relates to a Tongjingning granule and preparation thereof. The preparation disclosed by the invention adopts new processes, namely 80% ethanol reflux extraction and decompression and concentration extraction, and furthest retains and increases the effective components of drugs. The prepared product is stable in property and solves the problems of easiness for breakage and deliquescence, softening spoilage, inapplicability of long-time preservation, and the like of a sugary granule by taking sodium carboxymethylcellulose as an adhesive. Besides, the amount of extracts is reduced so that the single-dose packaging weight of a drug is greatly reduced, and therefore the drug is more conveniently taken and carried. The Tongjingning granule disclosed by the invention has the advantages of good treatment effect, little side effect, quick effect, good mouthfeel, long drug quality guarantee period, low cost, simpler preparation process, drug preparation time conservation, and the like.
Description
Technical field
The invention belongs to the Chinese materia medica field, be specifically related to Chinese medicine granules of a kind of menstruction regulating and pain relieving and preparation method thereof.
Background technology
Dysmenorrhea rather is a kind of by Radix Angelicae Sinensis (wine stir-fry) 333g, Rhizoma Cyperi (vinegar system) 333g, the Radix Paeoniae Alba (stir-fry) 333g, Radix Salviae Miltiorrhizae 333g, Rhizoma Corydalis (vinegar system) 300g, Fructus Toosendan (stir-fry), Rhizoma Chuanxiong (stir-fry) 200g, Radix Glycyrrhizae Preparata 133g, the Chinese patent medicine preparation of Flos Carthami 167g preparation, be used for menstruction regulating and pain relieving, be used for menoxenia, suffer from abdominal pain through front, menstrual period.Listing granule and capsule arranged.
Although 'Tongjingning ' has gone on the market for many years, the patient is dissatisfied to its effect, the 'Tongjingning ' of selling in the market, what use is traditional extraction process by water, improves the step that has added precipitate with ethanol although have afterwards, and still there is the defective of traditional Chinese patent medicine in it, after being length standing time, the granule moisture absorption is gone mouldy, preparation colour-darkening etc., simultaneously, because use extraction process by water, bioavailability is not high, dose is large.
The present invention develops a kind of new granular preparation for dysmenorrhea by to the improvement of extraction process and the improvement of preparation process, and its drug content is improved, Packing Unit reduces, and stability improves, and takes more convenient, mouthfeel is better, and drug effect and bioavailability improve greatly, obtains beyond thought effect.
Summary of the invention
The object of the present invention is to provide a kind of Chinese medicine granules of menstruction regulating and pain relieving.
Chinese medicinal granule of the present invention is prepared from by following raw material of Chinese medicine and the processing of medicine acceptable carrier:
Radix Angelicae Sinensis (wine stir-fry) 333g, Rhizoma Cyperi (vinegar system) 333g, the Radix Paeoniae Alba (stir-fry) 333g, Radix Salviae Miltiorrhizae 333g, Rhizoma Corydalis (vinegar system) 300g, Fructus Toosendan (stir-fry), Rhizoma Chuanxiong (wine stir-fry) 200g, Radix Glycyrrhizae Preparata 133g, Flos Carthami 167g are crude drug, form in order to the below legal system is standby:
Medical material adds 8-10 and doubly measures 80% alcohol reflux 2 times, and each 1-2 hour, merge extractive liquid,, Recycled ethanol obtains thick paste shape product, adds cross-linking sodium carboxymethyl cellulose 10g and binding agent and correctives, mixes, granulate, drying, and get final product.
In the above composition, the weight of medicine is calculated with crude drug, with weight as proportioning, when producing, can proportionally increase or reduce, can be take kilogram as unit such as large-scale production, or take ton as unit, small-scale production also can be in grams, weight can increase or reduce, but the constant rate of the raw medicinal herbs weight proportion between each composition.
The ratio of above weight proportion obtains through science screening, for especial patient, and such as serious symptom or light disease, fat or modest patient, the proportioning of the amount that can corresponding adjustment forms increases or reduces being no more than 100%, and drug effect is constant.
Above composition can be made granule 500-1000 grams of the present invention.
Preferably, Chinese medicinal granule of the present invention is prepared from by following raw material of Chinese medicine and the processing of medicine acceptable carrier:
Get Radix Angelicae Sinensis (wine stir-fry) 333g, Rhizoma Cyperi (vinegar system) 333g, the Radix Paeoniae Alba (stir-fry) 333g, Radix Salviae Miltiorrhizae 333g, Rhizoma Corydalis (vinegar system) 300g, Fructus Toosendan (stir-fry), Rhizoma Chuanxiong (wine stir-fry) 200g, Radix Glycyrrhizae Preparata 133g, Flos Carthami 167g is with 80% alcohol reflux 2 times, for the first time add 10 times of amounts, reflux, extract, 2 hours is filtered, medicinal residues add 8 times of amounts for the second time, and reflux, extract, 1 hour is filtered, merging filtrate, decompression recycling ethanol is to distinguishing the flavor of without alcohol, and merge extractive liquid, filters, filtrate is concentrated into 60 ℃, and to survey density be 1.15-1.20 thick paste shape, add cross-linking sodium carboxymethyl cellulose 10g and binding agent and correctives, mix, granulate, drying, and get final product.
Wherein, described binding agent includes but not limited to starch, pregelatinized Starch, dextrin, maltodextrin, polyvinylpyrrolidone, cross-linking sodium carboxymethyl cellulose.
Wherein, described correctives includes but not limited to sucrose, mannitol, xylitol, stevioside, lactose, fructose, protein sugar, maltose alcohol, aspartame, flavoring banana essence, flavoring pineapple essence, vanillin, fragrant citrus essence, Mint Essence, citric acid, can use separately, also use capable of being combined.
Special character of the present invention is existing extraction process is improved, and changes decocting in water or water boiling and precipitation with ethanol technique into 80% ethanol extraction.
The non-medicinal ingredient that extraction process by water extracts is more, and extraction process by water medicament contg diversity is large and hygroscopicity is large, disturbs simultaneously the detection of drug standard, can not accurately control drug quality, and technique is unstable simultaneously; Although water boiling and precipitation with ethanol technique corrects to some extent to extraction process by water, its loss of effective components is large, and the curative effect of product is had certain impact, and some defectives such as the non-medicinal ingredient that can't overcome in the extraction process by water simultaneously are many, and hygroscopicity is large etc.
The present invention is through research, according to the characteristic of medicine and the screening of extracting method, select 80% ethanol extraction, active constituent content is improved greatly, content such as peoniflorin increases more than 50%, and tetrahydropalmatine, the content of ligustrazine and TANSHINONES also improve greatly, the active constituent content diversity is little, and technology stability is good.
Granule of the present invention, owing to using alcohol extraction process, be difficult to bonding after its extractum is pulverized, unstable behind the particle drying of preparing, frangible, after packed products length standing time, powder increases, so the present invention has selected cross-linking sodium carboxymethyl cellulose as filler through screening, and then add an amount of binding agent and correctives, the present invention has improved the stability of medicine by the adding of cross-linking sodium carboxymethyl cellulose composition, has avoided the frangible of granules of sugar agent, easy deliquescence, softening rotten, the unsuitable problems such as deficiency stored for a long time, in addition, owing to having reduced the amount of extract, therefore the unit dose package quality of medicine greatly reduces, and makes drug administration, carry all more convenient.
In addition, it is good that the present invention also has a therapeutic effect, few side effects, and instant effect, mouthfeel is good, and the quality guarantee period of medicament phase is long, and cost is low, and preparation technology is simpler, has saved the plurality of advantages such as time of preparation medicine.
Further specify beneficial effect of the present invention by following experimental data:
(1) Study on extraction
1. process route:
Route 1. water extraction:
Radix Angelicae Sinensis, the Radix Paeoniae Alba, Rhizoma Cyperi, Radix Salviae Miltiorrhizae, Rhizoma Corydalis, Fructus Toosendan, Rhizoma Chuanxiong, Radix Glycyrrhizae are required to concoct into Radix Angelicae Sinensis (wine stir-fry), the Radix Paeoniae Alba (wine stir-fry), Rhizoma Corydalis (vinegar system), Fructus Toosendan (stir-fry), Rhizoma Chuanxiong (wine stir-fry), Radix Glycyrrhizae (processing), salvia piece according to concocted specification respectively, and Flos Carthami in addition 8-10 times of water gaging soak after 4 hours, heating heats up, be heated to nearly boiling, temperature is controlled at about 95-100 ℃, time 2 h, collect extracting solution, it is the same that other adds water continuation heating decoction temperature, time 2 h.2 decoction liquor merge, and thin film concentration decocting liquid adds dextrin, sucrose, cross-linking sodium carboxymethyl cellulose at last to rare flowing soaking paste, stir and granulate, and dry below 60 ℃, granulate gets product.
Route 2. water boiling and precipitation with ethanols extract:
Radix Angelicae Sinensis, the Radix Paeoniae Alba, Rhizoma Cyperi, Radix Salviae Miltiorrhizae, Rhizoma Corydalis, Fructus Toosendan, Rhizoma Chuanxiong, Radix Glycyrrhizae are required to concoct into Radix Angelicae Sinensis (wine stir-fry), the Radix Paeoniae Alba (wine stir-fry), Rhizoma Corydalis (vinegar system), Fructus Toosendan (stir-fry), Rhizoma Chuanxiong (wine stir-fry), Radix Glycyrrhizae (processing), salvia piece according to concocted specification respectively, and Flos Carthami in addition 8-10 times of water gaging soak after 4 hours, heating heats up, be heated to nearly boiling, temperature is controlled at about 95-100 ℃, time 2 h, collect extracting solution, other adds water and continues the heating decoction, temperature is the same, time 2 h.2 times decoction liquor merges, and the condensed water decocting liquid is doubly measured 2-3 95% ethanol again and added to rare flowing soaking paste, stirs, is diluted to evenly, leaves standstill 24 hours, makes precipitation fully, gets supernatant, is evaporated to flowing soaking paste, makes cooling.Add dextrin, sucrose, cross-linking sodium carboxymethyl cellulose, stir and granulate, dry below 60 ℃, granulate gets product.
Route 3 methanol extraction:
With Radix Angelicae Sinensis, the Radix Paeoniae Alba, Rhizoma Cyperi, Radix Salviae Miltiorrhizae, Rhizoma Corydalis, Fructus Toosendan, Rhizoma Chuanxiong, Radix Glycyrrhizae respectively according to concocted specification require to concoct into Radix Angelicae Sinensis (wine stir-frys), the Radix Paeoniae Alba (wine stir-frys), Rhizoma Corydalis (vinegar system), Fructus Toosendan (stir-frys), Rhizoma Chuanxiong (wine stir-fry), Radix Glycyrrhizae (processing), salvia piece, reach Flos Carthami in addition 10 times measure the methanol immersion after 4 ~ 8 hours, heating and refluxing extraction 2 times, each time 2 h.2 times extracting solution merges, and leaves standstill 24 hours, makes precipitation fully, gets supernatant, is concentrated into flowing soaking paste, makes cooling.Add at last dextrin, sucrose, cross-linking sodium carboxymethyl cellulose, stir and granulate, dry below 60 ℃, granulate gets product.
Route 4. 95% ethanol extractions
With Radix Angelicae Sinensis, the Radix Paeoniae Alba, Rhizoma Cyperi, Radix Salviae Miltiorrhizae, Rhizoma Corydalis, Fructus Toosendan, Rhizoma Chuanxiong, Radix Glycyrrhizae respectively according to concocted specification require to concoct into Radix Angelicae Sinensis (wine stir-frys), the Radix Paeoniae Alba (wine stir-frys), Rhizoma Corydalis (vinegar system), Fructus Toosendan (stir-fry), Rhizoma Chuanxiong (wine stir-fry), Radix Glycyrrhizae (processing), salvia piece, reach Flos Carthami in addition 10 times measure 95% soak with ethanol after 4 ~ 8 hours, heating and refluxing extraction, collect extracting solution, time 2 h, residue adds 95% ethanol to be continued to extract time 2 h.2 times extracting solution merges, and leaves standstill 24 hours, makes precipitation fully, gets supernatant, is concentrated into flowing soaking paste, makes cooling.Add at last dextrin, sucrose, cross-linking sodium carboxymethyl cellulose, stir and granulate, dry below 60 ℃, granulate gets product.
Route 5. 80% ethanol extractions
With Radix Angelicae Sinensis, the Radix Paeoniae Alba, Rhizoma Cyperi, Radix Salviae Miltiorrhizae, Rhizoma Corydalis, Fructus Toosendan, Rhizoma Chuanxiong, Radix Glycyrrhizae respectively according to concocted specification require to concoct into Radix Angelicae Sinensis (wine stir-frys), the Radix Paeoniae Alba (wine stir-frys), Rhizoma Corydalis (vinegar system), Fructus Toosendan (stir-fry), Rhizoma Chuanxiong (wine stir-fry), Radix Glycyrrhizae (processing), salvia piece, reach Flos Carthami in addition 10 times measure 80% soak with ethanol after 4 ~ 8 hours, heating and refluxing extraction, collect extracting solution, time 2 h, residue adds 8 times of amount 80% ethanol to be continued to extract 1 hour time.2 times extracting solution merges, and leaves standstill 24 hours, makes precipitation fully, gets supernatant, is concentrated into flowing soaking paste, makes cooling.Add at last dextrin, sucrose, cross-linking sodium carboxymethyl cellulose, stir and granulate, dry below 60 ℃, granulate gets product.
Route 6. 65% ethanol extractions
With Radix Angelicae Sinensis, the Radix Paeoniae Alba, Rhizoma Cyperi, Radix Salviae Miltiorrhizae, Rhizoma Corydalis, Fructus Toosendan, Rhizoma Chuanxiong, Radix Glycyrrhizae respectively according to concocted specification require to concoct into Radix Angelicae Sinensis (wine stir-frys), the Radix Paeoniae Alba (wine stir-frys), Rhizoma Corydalis (vinegar system), Fructus Toosendan (stir-fry), Rhizoma Chuanxiong (wine stir-fry), Radix Glycyrrhizae (processing), salvia piece, reach Flos Carthami in addition 10 times measure 65% soak with ethanol after 4 ~ 8 hours, heating and refluxing extraction, collect extracting solution, time 2 h, other adds 65% ethanol and continues to extract time 2 h.2 times extracting solution merges, and leaves standstill 24 hours, makes precipitation fully, gets supernatant, is concentrated into flowing soaking paste, makes cooling.Add at last dextrin, sucrose, cross-linking sodium carboxymethyl cellulose, stir and granulate, dry below 60 ℃, granulate gets product.
2. preparation method:
Take by weighing respectively Radix Angelicae Sinensis (wine stir-fry) 333g by the prescription usage ratio, Rhizoma Cyperi (vinegar system) 333g, the Radix Paeoniae Alba (stir-fry) 333g, Radix Salviae Miltiorrhizae 333g, Rhizoma Corydalis (vinegar system) 300g, Fructus Toosendan (stir-fry) 300g, Rhizoma Chuanxiong (wine stir-fry) 200g, Radix Glycyrrhizae Preparata 133g, Flos Carthami 167g, totally 6 parts, extract with above-mentioned six kinds of routes respectively and obtain dry extract.
The above-mentioned 1-6 dry extract sample for preparing carries out the assay of effective ingredient as test sample.
3. measure the active constituent content of each sample:
Paeoniflorin content
Wherein the assay method of peoniflorin is as follows:
Measure according to high performance liquid chromatography (2010 editions one appendix VI D of Chinese Pharmacopoeia).
Chromatographic condition and system suitability: Waters600 controller high performance liquid chromatograph Agilent 4.6*150mm 5 μ m octadecylsilane chemically bonded silicas are filler; Methanol-0.05% biphosphate first solution (regulating pH value to 360.1 with phosphoric acid) is mobile phase (35:65); Detecting wavelength is that the 230nm. number of theoretical plate should be not less than 2500. by the peoniflorin peak.
The preparation of reference substance solution: 36 hours the peoniflorin reference substance of phosphorus pentoxide drying under reduced pressure of learning from else's experience is an amount of, accurately weighed, adds methanol and makes the solution that every 1ml contains 0.1mg, and get final product.
The preparation of need testing solution: get extract granule, porphyrize is got 0.4g accurately weighed, puts in the tool plug Erlenmeyer flask, the accurate Diluted Alcohol 20ml that adds shakes up, and weighs, and places 12 hours, supply the weight of minimizing with Diluted Alcohol, filter with microporous filter membrane (0.45 μ m), get subsequent filtrate, and get final product.
Algoscopy: precision is drawn reference substance solution and each 10ul of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
Content determination of dl-tetrahydropalmatine
| Sample 1 | Sample 2 | Sample 3 | Sample 4 | Sample 5 | Sample 6 |
| 17.15μg/g | 19.24 | 23.36 | 20.13 | 25.21 | 18.26 |
The assay method of tetrahydropalmatine is as follows:
Instrument and reagent:
High performance liquid chromatograph (Waters 600cntroller); C18 ODS2 chromatographic column (4.6*250mm, 20 μ m) is measured.
Chromatographic condition and system suitability: be filler with octadecylsilane chemically bonded silica; Methanol-0.1% phosphoric acid solution (regulating pH value to 6.0 with triethylamine) is mobile phase (55:45); Flow velocity 1.0ml/min, the detection wavelength is 280nm, number of theoretical plate calculates by the tetrahydropalmatine peak should be not less than 3000..
The preparation of reference substance solution: precision takes by weighing through the tetrahydropalmatine reference substance an amount of, and is accurately weighed, adds methanol and makes the solution that every 1ml contains 46 μ g, and get final product.
The preparation of need testing solution: get this product extract granule, porphyrize is got 0.50g accurately weighed, in the flask, accurate dense ammonia methanol (1:20) the mixed solution 50ml that adds shakes up at the bottom of the horizontalization, weigh, 1 hour post-heating of merceration refluxed 1 hour, let cool, more weighed weight, supply the weight of minimizing with strong ammonia solution methanol (1:20) mixed solution, shake up, filter, the accurate subsequent filtrate 25ml that draws, put evaporate to dryness in the water-bath, residue adds dissolve with methanol, is transferred in the 5ml measuring bottle, and is diluted to scale, shake up, filter, get subsequent filtrate, and get final product.
Algoscopy: accurately draw each 10.0 μ l of above-mentioned reference substance solution and need testing solution, the injection liquid chromatography is measured peak area value, and be get final product.
Ligustrazine content
| Sample 1 | Sample 2 | Sample 3 | Sample 4 | Sample 5 | Sample 6 |
| 39.21μg/g | 40.25 | 42.54 | 42.36 | 63.71 | 51.43 |
Ferulaic acid content
| Sample 1 | Sample 2 | Sample 3 | Sample 4 | Sample 5 | Sample 6 |
| 23.63μg/g | 25.05 | 70.21 | 69.28 | 76.42 | 53.31 |
The assay method of ligustrazine and ferulic acid is as follows:
High performance liquid chromatograph Agilent 2 series
Chromatographic condition adopts Kromasil C8 (4.6mm*200mm, 5 μ m) chromatographic column; Mobile phase: methanol-0.1% phosphoric acid=40:60, solution; Flow velocity: 1.0ml/min detects 30 ℃ of wavelength 294nm. column temperatures, sample size 10 μ l.
The preparation of reference substance solution: precision takes by weighing ligustrazine and the ferulic acid reference substance is an amount of, uses respectively the chromatograph methanol constant volume to 50ml, and supersound process 10min namely gets ligustrazine and ferulic acid reference substance solution.
The preparation of need testing solution: with the extract granule porphyrize, the 95% ethanol water-bath reflux, extract, 1 hour that adds 1 times of amount, filter, filtrate is concentrated into extractum, be transferred in the evaporating dish, to the vacuum drying oven below 60 ℃ dry 24 hours, get dry after extract powder an amount of, put in the 50ml beaker, add 30ml chromatograph methanol to dissolving, leave standstill, pipet pipettes 3.00ml filtrate, places the 10ml measuring bottle, the accurate chromatograph methanol solution that adds is to scale, shake up, through 0.45 μ m filtering with microporous membrane, namely get sample solution again.
Algoscopy: precision is drawn reference substance solution and each 10 μ l of need testing solution respectively, and the injection liquid chromatography is measured, and be get final product.
TANSHINONES content
| Sample 1 | Sample 2 | Sample 3 | Sample 4 | Sample 5 | Sample 6 |
| 0.164mg/g | 0.183 | 0.203 | 0.196 | 0.241 | 0.192 |
The assay method of TANSHINONES is as follows:
Adopt ultraviolet spectrophotometry
Reagent tanshinone ⅡA reference substance, extractum.
The preparation of reference substance solution: it is an amount of that precision takes by weighing the tanshinone ⅡA reference substance, and chlorination is copied into the solution that every ml contains 0.108mg;
The preparation of need testing solution: 1. get the extract granule porphyrize, get approximately 0.2g powder, accurately weighed, add the 50ml chloroform, supersound process 15min lets cool, and filters evaporate to dryness;
2. residue adds NaOH solution (pH10) 40ml dissolving, filters evaporate to dryness;
3. residue adds acetone solution, filters the filtrate evaporate to dryness.Residue dissolves with chloroform, filters, and is settled to 25ml with chloroform and shakes up.
Algoscopy: measure trap at 268nm wavelength place with ultraviolet spectrophotometry, according to the content of total tanshinone in the standard curve calculation sample.
4. measure the hygroscopicity of each sample:
Each sample was placed 10 days in room temperature in the environment of relative humidity 75%, measured wherein moisture, and assay method adopts boulton process, and moisture is as follows in each sample:
| Sample 1 | Sample 2 | Sample 3 | Sample 4 | Sample 5 | Sample 6 |
| 16.3% | 15.2% | 11.2% | 8.9% | 8.4% | 9.2% |
5. measure the stability of peoniflorin in each sample:
Each sample was placed 90 days in the 40C incubator, measured the content of peoniflorin wherein, and assay method is the same, and the result is as follows:
The result: from every testing results such as above assays, adopt the extract active constituent content of 80% ethanol extraction of the present invention the highest, hygroscopicity (lacking) is best, and stability is the highest.(the methanol extraction method is got rid of because of the toxicity reason, does not consider)
The preparations shaping Journal of Sex Research
1. the screening of correctives
For regulating the mouthfeel of granule of the present invention, selected at first respectively sucrose, aspartame, stevioside to make respectively 5%, 10%, 15%, 0.3%, 0.1% compares as correctives, and the result shows: 15% cane-sugar taste is better than 0.3% aspartame and 0.1% stevioside.
2. the screening of correctives consumption
Select sucrose to be made into respectively variable concentrations and compare, the results are shown in Table
The screening comparative result of correctives
Annotate :+expression is better, ++ represent, +++expression is fine
By the result as seen, select sucrose both can improve the taste of granule, and appearance character do not change, and with
Sugariness was best when sucrose was 10-15%, passed through mouthfeel comparison and cost calculation again, determined that finally dosage of sucrose is 10% in the granule.
3. the selection of filler
Granule is fine particle, requires particle stabilizedly, soluble, in order to guarantee the quality of preparation, needs to add filler.
4. kind, the consumption of filler are carried out analysis-by-synthesis.
Filler is selected: pregelatinized Starch, dextrin, microcrystalline Cellulose, Polyethylene Glycol, hydroxypropyl methylcellulose, cross-linking sodium carboxymethyl cellulose.
As active constituents of medicine, above filler and dextrin and sucrose mix as auxiliary element, granulate with extract of the present invention, and drying gets granule.
The filler screening test relatively
Result of the test shows: use the effect of cross-linking sodium carboxymethyl cellulose better
The specific embodiment
The invention will be further described by following specific embodiment, but not as limitation of the present invention.
Embodiment 1 granule
Get Radix Angelicae Sinensis (wine stir-fry) 333g, Rhizoma Cyperi (vinegar system) the 333g Radix Paeoniae Alba (wine stir-fry) 333g, Rhizoma Corydalis (vinegar system) 300g, Fructus Toosendan (stir-fry) 300g, Rhizoma Chuanxiong (wine stir-fry) 200g, Radix Glycyrrhizae (processing) 133g, Radix Salviae Miltiorrhizae 333g, and Flos Carthami 167g 10 times of amount 80% soak with ethanol in addition, heating and refluxing extraction 2 hours, collect extracting solution, filter, medicinal residues add in addition 8 times of amount 80% ethanol and continue reflux, extract,, 1 hour time.2 times extracting solution merges, and leaves standstill 24 hours, makes precipitation fully, gets supernatant, is concentrated into flowing soaking paste (60 ℃ of lower densities are 1.15_1.20), makes cooling.Add at last dextrin 250g, sucrose 100g, cross-linking sodium carboxymethyl cellulose 10g, stir and granulate, dry below 60 ℃, granulate gets product.
Embodiment 2 granules
Get Radix Angelicae Sinensis (wine stir-fry) 333g, Rhizoma Cyperi (vinegar system) the 333g Radix Paeoniae Alba (wine stir-fry) 333g, Rhizoma Corydalis (vinegar system)
300g, Fructus Toosendan (stir-fry) 300g, Rhizoma Chuanxiong (wine stir-fry) 200g, Radix Glycyrrhizae (processing) 133g, Radix Salviae Miltiorrhizae 333g, and Flos Carthami 167g 10 times of amount 80% soak with ethanol in addition, heating and refluxing extraction 2 hours is collected extracting solution, filters, medicinal residues add in addition 8 times of amount 80% ethanol and continue reflux, extract,, 1 hour time.2 times extracting solution merges, and leaves standstill 24 hours, makes precipitation fully, gets supernatant, is concentrated into flowing soaking paste (60 ℃ of lower densities are 1.15_1.20), makes cooling.Add at last dextrin 150g, steviosin 1.5g, cross-linking sodium carboxymethyl cellulose 10g, stir and granulate, dry below 60 ℃, granulate gets product.(being sugarless products)
Embodiment 3 granules
Get Radix Angelicae Sinensis (wine stir-fry) 333g, Rhizoma Cyperi (vinegar system) the 333g Radix Paeoniae Alba (wine stir-fry) 333g, Rhizoma Corydalis (vinegar system) 300g, Fructus Toosendan (stir-fry) 300g, Rhizoma Chuanxiong (stir-fry) 200g, Radix Glycyrrhizae (processing) 133g, Radix Salviae Miltiorrhizae 333g, and Flos Carthami 167g 10 times of amount 80% soak with ethanol in addition, heating and refluxing extraction 2 hours, collect extracting solution, filter, medicinal residues add in addition 8 times of amount 80% ethanol and continue reflux, extract,, 1 hour time.2 times extracting solution merges, and leaves standstill 24 hours, makes precipitation fully, gets supernatant, is concentrated into flowing soaking paste (60 ℃ of lower densities are 1.15_1.20), makes cooling.Add at last pregelatinized Starch 20g, aspartame 2.5g, cross-linking sodium carboxymethyl cellulose 20g, stir and granulate, dry below 60 ℃, granulate gets product.(being sugarless products)
Embodiment 4 granules
Get Radix Angelicae Sinensis (wine stir-fry) 333g, Rhizoma Cyperi (vinegar system) the 333g Radix Paeoniae Alba (wine stir-fry) 333g, Rhizoma Corydalis (vinegar system) 300g, Fructus Toosendan (stir-fry) 300g, Rhizoma Chuanxiong (stir-fry) 200g, Radix Glycyrrhizae (processing) 133g, Radix Salviae Miltiorrhizae 333g, and Flos Carthami 167g 10 times of amount 80% soak with ethanol in addition, heating and refluxing extraction 2 hours, collect extracting solution, filter, medicinal residues add in addition 8 times of amount 80% ethanol and continue reflux, extract,, 1 hour time.2 times extracting solution merges, and leaves standstill 24 hours, makes precipitation fully, gets supernatant, is concentrated into flowing soaking paste (60 ℃ of lower densities are 1.15_1.20), makes cooling.Add at last dextrin 150g, sucrose 100g, hydroxypropyl methylcellulose 50g, cross-linking sodium carboxymethyl cellulose 5g stirs and granulates, and dry below 60 ℃, granulate gets product.
Embodiment 5 granules
Get Radix Angelicae Sinensis (wine stir-fry) 333g, Rhizoma Cyperi (vinegar system) the 333g Radix Paeoniae Alba (wine stir-fry) 333g, Rhizoma Corydalis (vinegar system)
300g, Fructus Toosendan (stir-fry) 300g, Rhizoma Chuanxiong (stir-fry) 200g, Radix Glycyrrhizae (processing) 133g, Radix Salviae Miltiorrhizae 333g, and Flos Carthami 167g 10 times of amount 80% soak with ethanol in addition, heating and refluxing extraction 2 hours is collected extracting solution, filters, medicinal residues add in addition 8 times of amount 80% ethanol and continue reflux, extract,, 1 hour time.2 times extracting solution merges, and leaves standstill 24 hours, makes precipitation fully, gets supernatant, is concentrated into flowing soaking paste (60 ℃ of lower densities are 1.15_1.20), makes cooling.Add at last pregelatinized Starch 25g, dextrin 100g, sucrose 100g, hydroxypropyl methylcellulose 10g, cross-linking sodium carboxymethyl cellulose 10g stirs and granulates, and dry below 60 ℃, granulate gets product.
Embodiment 6 granules
Get Radix Angelicae Sinensis (wine stir-fry) 333g, Rhizoma Cyperi (vinegar system) the 333g Radix Paeoniae Alba (wine stir-fry) 333g, Rhizoma Corydalis (vinegar system) 300g, Fructus Toosendan (stir-fry) 300g, Rhizoma Chuanxiong (wine stir-fry) 200g, Radix Glycyrrhizae (processing) 133g, Radix Salviae Miltiorrhizae 333g, and Flos Carthami 167g 10 times of amount 80% soak with ethanol in addition, heating and refluxing extraction 2 hours, collect extracting solution, filter, medicinal residues add in addition 8 times of amount 80% ethanol and continue reflux, extract,, 1 hour time.2 times extracting solution merges, and leaves standstill 24 hours, makes precipitation fully, gets supernatant, is concentrated into flowing soaking paste (60 ℃ of lower densities are 1.15_1.20), makes cooling.Add at last dextrin 120g, aspartame 2.5g, cross-linking sodium carboxymethyl cellulose 20g, stir and granulate, dry below 60 ℃, granulate, (for sugarless products) gets product.
Claims (6)
1. granular preparation for dysmenorrhea, described granule is by Radix Angelicae Sinensis (wine stir-fry) 333g, Rhizoma Cyperi (vinegar system) 333g, the Radix Paeoniae Alba (stir-fry) 333g, Radix Salviae Miltiorrhizae 333g, Rhizoma Corydalis (vinegar system) 300g, Fructus Toosendan (stir-fry), Rhizoma Chuanxiong (wine stir-fry) 200g, Radix Glycyrrhizae Preparata 133g, Flos Carthami 167g is crude drug, forms in order to the below legal system is standby:
Medical material adds 80% alcohol reflux 2 times that 8-10 doubly measures, and each 1-2 hour, merge extractive liquid,, Recycled ethanol gets thick paste shape product, adds cross-linking sodium carboxymethyl cellulose 10g, and binding agent and correctives, mixes, granulate, drying, and get final product.
2. the described granular preparation for dysmenorrhea of claim 1 is characterized in that, binding agent includes but not limited to starch, pregelatinized Starch, dextrin, maltodextrin, polyvinylpyrrolidone.
3. the described granular preparation for dysmenorrhea of claim 1, it is characterized in that, correctives includes but not limited to sucrose, mannitol, xylitol, stevioside, lactose, fructose, protein sugar, maltose alcohol, aspartame, flavoring banana essence, flavoring pineapple essence, vanillin, fragrant citrus essence, Mint Essence, citric acid, can use separately, or be used in combination.
4. the described granular preparation for dysmenorrhea of claim 1 can according to clinical needs, use control correctives addition to make sugar product or sugarless products.
5. the preparation method of Tongjingning granula of TCD agent claimed in claim 1 is characterized in that, may further comprise the steps: get Radix Angelicae Sinensis (wine stir-fry) 333g, Rhizoma Cyperi (vinegar system) 333g, the Radix Paeoniae Alba (stir-fry) 333g, Radix Salviae Miltiorrhizae 333g, Rhizoma Corydalis (vinegar system) 300g, Fructus Toosendan (stir-fry), Rhizoma Chuanxiong (wine stir-fry) 200g, Radix Glycyrrhizae Preparata 133g, Flos Carthami 167g adds 10 times of amounts, reflux, extract, 2 hours for the first time with 80% alcohol reflux 2 times, filter, medicinal residues add 8 times of amounts for the second time, and reflux, extract, 1 hour is filtered, merging filtrate, decompression recycling ethanol is to distinguishing the flavor of without alcohol, and merge extractive liquid, filters, filtrate is concentrated into 60 ℃, and to survey density be 1.15-1.20 thick paste shape, add cross-linking sodium carboxymethyl cellulose 10g and binding agent and correctives, mix, granulate, drying, and get final product.
6. preparation method claimed in claim 5 is characterized in that, may further comprise the steps:
Get Radix Angelicae Sinensis (parched with wine) 333g, Rhizoma Cyperi (processed with vinegar) 333g, Radix Paeoniae Alba (parched with wine) 333g, Rhizoma Corydalis (processed with vinegar) 300g, Fructus Toosendan (parched) 300g, wine Rhizoma Chuanxiong (parched) 200g, Radix Glycyrrhizae Preparata 133g, Radix Salviae Miltiorrhizae 333g, and Flos Carthami 167g 10 times of amount 80% soak with ethanol in addition, heating and refluxing extraction 2 hours, collect extracting solution, filter, medicinal residues add in addition 8 times of amount 80% ethanol and continue reflux, extract,, 1 hour time.2 times extracting solution merges, left standstill 24 hours, and made precipitation fully, get supernatant, be concentrated into flowing soaking paste, 60 ℃ of lower densities are 1.15_1.20, make cooling, add at last dextrin 250g, sucrose 100g, cross-linking sodium carboxymethyl cellulose 10g, stir and granulate, dry below 60 ℃, granulate gets product.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1768820A (en) * | 2005-10-13 | 2006-05-10 | 贵州中卫时代医药经营有限公司 | Dysmenorrhea treating pharmaceutical formulation and preparation method thereof |
| CN102228591A (en) * | 2011-06-23 | 2011-11-02 | 贵州弘康药业有限公司 | Preparation method of oral medicinal preparation for regulating menstruation and stopping pains |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1768820A (en) * | 2005-10-13 | 2006-05-10 | 贵州中卫时代医药经营有限公司 | Dysmenorrhea treating pharmaceutical formulation and preparation method thereof |
| CN102228591A (en) * | 2011-06-23 | 2011-11-02 | 贵州弘康药业有限公司 | Preparation method of oral medicinal preparation for regulating menstruation and stopping pains |
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