CN102228591B - Preparation method of oral medicinal preparation for regulating menstruation and stopping pains - Google Patents
Preparation method of oral medicinal preparation for regulating menstruation and stopping pains Download PDFInfo
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Abstract
The invention discloses a preparation method of an oral medicinal preparation for regulating menstruation and stopping pains, which is prepared from the following nine Chinese medicinal herbs: Angelica (fried), cyperus rotundus (prepared), white paeony root (fried), corydalis tuber (fried), ligusticum wallichii (fried), liquorice (roasted), red-rooted salvia, toosendan fruit (fried) and safflower carthamus. The preparation method of the oral medicinal preparation for regulating menstruation and stopping the pains is optimized; an advanced steam distillation method is adopted, cyperus rotundus is extracted by using an ethanol extraction method, and corydalis tuber is extracted by using an ethanol refluxing extraction method; and compared with the prior art, the oral medicinal preparation prepared by using the method is more refined, has a more obvious medicinal effect and has better therapeutic effects on abnormal menstruation and dysmenorrheal.
Description
Technical field: the present invention relates to a kind of method for preparing of drug oral preparation of menstruction regulating and pain relieving, belong to the field of medicine technology.
Technical background: dysmenorrhea be meant that the women occurs before and after the menstrual period and between menstrual period with the waist sacrum, lower abdomen pain and general malaise are one type of disease of principal character.Whenever send out with menstrual cycle, severe patient can be accompanied nausea and vomiting, dripping cold sweat, deadly cold hand and foot, even faints, and brings influence for work and life.The traditional Chinese medical science thinks, dysmenorrhea is mainly smooth or experience pathogen because of feelings will, causes that QI and blood is not smooth in the body, invasion and attack women uterus, qi depression to blood stasis, the damage of cloudy blood, stagnation of QI and blood may bring about pain.With the passing of time do not heal, cause that very then the Secondary cases structural disease becomes.
'Tongjingning ' is derived from effective proved recipe of clinical menstruction regulating and pain relieving, and collection menstruction regulating and pain relieving, vital energy regualting and blood circulation-promoting, comprehensive method of treatment such as protecting this nourishes blood.Radix Angelicae Sinensis (stir-fry), Rhizoma Cyperi (system), the Radix Paeoniae Alba (stir-fry), Rhizoma Corydalis (stir-fry), Rhizoma Chuanxiong (stir-fry), Radix Glycyrrhizae (processing), Radix Salviae Miltiorrhizae, Fructus Toosendan (stir-fry) and Flos Carthami totally nine herbal medicines be prepared from, Radix Angelicae Sinensis nourishing blood and promoting blood circulation in the side is " regulating menstruation panacea " that the historical traditional Chinese medical science is praised highly; The kind especially regulating functional activities of vital QI of Rhizoma Cyperi and the pain relieving warp has the effect of the smooth feelings will of resolving depression simultaneously has " the women chief commander of section " good reputation.Two herbal medicines cooperate, embody vital energy regualting and blood circulation-promoting with pain relieving, nourish blood the menstruction regulating and pain relieving method basic admittedly.Radix Paeoniae Alba preserving YIN with astringents and nourishing blood protects the cloudy red root of women originally admittedly to assist Radix Angelicae Sinensis, is good at the easing the affected liver relieving spasm to stop pain again; Rhizoma Corydalis, Fructus Toosendan, Rhizoma Chuanxiong, Flos Carthami, Radix Salviae Miltiorrhizae or be longer than promoting blood circulation and stopping pain or be longer than promoting the circulation of QI to relieve pain, be and strengthen the active drug of analgesic effect in the other drug with thorough releasing dysmenorrhea; The collaborative onset of all medicines in the Radix Glycyrrhizae Preparata conditioning side, also can relieving spasm to stop pain.All medicines share that then menstruction regulating and pain relieving power is strong, and relieving dysmenorrhea symptom fast can be eliminated dysmenorrhoea disease again because of, the merit of playing menstruction regulating and pain relieving altogether, reaches the purpose of treating both the principal and secondary aspects of a disease.The method for distilling of existing 'Tongjingning ' generally is to adopt the peaceful syrupy method for preparing of putting down in writing on the ministry standard of dysmenorrhea: each medical material water is decocted; Wherein fry in shallow oil behind the Flos Carthami, get supernatant concentration after the decocting liquid hold over night, reuse ethanol precipitate with ethanol; Leave standstill, promptly get behind the recovery ethanol.Because there is defective in the said extracted method, makes that the part effective ingredient in the medicine runs off in leaching process, thereby makes that the clinical efficacy of medicine is not ideal enough.
Summary of the invention: technical problem to be solved by this invention is to provide a kind of method for preparing of drug oral preparation of menstruction regulating and pain relieving.
For solving the problems of the technologies described above; The present invention adopts following technical scheme to realize: a kind of drug oral preparation of menstruction regulating and pain relieving; Calculate according to composition by weight, it is prepared from Radix Angelicae Sinensis (stir-fry) 40-160, Rhizoma Cyperi (system) 40-160, the Radix Paeoniae Alba (stir-fry) 40-160, Rhizoma Corydalis (stir-fry) 35-150, Rhizoma Chuanxiong (stir-fry) 20-80, Radix Glycyrrhizae (processing) 15-60, Radix Salviae Miltiorrhizae 40-160, Fructus Toosendan (stir-fry) 35-150, Flos Carthami 20-80 and adjuvant;
Specifically: calculate according to composition by weight, it is prepared from Radix Angelicae Sinensis (stir-fry) 80, Rhizoma Cyperi (system) 80, the Radix Paeoniae Alba (stir-fry) 80, Rhizoma Corydalis (stir-fry) 72, Rhizoma Chuanxiong (stir-fry) 48, Radix Glycyrrhizae (processing) 32, Radix Salviae Miltiorrhizae 80, Fructus Toosendan (stir-fry) 72, Flos Carthami 40 and adjuvant.
The preparation method of the drug oral preparation of menstruction regulating and pain relieving according to the invention is: get rhizoma cyperi and extract volatile oil with steam distillation; The volatile oil single collection is subsequent use; Low amounts of water solution device is in addition collected; Adding the soaked in absolute ethyl alcohol that 10-30 doubly measures again spends the night; Refluxing extraction 2-6 hour, collect filtrating, behind the recovery ethanol; Add the aqueous solution that above-mentioned device is in addition collected, decompression concentrates and obtains Rhizoma Cyperi extract; Get corydalis tuber and pulverize, add the ethanol of 60-80%, refluxing extraction 1-3 time was extracted 0.5-5 hour with the alcohol reflux that 3-10 doubly measures 60-80% at every turn, merged extract, reclaimed ethanol, was evaporated to thick paste, got Corydalis P.E; Get Radix Angelicae Sinensis, the root of herbaceous peony, Ligusticum wallichii, Radix Glycyrrhizae, the red sage root and Fructus meliae toosendan, add 8-15 times of water gaging and decoct after 0.5-3 hour, add safflower; Continue to decoct 0.1-1 hour; Add 8-15 times of water gaging again and decocted 0.5-3 hour, collecting decoction filters; Filtrating is left standstill; Get supernatant concentration to thick paste, use the ethanol alcohol precipitation, leave standstill 12-48 hour after; Supernatant reclaims ethanol, is concentrated into thick paste; Above thick paste mixes with Rhizoma Cyperi extract and Corydalis P.E, and drying under reduced pressure is pulverized, and adds above-mentioned volatile oil and makes different oral formulations with conventional auxiliary material with conventional method.
Specifically; The preparation method of the drug oral preparation of menstruction regulating and pain relieving according to the invention is: get the rhizoma cyperi steam distillation and extract volatile oil; The volatile oil single collection is subsequent use; Low amounts of water solution device is in addition collected, and the soaked in absolute ethyl alcohol that adds 20 times of amounts is again spent the night, refluxing extraction 5 hours; Collect filtrating; After reclaiming ethanol, add the aqueous solution that above-mentioned device is in addition collected, decompression concentrates and obtains Rhizoma Cyperi extract; Get corydalis tuber and be ground into meal, add 70% ethanol, refluxing extraction 2 times is measured 70% ethanol with 8 times for the first time; Refluxing extraction 2 hours, with 6 times of amount 70% ethanol, refluxing extraction 1.5 hours merges extract for the second time; Reclaim ethanol, be evaporated to thick paste, get Corydalis P.E; Get Radix Angelicae Sinensis, the root of herbaceous peony, Ligusticum wallichii, Radix Glycyrrhizae, the red sage root and Fructus meliae toosendan, add 12 times of water gagings and decoct after 2 hours, add safflower; Continue to decoct 0.5 hour, add 10 times of water gagings again and decocted 1.5 hours, merge decocting liquid; Filter, the filtrating standing over night is got supernatant; Be concentrated into relative density being 85 ℃ is 1.10～1.12, puts coldly, adds the ethanol of 2 times of amounts; Stir; Left standstill 24 hours, and got supernatant and reclaim ethanol, be concentrated into thick paste; Above thick paste mixes with Rhizoma Cyperi extract and Corydalis P.E, and drying under reduced pressure is pulverized, and adds above-mentioned volatile oil and makes different oral formulations with conventional auxiliary material with conventional method.
Said oral formulations is meant capsule, tablet, pill and syrup.
Said tablet is meant coated tablet and Film coated tablets.
Specifically: the method for preparing of capsule according to the invention is: get after Rhizoma Cyperi extracts volatile oil with vapor distillation, the volatile oil single collection is subsequent use, and low amounts of water solution device is in addition collected; Adding the soaked in absolute ethyl alcohol that 10-30 doubly measures again spends the night; Reflux, extract, 2-6 hour, collect filtrating, behind the recovery ethanol; Add the aqueous solution that above-mentioned device is in addition collected, concentrating under reduced pressure obtains Rhizoma Cyperi extract; Get Rhizoma Corydalis and pulverize, add the ethanol of 60-80%, reflux, extract, 1-3 time is doubly measured alcohol reflux 0.5-5 hour of 60-80% with 3-10 at every turn, and merge extractive liquid, reclaims ethanol, is evaporated to thick paste, gets Rhizoma Corydalis extract; Get Radix Angelicae Sinensis, the Radix Paeoniae Alba, Rhizoma Chuanxiong, Radix Glycyrrhizae, Radix Salviae Miltiorrhizae and Fructus Toosendan, add 8-15 times of water gaging and decoct after 0.5-3 hour, add Flos Carthami, continue to decoct 0.1-1 hour; Add 8-15 times of water gaging again and decocted 0.5-3 hour, collecting decoction filters; Filtrating is left standstill, and gets supernatant concentration to thick paste, uses the ethanol precipitate with ethanol; After leaving standstill 12-48 hour, supernatant reclaims ethanol, is concentrated into thick paste; Above thick paste mixes with Rhizoma Cyperi extract and Rhizoma Corydalis extract, and drying under reduced pressure is pulverized, and gets medicated powder; Other mixes with above-mentioned volatile oil the get it filled starch of the thing amount of processing 3-10%, adds above-mentioned medicated powder mixing, incapsulates promptly to get.
The preparation method of pill according to the invention is: get after rhizoma cyperi extracts volatile oil with steam distillation; The volatile oil single collection is subsequent use; Low amounts of water solution device is in addition collected; Adding the soaked in absolute ethyl alcohol that 10-30 doubly measures again spends the night; Refluxing extraction 2-6 hour, collect filtrating, behind the recovery ethanol; Add the aqueous solution that above-mentioned device is in addition collected, decompression concentrates and obtains Rhizoma Cyperi extract; Get corydalis tuber and pulverize, add the ethanol of 60-80%, refluxing extraction 1-3 time was extracted 0.5-5 hour with the alcohol reflux that 3-10 doubly measures 60-80% at every turn, merged extract, reclaimed ethanol, was evaporated to thick paste, got Corydalis P.E; Get Radix Angelicae Sinensis, the root of herbaceous peony, Ligusticum wallichii, Radix Glycyrrhizae, the red sage root and Fructus meliae toosendan, add 8-15 times of water gaging and decoct after 0.5-3 hour, add safflower; Continue to decoct 0.1-1 hour; Add 8-15 times of water gaging again and decocted 0.5-3 hour, collecting decoction filters; Filtrating is left standstill; Get supernatant concentration to thick paste, use the ethanol alcohol precipitation, leave standstill 12-48 hour after; Supernatant reclaims ethanol, is concentrated into thick paste; Above thick paste mixes with Rhizoma Cyperi extract and Corydalis P.E, and drying under reduced pressure is pulverized, and gets medicinal powder; Other mixes with above-mentioned volatile oil the get it filled starch of the thing amount of making 3-10%, adds above-mentioned medicinal powder, mixing, and pill, drying, polishing or sugar coating or bag film-coating promptly get pill.
The method for preparing of syrup according to the invention is: get after Rhizoma Cyperi extracts volatile oil with vapor distillation, the volatile oil single collection is subsequent use, and low amounts of water solution device is in addition collected; Adding the soaked in absolute ethyl alcohol that 10-30 doubly measures again spends the night; Reflux, extract, 2-6 hour, collect filtrating, behind the recovery ethanol; Add the aqueous solution that above-mentioned device is in addition collected, concentrating under reduced pressure obtains Rhizoma Cyperi extract; Get Rhizoma Corydalis and pulverize, add the ethanol of 60-80%, reflux, extract, 1-3 time is doubly measured alcohol reflux 0.5-5 hour of 60-80% with 3-10 at every turn, and merge extractive liquid, reclaims ethanol, is evaporated to thick paste, gets Rhizoma Corydalis extract; Get Radix Angelicae Sinensis, the Radix Paeoniae Alba, Rhizoma Chuanxiong, Radix Glycyrrhizae, Radix Salviae Miltiorrhizae and Fructus Toosendan, add 8-15 times of water gaging and decoct after 0.5-3 hour, add Flos Carthami, continue to decoct 0.1-1 hour; Add 8-15 times of water gaging again and decocted 0.5-3 hour, collecting decoction filters, and filtrating is left standstill; Get supernatant concentration to thick paste, use the ethanol precipitate with ethanol, leave standstill 12-48 hour after; Supernatant reclaims ethanol, is concentrated into thick paste, gets drug extract; Other gets sucrose and adds water boil, filters, and be concentrated into relative density being 85 ℃ is 1.07～1.08; Above thick paste and said extracted thing mixing continue to be concentrated into thick paste, put cold; Filter, filtrating adds the benzoic acid of volatile oil and 0.1-0.25%, the ethylparaben of 0.01-0.25%; Add water to full dose again, stir, promptly get syrup.
The method for preparing of tablet according to the invention is: get after Rhizoma Cyperi extracts volatile oil with vapor distillation, the volatile oil single collection is subsequent use, and low amounts of water solution device is in addition collected; Adding the soaked in absolute ethyl alcohol that 10-30 doubly measures again spends the night; Reflux, extract, 2-6 hour, collect filtrating, behind the recovery ethanol; Add the aqueous solution that above-mentioned device is in addition collected, concentrating under reduced pressure obtains Rhizoma Cyperi extract; Get Rhizoma Corydalis and pulverize, add the ethanol of 60-80%, reflux, extract, 1-3 time is doubly measured alcohol reflux 0.5-5 hour of 60-80% with 3-10 at every turn, and merge extractive liquid, reclaims ethanol, is evaporated to thick paste, gets Rhizoma Corydalis extract; Get Radix Angelicae Sinensis, the Radix Paeoniae Alba, Rhizoma Chuanxiong, Radix Glycyrrhizae, Radix Salviae Miltiorrhizae and Fructus Toosendan, add 8-15 times of water gaging and decoct after 0.5-3 hour, add Flos Carthami, continue to decoct 0.1-1 hour; Add 8-15 times of water gaging again and decocted 0.5-3 hour, collecting decoction filters; Filtrating is left standstill, and gets supernatant concentration to thick paste, uses the ethanol precipitate with ethanol; After leaving standstill 12-48 hour, supernatant reclaims ethanol, is concentrated into thick paste; Above thick paste mixes with Rhizoma Cyperi extract and Rhizoma Corydalis extract, and drying under reduced pressure is pulverized, and gets medicated powder; Other gets the magnesium stearate of 0.5-1% and mixes with above-mentioned volatile oil, adds above-mentioned medicated powder mixing, tabletting, and sugar coating or film-coat promptly get tablet.
In the pharmaceutical preparation prescription of menstruction regulating and pain relieving, Rhizoma Cyperi has the resolving depression of regulating the flow of vital energy, the effect of menstruction regulating and pain relieving.Be used for stagnation of QI due to depression of the liver, breast, the side of body, abdominal distention, distending pain of the breast, menoxenia, amenorrhea dysmenorrhea etc.; The kind especially regulating functional activities of vital QI of Rhizoma Cyperi and the pain relieving warp has the effect of the smooth feelings will of resolving depression simultaneously is described as by the successive dynasties traditional Chinese medical science " Directorate-General DG of disorder of QI; the chief commander of women section "; Contain multiple monoterpene in the effective ingredient of Rhizoma Cyperi, sesquiterpene and oxide thereof and glycoside, flavonoid; Phenols and triterpenoid compound mainly are present in the volatile oil.In the primary standard technology, Rhizoma Cyperi adopts the decocting in water alcohol deposition method to extract, because the part effective ingredient is water insoluble, and the component of poor heat stability is prone to decompose in the Rhizoma Cyperi, makes content of effective lower; In this patent, extract Rhizoma Cyperi volatile oil with steam distillation earlier, can preserve volatile ingredient thermally labile and easy oxidation; The lixiviate of reuse ethanol can improve triterpenoid compound and other water-fast content of effective.Rhizoma Corydalis have invigorate blood circulation, promoting the circulation of QI, analgesic effect, its chemical constituent is mainly alkaloid, main effective ingredient of its performance analgesic effect is a tetrahydropalmatine; The analgesic activity of tetrahydropalmatine is strong, in the primary standard technology, adopts the decocting in water alcohol deposition method to extract Rhizoma Corydalis; Make that the extraction ratio of tetrahydropalmatine is not high; In this patent, adopt ethanol reflux extraction to extract Rhizoma Corydalis, can improve the content of tetrahydropalmatine.
Compared with prior art, the present invention is directed to and contain a large amount of water insoluble reaching heat-labile material in the Rhizoma Cyperi, take to extract Rhizoma Cyperi volatile oil with steam distillation earlier, the method for reuse ethanol lixiviate can be preserved wherein to heat-labile volatile material; Improve triterpenoid compound and other water-fast content of effective.Make and the not high shortcoming of extraction ratio of tetrahydropalmatine adopt ethanol reflux extraction to extract Rhizoma Corydalis to taking the decocting in water alcohol deposition method to extract Rhizoma Corydalis in the prior art, can improve the content of tetrahydropalmatine.The present invention is according to the character of each medicine in the pharmaceutical preparation of menstruction regulating and pain relieving; And this medicine role in prescription, the technology of the pharmaceutical preparation of menstruction regulating and pain relieving is optimized, make the refine more of this medicine; Drug effect is more remarkable, for menoxenia, dysmenorrhea better therapeutical effect is arranged.Compare with existing preparation, preparation active constituent content of the present invention is high, and clinical efficacy is good, has reached the purpose of invention.
The applicant has carried out following experiment, and provable the present invention has effective effect;
Experimental example 1: Rhizoma Corydalis Study on extraction
Preparation process of the present invention: get corydalis tuber and be ground into meal; The ethanol of adding 70%; Backflow refluxing extraction 2 times is for the first time with 8 times of amount 70% ethanol, refluxing extraction 2 hours; For the second time with 6 times of amount 70% ethanol; Refluxing extraction 1.5 hours merges extract, reclaims ethanol; Be evaporated to thick paste, promptly get;
Former preparation process: get Rhizoma Corydalis and add 12 times of water gagings decoctions after 2.5 hours, add 10 times of water gagings again and decocted 1.5 hours, merge decocting liquid, filter; The filtrating hold over night is got supernatant, and being concentrated into relative density is 1.10～1.12 (85 ℃), puts cold; Add the ethanol of 2 times of amounts, stir, left standstill 24 hours; Get supernatant and reclaim ethanol, be concentrated into thick paste, promptly get;
Detect the wherein content of tetrahydropalmatine respectively, the result is:
| Project | Preparation process of the present invention (relative amount %) | Former preparation process (relative amount %) |
| Tetrahydropalmatine | 0.06％ | 0.03％ |
Above experimental result shows that the content of tetrahydropalmatine is higher in the preparation process extract of the present invention, is superior to former preparation process.
Experimental example 2: the Rhizoma Cyperi Different Extraction Method is to the influence of dysmenorrhea model in mice
1, material:
1.1 medicine:
Rhizoma Cyperi is purchased the medical material company in Guizhou Province, is accredited as the dry rhizome into sedge dried tuber Cyperur rotundus L. through institute for drug control, Guizhou Province associate professor Lin Kaizhong.Diethylstilbestrol injection (20100801); Guangzhou Baiyunshan Mingxing Pharmaceutical Co., Ltd. produces, oxytocin solution (20100902), and Shanghai No.1 Bio-Chemical Pharmacetical Industry Co., Ltd produces; Ibuprofen oral administration mixed suspension (20100304), Tianda Pharmaceutical (Zhuhai) Co., Ltd. produces.
1.2 animal:
Kunming mouse, body weight 18～24g is provided by the Guiyang Medical College Experimental Animal Center.
1.3 laboratory sample
Preparation of the present invention: get the rhizoma cyperi steam distillation and extract volatile oil; The volatile oil single collection is subsequent use; Low amounts of water solution device is in addition collected, and the soaked in absolute ethyl alcohol that adds 20 times of amounts is again spent the night, and extracts 5 hours; Collect filtrating; Reclaim ethanol, add the above-mentioned aqueous solution, decompression is condensed into thick paste; Add the volatile oil mixing, promptly get;
Former technology preparation: get Rhizoma Cyperi and add 12 times of water gagings decoctions after 2.5 hours, add 10 times of water gagings again and decocted 1.5 hours, merge decocting liquid, filter; The filtrating hold over night is got supernatant, and being concentrated into relative density is 1.10～1.12 (85 ℃), puts cold; Add the ethanol of 2 times of amounts, stir, left standstill 24 hours; Get supernatant and reclaim ethanol, be concentrated into thick paste, promptly get; 1.4 the preparation of positive control solution: get ibuprofen suspension, with 3% tween solution diluted for use.
2, experimental technique:
Get 48 of female Kunming mouses, body weight 18～24g is divided into 4 groups at random, respectively as blank control group, positive controls, former technology group and of the present invention group.Every the equal subcutaneous injection diethylstilbestrol of animal 0.2mg/20g (except the blank control group), for three days on end, in the 1st day beginning gastric infusion; Continuous 4 days; After the last administration 1 hour, every animal is lumbar injection oxytocin 2u/20g again, observe and record 30min in mice turn round the body number of times.
3, result
Annotate: of the present invention group and the comparison of former technology group,
*P＜0.05
4, conclusion:
Learn that according to experimental result of the present invention group all has significant analgesia role with former technology group, can alleviate the fierceness that the uterine contraction element causes Mouse Uterus and shrink the pain symptom in the time of to alleviate dysmenorrhea; Wherein of the present invention group is superior to former technology group (P＜0.05).
Experimental example 3: pharmacodynamic study
Be the medicine that the confirms the method for the invention preparation effect for the dysmenorrhea due to women's qi stagnation blood stasis, our design has also been accomplished following test.
One, glacial acetic acid is caused the influence of pain effect to mice
1 experiment material
1.1 animal Kunming kind white mice, ♀ property, body weight 22～25g; Provide by the Guiyang Medical College Experimental Animal Center.
1.2 medicine: preparation of the present invention: be prepared into extractum according to the method for the invention; Former technology group: be prepared into extractum according to the 11st said method for distilling of the peaceful syrup of dysmenorrhea of the Sanitation Ministry medicine standard Chinese traditional patent formulation preparation; Above-mentioned medicine is used dissolved in distilled water respectively.
2 methods and result
Get 80 of Kunming kind ♀ property mices, be divided into 4 groups at random, 20 every group.The various 0.2ml/10g of lumbar injection (ip) medicine respectively, pethidine hydrochloride 10mg/kg, NS0.2ml/10g, behind the 15min, every Mus ip0.7% glacial acetic acid 0.1ml/10g causes pain; Interior each Mus of 15min is turned round the body number of times behind the record injection algogen.The result sees the following form.
Glacial acetic acid is caused the influence
of pain effect to mice
Annotate: of the present invention group and the comparison of former technology group,
*P＜0.05;
Learn that according to experimental result of the present invention group all can significantly be suppressed glacial acetic acid with former technology group causing bitterly of mice acted on; Wherein of the present invention group is superior to former technology group (P＜0.05).
Two, to the influence of normal rat uterus smooth muscle contraction function
1 experiment material
1.1 animal: Wistar kind rat, ♀ property, body weight 220～260g is provided by Guiyang Medical College medical experiment animal center.
1.2 medicine: preparation of the present invention: be prepared into extractum according to the method for the invention; Former technology group: be prepared into extractum according to the 11st said method for distilling of the peaceful syrup of dysmenorrhea of the Sanitation Ministry medicine standard Chinese traditional patent formulation preparation; Above-mentioned medicine is used dissolved in distilled water respectively.
2 methods and result
Get Wistar kind ♀ property virginity rat; Oestrus with the diethylstilbestrol manual work; Acute execution rat behind the 48h, preparation isolated uterine smooth muscle is fixed on the constant temperature (30 ℃ ± 1 ℃) that fills Rockwell liquid and bathes in the ware; The uterine smooth muscle load forces is 1g, with frequency of uterine contraction, amplitude before and after the two road physiology monitor record administrations.Behind uterine smooth muscle balance 30min, adding receives test product.The result sees table 1.Can be got by table 1, drug group all has the effect that suppresses frequency of uterine contraction, amplitude.
The influence
of table 2 pair normal rat uterus smooth muscle contraction function
Annotate: of the present invention group and the comparison of former technology group,
*P＜0.05;
Can know according to experimental result, all can control to some extent with former technology group for of the present invention group rat normal uterus smooth muscle contraction function; Wherein of the present invention group is superior to former technology group (P＜0.05).
Show according to above experimental result: medicine according to the invention can significantly be alleviated the fierceness contraction that the uterine contraction element causes Mouse Uterus; Suppress the cause pain effect of glacial acetic acid to mice; Rat normal uterus smooth muscle contraction function is suppressed to some extent, thus the pain symptom when alleviating dysmenorrhea; Prove that preparation of the present invention has blood-activating and qi-promoting analgesic function, has significant curative effect for the dysmenorrhea due to the qi stagnation blood stasis.
The specific embodiment:
Embodiment 1:
Prescription: Radix Angelicae Sinensis (stir-fry) 800g, Rhizoma Cyperi (system) 800g, the Radix Paeoniae Alba (stir-fry) 800g, Rhizoma Corydalis (stir-fry) 720g, Rhizoma Chuanxiong (stir-fry) 480g, Radix Glycyrrhizae (processing) 320g, Radix Salviae Miltiorrhizae 800g, Fructus Toosendan (stir-fry) 720g, Flos Carthami 400g
Technology: get the rhizoma cyperi steam distillation and extract volatile oil; The volatile oil single collection is subsequent use; Low amounts of water solution device is in addition collected; The soaked in absolute ethyl alcohol that adds 20 times of amounts is again spent the night; Refluxing extraction 5 hours is collected filtrating, behind the recovery ethanol; Add the aqueous solution that above-mentioned device is in addition collected, decompression concentrates and obtains Rhizoma Cyperi extract; Get corydalis tuber and be ground into meal, add 70% ethanol, refluxing extraction 2 times is measured 70% ethanol with 8 times for the first time; Refluxing extraction 2 hours, with 6 times of amount 70% ethanol, refluxing extraction 1.5 hours merges extract for the second time; Reclaim ethanol, be evaporated to thick paste, get Corydalis P.E; Get Radix Angelicae Sinensis, the root of herbaceous peony, Ligusticum wallichii, Radix Glycyrrhizae, the red sage root and Fructus meliae toosendan, add 12 times of water gagings and decoct after 2 hours, add safflower; Continue to decoct 0.5 hour, add 10 times of water gagings again and decocted 1.5 hours, merge decocting liquid; Filter, the filtrating standing over night is got supernatant; Be concentrated into relative density being 85 ℃ is 1.10～1.12, puts coldly, adds the ethanol of 2 times of amounts; Stir; Left standstill 24 hours, and got supernatant and reclaim ethanol, be concentrated into thick paste; Above thick paste mixes with Rhizoma Cyperi extract and Corydalis P.E, and drying under reduced pressure is pulverized, and gets medicinal powder; Other mixes with above-mentioned volatile oil the get it filled starch of the thing amount of making 5%, adds above-mentioned medicinal powder mixing, incapsulates promptly to get.
Usage and consumption: oral.One time 5,2 times on the one, take on an empty stomach, in day beginning to take continuous 10 days through the first seven.
Embodiment 2:
Prescription: Radix Angelicae Sinensis (stir-fry) 1600g, Rhizoma Cyperi (system) 1600g, the Radix Paeoniae Alba (stir-fry) 1600g, Rhizoma Corydalis (stir-fry) 1500g, Rhizoma Chuanxiong (stir-fry) 800g, Radix Glycyrrhizae (processing) 600g, Radix Salviae Miltiorrhizae 1600g, Fructus Toosendan (stir-fry) 1500g, Flos Carthami 800g
Technology: get rhizoma cyperi and extract volatile oil with steam distillation; The volatile oil single collection is subsequent use; Low amounts of water solution device is in addition collected; The soaked in absolute ethyl alcohol that adds 30 times of amounts is again spent the night; Refluxing extraction 6 hours is collected filtrating, behind the recovery ethanol; Add the aqueous solution that above-mentioned device is in addition collected, decompression concentrates and obtains Rhizoma Cyperi extract; Getting corydalis tuber pulverizes; The ethanol of adding 80%; Refluxing extraction 3 times; Extracted 5 hours with 10 times of amount 80% alcohol refluxs for the first time, extracted 3 hours with 6 times of amount 80% alcohol refluxs for the second time, extracted 0.5 hour with 3 times of amount 80% alcohol refluxs for the third time; Merge extract; Reclaim ethanol, be evaporated to thick paste, get Corydalis P.E; Get Radix Angelicae Sinensis, the root of herbaceous peony, Ligusticum wallichii, Radix Glycyrrhizae, the red sage root and Fructus meliae toosendan, add 15 times of water gagings and decoct after 3 hours, add safflower; Continue to decoct 1 hour, add 15 times of water gagings again and decocted collecting decoction 3 hours; Filter, filtrating is left standstill, and getting supernatant concentration is 1.10～1.12 to being 85 ℃ to relative density; Put cold; Add 80% ethanol of 4 times of amounts, stir, leave standstill 48 hours after; Supernatant reclaims ethanol, is concentrated into thick paste; Above thick paste mixes with Rhizoma Cyperi extract and Corydalis P.E, and drying under reduced pressure is pulverized, and gets medicinal powder; Other mixes with above-mentioned volatile oil the get it filled starch of the thing amount of making 8%, adds above-mentioned medicinal powder, mixing, and pill, drying, polishing or sugar coating or bag film-coating promptly get pill.
Usage and consumption: oral.A 5-10 ball 2 times on the one, is taken, in beginning to take continuous 10 days through the first seven day on an empty stomach.
Embodiment 3:
Prescription: Radix Angelicae Sinensis (stir-fry) 400g, Rhizoma Cyperi (system) 400g, the Radix Paeoniae Alba (stir-fry) 400g, Rhizoma Corydalis (stir-fry) 350g, Rhizoma Chuanxiong (stir-fry) 200g, Radix Glycyrrhizae (processing) 150g, Radix Salviae Miltiorrhizae 400g, Fructus Toosendan (stir-fry) 350g, Flos Carthami 200g
Technology: after getting rhizoma cyperi steam distillation extraction volatile oil; The volatile oil single collection is subsequent use; Low amounts of water solution device is in addition collected; The soaked in absolute ethyl alcohol that adds 20 times of amounts is again spent the night; Refluxing extraction 5 hours is collected filtrating, behind the recovery ethanol; Add the aqueous solution that above-mentioned device is in addition collected, decompression concentrates and obtains Rhizoma Cyperi extract; Get corydalis tuber and be ground into meal, add 70% ethanol, refluxing extraction 2 times is measured 70% ethanol with 8 times for the first time; Refluxing extraction 2 hours, with 6 times of amount 70% ethanol, refluxing extraction 1.5 hours merges extract for the second time; Reclaim ethanol, be evaporated to thick paste, get Corydalis P.E; Get Radix Angelicae Sinensis, the root of herbaceous peony, Ligusticum wallichii, Radix Glycyrrhizae, the red sage root and Fructus meliae toosendan, add 10 times of water gagings and decoct after 1 hour, add safflower; Continue to decoct 1 hour, add 12 times of water gagings again and decocted 2 hours, merge decocting liquid; Filter, the filtrating standing over night is got supernatant; Be concentrated into relative density being 85 ℃ is 1.10～1.12, puts coldly, adds the ethanol of 3 times of amounts; Stir, left standstill 35 hours, get supernatant and reclaim ethanol; Be concentrated into thick paste, get drug extract; Other gets sucrose and adds water boil; Filter, be concentrated into relative density being 85 ℃ is 1.07～1.08, above thick paste and said extracted thing mixing; Continue to be concentrated into thick paste; Put coldly, filter, filtrating adds the benzoic acid of volatile oil and 0.2%; 0.1% ethyl-para-hydroxybenzoate; Add water to 2000ml again, stir, promptly get syrup.
Usage and dosage: oral, a 25ml, 2 times on the one, decoction being taken warmly is used for beginning to take continuous 10 days through the first seven day on an empty stomach.
Embodiment 4:
Prescription: Radix Angelicae Sinensis (stir-fry) 1600g, Rhizoma Cyperi (system) 1600g, the Radix Paeoniae Alba (stir-fry) 400g, Rhizoma Corydalis (stir-fry) 350g, Rhizoma Chuanxiong (stir-fry) 200g, Radix Glycyrrhizae (processing) 150g, Radix Salviae Miltiorrhizae 1600g, Fructus Toosendan (stir-fry) 1500g, Flos Carthami 800g
Technology: get Rhizoma Cyperi and extract volatile oil with vapor distillation, the volatile oil single collection is subsequent use, and low amounts of water solution device is in addition collected; The soaked in absolute ethyl alcohol that adds 10 times of amounts is again spent the night; Reflux, extract, 2 hours is collected filtrating, behind the recovery ethanol; Add the aqueous solution that above-mentioned device is in addition collected, concentrating under reduced pressure obtains Rhizoma Cyperi extract; Get Rhizoma Corydalis and pulverize, add the ethanol of 10 times of amounts 60%, reflux, extract, 5 hours, extracting solution reclaims ethanol, is evaporated to thick paste, gets Rhizoma Corydalis extract; Get Radix Angelicae Sinensis, the Radix Paeoniae Alba, Rhizoma Chuanxiong, Radix Glycyrrhizae, Radix Salviae Miltiorrhizae and Fructus Toosendan, add 8 times of water gagings and decoct after 0.5 hour, add Flos Carthami, continue to decoct 0.1 hour; Add 8 times of water gagings again and decocted 0.5 hour, collecting decoction filters; Filtrating is left standstill, and gets supernatant concentration to thick paste, with the ethanol precipitate with ethanol of 3 times of amounts 60%; After leaving standstill 12 hours, supernatant reclaims ethanol, is concentrated into thick paste; Above thick paste mixes with Rhizoma Cyperi extract and Rhizoma Corydalis extract, and drying under reduced pressure is pulverized, and gets medicated powder; Other gets 0.8% magnesium stearate and mixes with above-mentioned volatile oil, adds above-mentioned medicated powder mixing, tabletting, and sugar coating promptly gets tablet.
Usage and consumption: oral.One time 5,2 times on the one, take on an empty stomach, in day beginning to take continuous 10 days through the first seven.
Claims (8)
1. the method for preparing of the peaceful oral formulations of dysmenorrhea is characterized in that: calculate according to composition by weight, it is prepared from according to following method Radix Angelicae Sinensis (parched) 40-160, Rhizoma Cyperi (processed) 40-160, Radix Paeoniae Alba (parched) 40-160, Rhizoma Corydalis (parched) rope 35-150, Rhizoma Chuanxiong (parched) 20-80, Radix Glycyrrhizae Preparata 15-60, Radix Salviae Miltiorrhizae 40-160, Fructus Toosendan (parched) 35-150, Flos Carthami 20-80 and adjuvant: get Rhizoma Cyperi and extract volatile oil with vapor distillation; The volatile oil single collection is subsequent use; Low amounts of water solution in addition device is collected, and adds the soaked in absolute ethyl alcohol that 10-30 doubly measures again and spends the night reflux, extract, 2-6 hour; Collect filtrating; After reclaiming ethanol, add the aqueous solution that above-mentioned device is in addition collected, concentrating under reduced pressure obtains Rhizoma Cyperi extract; Get Rhizoma Corydalis and pulverize, add the ethanol of 60-80%, reflux, extract, 1-3 time is doubly measured alcohol reflux 0.5-5 hour of 60-80% with 3-10 at every turn, and merge extractive liquid, reclaims ethanol, is evaporated to thick paste, gets Rhizoma Corydalis extract; Get Radix Angelicae Sinensis, the Radix Paeoniae Alba, Rhizoma Chuanxiong, Radix Glycyrrhizae, Radix Salviae Miltiorrhizae and Fructus Toosendan, add 8-15 times of water gaging and decoct after 0.5-3 hour, add Flos Carthami, continue to decoct 0.1-1 hour; Add 8-15 times of water gaging again and decocted 0.5-3 hour, collecting decoction filters; Filtrating is left standstill, and gets supernatant concentration to thick paste, uses the ethanol precipitate with ethanol; After leaving standstill 12-48 hour, supernatant reclaims ethanol, is concentrated into thick paste; Above thick paste mixes with Rhizoma Cyperi extract and Rhizoma Corydalis extract, and drying under reduced pressure is pulverized, and adds above-mentioned volatile oil and processes different oral formulations with conventional adjuvant with conventional method.
2. based on the preparation method of the peaceful oral formulations of the said dysmenorrhoea of claim 1; It is characterized in that: concrete preparation method is: get the rhizoma cyperi steam distillation and extract volatile oil; The volatile oil single collection is subsequent use; Low amounts of water solution device is in addition collected, and the soaked in absolute ethyl alcohol that adds 20 times of amounts is again spent the night, refluxing extraction 5 hours; Collect filtrating; After reclaiming ethanol, add the aqueous solution that above-mentioned device is in addition collected, decompression concentrates and obtains Rhizoma Cyperi extract; Get corydalis tuber and be ground into meal, add 70% ethanol, refluxing extraction 2 times is measured 70% ethanol with 8 times for the first time; Refluxing extraction 2 hours, with 6 times of amount 70% ethanol, refluxing extraction 1.5 hours merges extract for the second time; Reclaim ethanol, be evaporated to thick paste, get Corydalis P.E; Get Radix Angelicae Sinensis, the root of herbaceous peony, Ligusticum wallichii, Radix Glycyrrhizae, the red sage root and Fructus meliae toosendan, add 12 times of water gagings and decoct after 2 hours, add safflower; Continue to decoct 0.5 hour, add 10 times of water gagings again and decocted 1.5 hours, merge decocting liquid; Filter, the filtrating standing over night is got supernatant; Be concentrated into relative density being 85 ℃ is 1.10 ~ 1.12, puts coldly, adds the ethanol of 2 times of amounts; Stir; Left standstill 24 hours, and got supernatant and reclaim ethanol, be concentrated into thick paste; Above thick paste mixes with Rhizoma Cyperi extract and Corydalis P.E, and drying under reduced pressure is pulverized, and adds above-mentioned volatile oil and processes different oral formulations with conventional auxiliary material with conventional method.
3. according to the method for preparing of claim 1 or the peaceful oral formulations of 2 said dysmenorrheas, it is characterized in that: said oral formulations is meant capsule, tablet, pill or syrup.
4. according to the method for preparing of claim 1 or the peaceful oral formulations of 2 said dysmenorrheas, it is characterized in that: said tablet is meant coated tablet or Film coated tablets.
5. based on the preparation method of the peaceful oral formulations of the said dysmenorrhoea of claim 3; It is characterized in that: the preparation method of said capsule is: get after rhizoma cyperi extracts volatile oil with steam distillation; The volatile oil single collection is subsequent use; Low amounts of water solution in addition device is collected, and adds the soaked in absolute ethyl alcohol that 10-30 doubly measures again and spends the night refluxing extraction 2-6 hour; Collect filtrating; After reclaiming ethanol, add the aqueous solution that above-mentioned device is in addition collected, decompression concentrates and obtains Rhizoma Cyperi extract; Get corydalis tuber and pulverize, add the ethanol of 60-80%, refluxing extraction 1-3 time was extracted 0.5-5 hour with the alcohol reflux that 3-10 doubly measures 60-80% at every turn, merged extract, reclaimed ethanol, was evaporated to thick paste, got Corydalis P.E; Get Radix Angelicae Sinensis, the root of herbaceous peony, Ligusticum wallichii, Radix Glycyrrhizae, the red sage root and Fructus meliae toosendan, add 8-15 times of water gaging and decoct after 0.5-3 hour, add safflower; Continue to decoct 0.1-1 hour; Add 8-15 times of water gaging again and decocted 0.5-3 hour, collecting decoction filters; Filtrating is left standstill; Get supernatant concentration to thick paste, use the ethanol alcohol precipitation, leave standstill 12-48 hour after; Supernatant reclaims ethanol, is concentrated into thick paste; Above thick paste mixes with Rhizoma Cyperi extract and Corydalis P.E, and drying under reduced pressure is pulverized, and gets medicinal powder; Other mixes with above-mentioned volatile oil the get it filled starch of the thing amount of processing 3-10%, adds above-mentioned medicinal powder mixing, incapsulates promptly to get.
6. based on the preparation method of the peaceful oral formulations of the said dysmenorrhoea of claim 3; It is characterized in that: the preparation method of said pill is: get after rhizoma cyperi extracts volatile oil with steam distillation; The volatile oil single collection is subsequent use; Low amounts of water solution in addition device is collected, and adds the soaked in absolute ethyl alcohol that 10-30 doubly measures again and spends the night refluxing extraction 2-6 hour; Collect filtrating; After reclaiming ethanol, add the aqueous solution that above-mentioned device is in addition collected, decompression concentrates and obtains Rhizoma Cyperi extract; Get corydalis tuber and pulverize, add the ethanol of 60-80%, refluxing extraction 1-3 time was extracted 0.5-5 hour with the alcohol reflux that 3-10 doubly measures 60-80% at every turn, merged extract, reclaimed ethanol, was evaporated to thick paste, got Corydalis P.E; Get Radix Angelicae Sinensis, the root of herbaceous peony, Ligusticum wallichii, Radix Glycyrrhizae, the red sage root and Fructus meliae toosendan, add 8-15 times of water gaging and decoct after 0.5-3 hour, add safflower; Continue to decoct 0.1-1 hour; Add 8-15 times of water gaging again and decocted 0.5-3 hour, collecting decoction filters; Filtrating is left standstill; Get supernatant concentration to thick paste, use the ethanol alcohol precipitation, leave standstill 12-48 hour after; Supernatant reclaims ethanol, is concentrated into thick paste; Above thick paste mixes with Rhizoma Cyperi extract and Corydalis P.E, and drying under reduced pressure is pulverized, and gets medicinal powder; Other mixes with above-mentioned volatile oil the get it filled starch of the thing amount of processing 3-10%, adds above-mentioned medicinal powder, mixing, and pill, drying, polishing or sugar coating or bag film-coating promptly get pill.
7. according to the method for preparing of the peaceful oral formulations of the said dysmenorrhea of claim 3, it is characterized in that: the method for preparing of said syrup is: get after Rhizoma Cyperi extracts volatile oil with vapor distillation, the volatile oil single collection is subsequent use; Low amounts of water solution in addition device is collected, and adds the soaked in absolute ethyl alcohol that 10-30 doubly measures again and spends the night reflux, extract, 2-6 hour; Collect filtrating; After reclaiming ethanol, add the aqueous solution that above-mentioned device is in addition collected, concentrating under reduced pressure obtains Rhizoma Cyperi extract; Get Rhizoma Corydalis and pulverize, add the ethanol of 60-80%, reflux, extract, 1-3 time is doubly measured alcohol reflux 0.5-5 hour of 60-80% with 3-10 at every turn, and merge extractive liquid, reclaims ethanol, is evaporated to thick paste, gets Rhizoma Corydalis extract; Get Radix Angelicae Sinensis, the Radix Paeoniae Alba, Rhizoma Chuanxiong, Radix Glycyrrhizae, Radix Salviae Miltiorrhizae and Fructus Toosendan, add 8-15 times of water gaging and decoct after 0.5-3 hour, add Flos Carthami, continue to decoct 0.1-1 hour; Add 8-15 times of water gaging again and decocted 0.5-3 hour, collecting decoction filters, and filtrating is left standstill; Get supernatant concentration to thick paste, use the ethanol precipitate with ethanol, leave standstill 12-48 hour after; Supernatant reclaims ethanol, is concentrated into thick paste, gets drug extract; Other gets sucrose and adds water boil, filters, and be concentrated into relative density being 85 ℃ is 1.07～1.08; Above thick paste and said extracted thing mixing continue to be concentrated into thick paste, put cold; Filter, filtrating adds the benzoic acid of volatile oil and 0.1-0.25%, the ethylparaben of 0.01-0.25%; Add water to full dose again, stir, promptly get syrup.
8. based on the preparation method of the peaceful oral formulations of the said dysmenorrhoea of claim 4; It is characterized in that: the preparation method of said tablet is: get after rhizoma cyperi extracts volatile oil with steam distillation; The volatile oil single collection is subsequent use; Low amounts of water solution in addition device is collected, and adds the soaked in absolute ethyl alcohol that 10-30 doubly measures again and spends the night refluxing extraction 2-6 hour; Collect filtrating; After reclaiming ethanol, add the aqueous solution that above-mentioned device is in addition collected, decompression concentrates and obtains Rhizoma Cyperi extract; Get corydalis tuber and pulverize, add the ethanol of 60-80%, refluxing extraction 1-3 time was extracted 0.5-5 hour with the alcohol reflux that 3-10 doubly measures 60-80% at every turn, merged extract, reclaimed ethanol, was evaporated to thick paste, got Corydalis P.E; Get Radix Angelicae Sinensis, the root of herbaceous peony, Ligusticum wallichii, Radix Glycyrrhizae, the red sage root and Fructus meliae toosendan, add 8-15 times of water gaging and decoct after 0.5-3 hour, add safflower; Continue to decoct 0.1-1 hour; Add 8-15 times of water gaging again and decocted 0.5-3 hour, collecting decoction filters; Filtrating is left standstill; Get supernatant concentration to thick paste, use the ethanol alcohol precipitation, leave standstill 12-48 hour after; Supernatant reclaims ethanol, is concentrated into thick paste; Above thick paste mixes with Rhizoma Cyperi extract and Corydalis P.E, and drying under reduced pressure is pulverized, and gets medicinal powder; The dolomol that other gets 0.5-1% mixes with above-mentioned volatile oil, adds above-mentioned medicinal powder mixing, compressing tablet, and sugar coating or film-coating promptly get tablet.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102727808B (en) * | 2012-06-27 | 2014-01-08 | 王忠民 | Drug for rapidly treating dysmenorrheal and abdomen mass |
| CN103006972B (en) * | 2012-12-31 | 2014-07-16 | 浙江万邦药业股份有限公司 | Tongjingning granule and preparation thereof |
| CN105582232A (en) * | 2015-12-30 | 2016-05-18 | 贵州弘康药业有限公司 | Production method of Tongjingning preparation |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1425457A (en) * | 2003-01-02 | 2003-06-25 | 濮桂宝 | Granular preparation for dysmenorrhea |
| 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 |
| CN101708262A (en) * | 2009-12-21 | 2010-05-19 | 株洲千金药业股份有限公司 | Chinese medicinal composition capsules for treating dysmenorrhea and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1425457A (en) * | 2003-01-02 | 2003-06-25 | 濮桂宝 | Granular preparation for dysmenorrhea |
| 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 |
| CN101708262A (en) * | 2009-12-21 | 2010-05-19 | 株洲千金药业股份有限公司 | Chinese medicinal composition capsules for treating dysmenorrhea and preparation method thereof |
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Denomination of invention: Preparation method of oral medicinal preparation for regulating menstruation and stopping pains Effective date of registration: 20160115 Granted publication date: 20120829 Pledgee: Agricultural Bank Chinese Limited by Share Ltd. Longli County branch Pledgor: GUIZHOU HONGKANG PHARMACEUTICAL Co.,Ltd. Registration number: 2016520000001 |
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Denomination of invention: Preparation method of oral preparation of drugs for regulating menstruation and relieving pain Effective date of registration: 20210809 Granted publication date: 20120829 Pledgee: Agricultural Bank Chinese Limited by Share Ltd. Longli County branch Pledgor: GUIZHOU HONGKANG PHARMACEUTICAL Co.,Ltd. Registration number: Y2021520000010 |
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Denomination of invention: Preparation method of oral medication for regulating menstruation and relieving pain Granted publication date: 20120829 Pledgee: Agricultural Bank Chinese Limited by Share Ltd. Longli County branch Pledgor: GUIZHOU HONGKANG PHARMACEUTICAL Co.,Ltd. Registration number: Y2024980036648 |
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