CN100415253C - Medicinal composition for treating dysmenorrhea and preparation method thereof - Google Patents
Medicinal composition for treating dysmenorrhea and preparation method thereof Download PDFInfo
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- CN100415253C CN100415253C CNB2005100086573A CN200510008657A CN100415253C CN 100415253 C CN100415253 C CN 100415253C CN B2005100086573 A CNB2005100086573 A CN B2005100086573A CN 200510008657 A CN200510008657 A CN 200510008657A CN 100415253 C CN100415253 C CN 100415253C
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Abstract
The present invention discloses a medicinal composition for treating dysmenorrhea and a preparation method thereof. The present invention is characterized in that the medicinal composition is prepared from the following raw materials by the weight ratio: 100 to 400 portions of angelica, 400 to 800 portions of white peony alba, 100 to 400 portions of hemlock parsley, 100 to 400 portions of corydalis tuber processed with vinegar, 30 to 70 portions of manchurian wildginger and 1 to 5 portions of borneol. The medicinal composition of the present invention is used for treating primary dysmenorrhea and has the functions of inhibiting uterine contraction, alleviating pain and resisting inflammation.
Description
Invention field
The present invention relates to a kind of pharmaceutical composition and preparation method thereof, particularly relate to a kind of pharmaceutical composition for the treatment of dysmenorrhea and preparation method thereof.
Background technology
Primary dysmenorrhea is one of modal gynaecopathia of adolescence women, investigate through the physical constants cooperative groups according to national woman month in 1980, the dysmenorrhea sickness rate is 33.19%, wherein primary dysmenorrhea is 36.08%, 10% patient is arranged approximately because of serious symptom, absence from duty in 1-3 days was arranged in every month, bring for women's physical and mental health and work and have a strong impact on.The method of modern medicine treatment primary dysmenorrhea has pain relieving, calmness, spasmolytic, prostaglandin inhibitor, gonadal hormone and contraceptive etc., and these medicines mostly do not reach the purpose of healing, and side effect is bigger.Chinese medicine is of long standing and well established to the understanding of dysmenorrhea, and system, complete pathogenesis and dialectical theoretical system are arranged, and abundant, effective treatment side medicine and experience are arranged.Select the advantage field of Chinese medicine, be necessary to develop the pure Chinese medicinal preparation of treatment primary dysmenorrhea.
Summary of the invention
The object of the invention is to provide a kind of pharmaceutical composition; The object of the invention also is to provide a kind of preparation of drug combination method for the treatment of dysmenorrhea.
The present invention seeks to be achieved through the following technical solutions.
Pharmaceutical composition crude drug of the present invention consists of:
Radix Angelicae Sinensis 100-400 weight portion Radix Paeoniae Alba 400-800 weight portion
Rhizoma Chuanxiong 100-400 weight portion Rhizoma Corydalis (processed with vinegar) 100-400 weight portion
Herba Asari 30-70 weight portion Borneolum Syntheticum 1-5 weight portion Radix Glycyrrhizae Preparata 70-150 weight portion.
Pharmaceutical composition crude drug of the present invention is formed optimum ratio:
Radix Angelicae Sinensis 200-300 weight portion Radix Paeoniae Alba 500-700 weight portion
Rhizoma Chuanxiong 150-250 weight portion Rhizoma Corydalis (processed with vinegar) 150-250 weight portion
Herba Asari 40-60 weight portion Borneolum Syntheticum 1-5 weight portion Radix Glycyrrhizae Preparata 70-150 weight portion.
Pharmaceutical composition crude drug of the present invention form proportioning can also for:
The Radix Angelicae Sinensis 250 weight portion Radix Paeoniae Albas 600 weight portion Rhizoma Chuanxiongs 200 weight portions
Rhizoma Corydalis (processed with vinegar) 200 weight portion Herba Asaris 50 weight portion Borneolum Syntheticums 1 weight portion
Radix Glycyrrhizae Preparata 100 weight portions;
The Radix Angelicae Sinensis 150 weight portion Radix Paeoniae Albas 700 weight portion Rhizoma Chuanxiongs 160 weight portions
Rhizoma Corydalis (processed with vinegar) 350 weight portion Herba Asaris 40 weight portion Borneolum Syntheticums 4 weight portions
Radix Glycyrrhizae Preparata 85 weight portions;
The Radix Angelicae Sinensis 350 weight portion Radix Paeoniae Albas 550 weight portion Rhizoma Chuanxiongs 300 weight portions
Rhizoma Corydalis (processed with vinegar) 120 weight portion Herba Asaris 60 weight portion Borneolum Syntheticums 3 weight portions
Radix Glycyrrhizae Preparata 120 weight portions.
The invention described above pharmaceutical composition can be made clinical acceptable any dosage form, as pill, powder, capsule, soft capsule, tablet and powder agent, drop pill, oral liquid, injection etc.
Preparation of drug combination method of the present invention is:
Get Radix Angelicae Sinensis, Rhizoma Chuanxiong, Herba Asari three flavors and add 4-10 times of water gaging and extracted volatile oil 3-8 hour, collect volatile oil; Aqueous solution after the distillation filters, and device is collected in addition; Other gets the Radix Paeoniae Alba, Rhizoma Corydalis, Radix Glycyrrhizae Preparata three flavor medical materials, adds 4-8 times of water gaging and decocts 2-4 time, and each 0.5-2 hour, collecting decoction filtered; Aqueous solution after filtrate and the distillation merges, and being concentrated into relative density is 25 ℃ of surveys 1.20, gets concentrated solution; Add suitable concentrated solution 1.5-3 and doubly measure ethanol, stir evenly, staticly settle; Filter, decompression filtrate recycling ethanol gets the precipitate with ethanol concentrated solution to the greatest extent; The precipitate with ethanol concentrated solution adds clinical acceptable auxiliary, adds volatile oil, Borneolum Syntheticum mf mass pil, powder, capsule, soft capsule, tablet, granule, drop pill, oral liquid, injection etc. according to practice of pharmacy.The quality determining method of drug composition oral liquid preparation of the present invention comprises following discriminating and/or assay, and discriminating comprises one or more in the following discriminating:
A. get this product 10ml, water-bath is steamed near and is done, and residue adds ethanol 10ml, and slight fever makes dissolving, filters, and filtrate is concentrated into 2ml, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with 40: 5: 10: 0.2 chloroform-ethyl acetate-methanol-formic acid was developing solvent, launched, and took out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical bluish violet speckle;
B. get this product 10ml, add diethyl ether and extract 2 times, each 20ml merges ether extracted liquid, flings to ether, and residue adds ethyl acetate 2ml makes dissolving, as need testing solution.Other gets Radix Angelicae Sinensis, each 0.5g of Rhizoma Chuanxiong control medicinal material, mixes, and the 20ml that adds diethyl ether, supersound process 15 minutes filters, and filtrate low temperature is flung to ether, and residue adds ethyl acetate 2ml makes dissolving, in contrast medical material solution.According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with 9: 1 normal hexane-ethyl acetates, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show identical fluorescence speckle;
C. get this product 30ml, add liquor ammoniae fortis 5ml, shake up, add chloroform and extract 3 times, each 20ml, combined chloroform liquid reclaims chloroform, and residue adds ethanol 2ml makes dissolving, as need testing solution; Other gets the tetrahydropalmatine reference substance, adds ethanol and makes the solution that contains 1mg among every 1ml, in contrast product solution; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with 7: 3 cyclohexane extraction-acetone, launch, take out, to dry, spray is with rare bismuth potassium iodide test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical orange-yellow speckle;
Assay comprises: according to high performance liquid chromatography, be filler with octadecylsilane chemically bonded silica, 32: 68 methanol-water is mobile phase; The detection wavelength is 230nm; Theoretical cam curve is calculated by the peoniflorin peak should be not less than 3000; It is an amount of that precision takes by weighing the peoniflorin reference substance, adds mobile phase and make the solution that every 1ml contains peoniflorin 0.025mg, in contrast product solution; Precision is measured this product 5ml, puts in the 500ml measuring bottle, and thin up shakes up to scale, filters, and gets subsequent filtrate, promptly gets need testing solution; Accurate reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid respectively, measure, and the every ml of oral liquid contains peoniflorin (G
23H
28O
11) must not be less than 2.5mg.
Radix Angelicae Sinensis, Radix Paeoniae Alba nourshing blood and promoting blood circulation menstruction regulating and pain relieving are principal agent in the pharmaceutical composition of the present invention, and it is ministerial drug that Rhizoma Chuanxiong, Rhizoma Corydalis assist principal agent to strengthen the promoting flow of QI and blood analgesic effect, and Herba Asari, Borneolum Syntheticum, Radix Glycyrrhizae Preparata are adjuvant drug, Radix Glycyrrhizae Preparata double as messenger drug.Cure mainly promoting flow of QI and blood, menstruction regulating and pain relieving.Be applicable to the gastric abscess that causes by syndrome of qi stagnation and blood stasis, primary dysmenorrhea.
The clinical observation of drug composition oral liquid formulation treatment primary dysmenorrhea 72 examples of the present invention shows cure rate 22.22%, obvious effective rate 43.06%, effective percentage 31.95%.Pharmacodynamic test of active extract shows that medicine composite for curing primary dysmenorrhea of the present invention has following effect: directly suppress the uterus muscle contraction; Obviously suppress rabbit in body unpregnancy uterus muscle normal contraction; Can significantly resist the spastic contraction of unpregnancy uterus muscle; The alleviation uterus muscle of highly significant is acutely shunk and the dysmenorrhea disease of generation; Have remarkable analgesic activity and antiinflammatory action; Experimental result shows that this pharmaceutical composition can not cause obvious harmful effect to developing womb in the therapeutic dose scope.
Following experimental example and embodiment are used for explanation but are not limited to the present invention.
Experimental example 1:Six batches of little test results
Get best proportional quantity (being converted into occurrence), make oral liquid by process program of the present invention.6 batches of little test results are as follows:
Six batches of lab scale products of table 1 composition oral liquid preparation situation
By six batches of little test results, show the oral liquid of making by above-mentioned process program, quality all meets quality standard of the present invention, and this process program has science, reasonability, feasibility.
Experimental example 2:Five crowdes of pilot plant test results
50 times by experimental example 1 amount feed intake, by process program system oral liquid 50L of the present invention.Five crowdes of results are as follows:
Five batches of pilot product situations of table 2
The TCL of 5 batches of pilot products of ※ differentiates all positive
By five batches of pilot-scale experiment, show the oral liquid of making by above-mentioned process program, quality all meets quality standard of the present invention, and this process program has science, reasonability, feasibility.
Experimental example 3:Influence to the stripped unpregnancy uterus of rat normal contraction:
Get after the ablactation promptly 10 of above-mentioned health, maturation, the female unpregnancy rat raised every cage with male Mus, in the experiment before continuous 2 days, intramuscular injection every day estradiol benzoate 0.25ml (250ug)/only, manually cause rutting period is to improve the sensitivity of uterus to medicine.
Adopt the intestinal smooth muscle experimental provision that exsomatizes.Adjust instrument (two lead the used parameter of instrument: time constant BC, filtering hertz, sensitivity 0.5mv/cm, chart speed 25mm/min), it is constant in 30～32 ℃ to regulate bath temperature, continuously bubbling air (1～2 bubble/S) in bathing pipe lentamente.After real beginning preparation is appropriate, rat is shot dead, cut open the belly and cut the both sides cornua uteri and place the glass dish that fills locke solution standby.Get a side cornua uteri (being about 1.5cm) and be suspended to and bathe in the pipe, treat that isolated uterine flesh specimen is stablized 10min after, trace the normal contraction curve earlier, add various dose composition oral liquid and 0.25% indometacin solution more successively.A medicinal liquid contact of every adding 2min observes the 5min shrinkage curve and changes, and then with locke solution flushing 3 times, treats that baseline returns to the preceding level of medication and adds second medicine again.Be about 10min the blanking time of twice dosing.
The result shows: 1. 140% composition oral liquid 0.1 all can obviously suppress the stripped unpregnancy uterus muscle normal contraction (Fig. 1) of rat with 0.2ml (containing 0.14g and 0.28g crude drug), uterus muscle is lax fully, shrinkage amplitude, frequency and baseline three are fused to be in the same place, and is a straight line; 2. o.25% indometacin solution 0.1ml (0.25mg) does not see inhibitory action, and o.2ml (0.5mg) then has slight inhibitory action, but obvious not as good as the composition oral liquid effects.
Experimental example 4:Oxytocin, ergometrine are brought out the influence of the stripped spastic contraction of unpregnancy uterus muscle of rat:
The experimental implementation step is the same.Get 20 of aforementioned female unpregnancy rat, be divided into two groups, 10 every group by the random group method.Each group adds following medicine respectively successively:
I group: oxytocin one composition oral liquid one oxytocin one indometacin
II group: ergometrine one composition oral liquid one ergometrine one indometacin
Each group is all with the various dose repetitively administered.
The result shows: 1. 140% composition oral liquid 0.1,0.2,0.4ml (contain respectively 0.14,0.28,0.56g crude drug) all can resist the spastic contraction of uterus muscle that oxytocin 1u and 2u, ergometrine 0.04mg, 0.08mg bring out fully.Do not see that composition oral liquid has obvious dose-effect relationship; 2. i.e. (0.25 and 0.50mg) the spastic contraction of isolated rat uterus muscle that oxytocin, ergometrine are brought out of positive control drug 0.25% indometacin 0.1,0.2ml has slight antagonism (it is about 40% that amplitude reduces, and composition oral liquid then can reduce by 100%).
Rat isolated uterine result of the test (seeing Table 3) prompting composition oral liquid has the contraction of direct inhibition uterus muscle.
Table 3 is with the unpregnancy uterine contraction amplitude that exsomatizes behind the composition oral liquid, frequency change (X ± SD)
Experimental example 5:Composition oral liquid brings out the influence (oxytocin pain part spasm method) of mice dysmenorrhea to oxytocin
Select 50 of aforementioned female mices for use, be divided into 5 groups by randomized blocks, be respectively the normal saline group, rotundine o.05g/kg, composition oral liquid 14.0,28.0,42.0g (crude drug)/kg (press the conversion of body surface area ratio, be equivalent to 3.33 times, 6.67 times, 10 times of clinical dosage), 10 every group.Every Mus is all irritated stomach 0.001% diethylstilbestrol solution 130ug/kg before the administration, and once a day, continuous 4 days (the female mice sexual cycle was generally 4) is in order to improve the sensitivity of uterus muscle to oxytocin.2h after last is given diethylstilbestrol, each treated animal is irritated the stomach relative medicine.The every Mus lumbar injection of 1h oxytocin 100u/kg (2u/20g) after the administration observes the twisted reaction times that each Mus occurs in the 20min immediately, presses the acetic acid twisting method and estimates and result of calculation.Experimental result sees Table 4
Table 4 composition oral liquid is to the influence of the twisted reaction of oxytocin induced mice
* and normal saline are relatively
△Compare P＞0.05 with rotundine
Table 4 is the result show: 1h all has the alleviation oxytocin 100u/kg (2u/20g) of highly significant to bring out violent contraction of Mouse Uterus flesh and the dysmenorrhea disease (comparing P＜0.01 with the normal saline group) of generation after each the dosage group administration of composition oral liquid; But do not see tangible dose-effect reaction relation (P＞0.05) is arranged between each dosage: action intensity and rotundine 0.05g/kg group that each dosage group is alleviated mice dysmenorrhea disease compare there was no significant difference (P＞0.05).
Experimental example 6:The analgesic activity of composition oral liquid
According to a conventional method, room temperature is controlled at 19 ± 1 ℃, and electric heating constant temperature water tank bath temperature is controlled under 55 ± 0.5 ℃ the condition and carries out.Select 20 ± 2g female mice for use, every mouse assay two subnormal pain thresholds (in 5～30s is qualified Mus) before the administration, with 2 normal pain threshold means of gained as this Mus administration before pain threshold.Get 100 of the qualified mices of screening, be divided into 5 groups, be respectively normal saline group, rotundine 0.05/kg group, composition oral liquid 14.0,28.0,42.0g (crude drug)/kg group, 20 every group by randomized blocks.More than each group the disposable filling stomach of appearance method relative medicine such as all press.15min, 30min, 60min, 90min measure each Mus pain threshold respectively behind medicine, surpass 60S as pain threshold behind the medicine, then stop test and by 60S.Obtain after experiment finishes and respectively organize different time pain threshold (X ± SD), by formula calculate the threshold of pain and improve percentage rate, and carry out statistical procedures (t check).Experimental result sees Table 5.
Table 5 composition oral liquid is to the analgesic activity (hot plate method) of mice (X ± SD)
* with before the medicine compare P＜0.05
Compare P＜0.01 behind the * medicine before different time and the medicine
△Compare P＞0.05 behind the medicine before different time and the medicine
Table 5 is the result show: 1. the different time pain threshold reaches the significantly increases of normal saline group respectively with before the medicine behind each dosage group medicine of composition oral liquid, and P＜0.001 shows that composition oral liquid has obvious analgesic activity.Its analgesic activity 15min behind medicine occurs, and 30-60min reaches the peak, keeps more than the 90min.And show-quantitative effect relationship, i.e. 42g (crude drug)/kg group analgesia is renderd a service and obviously is better than 14g (crude drug)/kg group, P＜0.005 (but 28g crude drug/kg respectively with 14.0,42.0g crude drug/kg organize relatively analgesia effectiveness there was no significant difference, P＞0.05).
2. positive control drug rotundine 0.05g/kg has remarkable effect, but does not have significant difference, P＞0.05 with seven flavor pain-relieving liquid each dosage group intensity of relatively easing pain.
Experimental example 7:The antiinflammatory action of composition oral liquid
Choose 40 of aforementioned healthy white rats, be divided into 4 groups by randomized blocks, promptly normal saline group, positive control drug dexamethasone 0.0025g/kg, composition oral liquid 14.0,28.0g (crude drug)/kg organize 10 every group.Measure the normal girth of the left back ankle joint of each Mus (every Mus uses ball pen in the standardized horizontal line of left back ankle, to guarantee each measuring point self-consistentency: self-control arrowband chi can not be flexible) respectively with the circumferential measurements method.Thereafter, positive drug control group is with dexamethasone injection 0.0025g/kg lumbar injection, all the other each groups all with etc. the appearance method irritate the stomach relative medicine.Half an hour is subcutaneous and only cause inflammation to the fresh Ovum Gallus domesticus album 0.1ml/ of ankle joint surrounding injection at the left back foot sole of the foot of each Mus respectively after the administration.Cause scorching back and measure the left back ankle joint girth of each Mus every 10min, tie-in 6 times as the ankle swelling degree, is carried out statistical procedures (t check) with the difference of each time girth meansigma methods before the administration and after the administration.The results are shown in Table 6.
Table 6 composition oral liquid is to the influence (cm) of rat Ovum Gallus domesticus album pedal swelling
* compare with normal saline
△Compare P＞0.05 with dexamethasone.
The result shows: 1. composition oral liquid 14.0,28.0 (crude drug)/kg all have the effect of remarkable inhibition rat Ovum Gallus domesticus album pedal swelling, compare P value difference＜0.05 and＜0.001 with the normal saline group; Do not see obvious dose-effect reaction relation between the composition oral liquid two dosage groups.2. positive control drug dexamethasone 0.0025g/kg has the effect of remarkable inhibition rat Ovum Gallus domesticus album pedal swelling, compares action intensity and there was no significant difference, P＞0.05 with each dosage group of composition oral liquid.
Embodiment 1:
Radix Angelicae Sinensis 250g, Radix Paeoniae Alba 600g, Rhizoma Chuanxiong 200g, Rhizoma Corydalis (vinegar system) 200g, Herba Asari 50g, Borneolum Syntheticum 1g, Radix Glycyrrhizae Preparata 100g
Get Radix Angelicae Sinensis, Rhizoma Chuanxiong, Herba Asari three flavors and add 8 times of water gagings and extracted volatile oil 6 hours, collects about 3ml, the aqueous solution after the distillation filters, other device collection.Other gets three flavor medical materials such as the Radix Paeoniae Alba, Rhizoma Corydalis, Radix Glycyrrhizae Preparata, add 6 times of water gagings and decoct three times, each 1 hour, collecting decoction, filter, aqueous solution after filtrate and the distillation merges, and being concentrated into relative density is 1.20 (25 ℃ of surveys), adds the ethanol doubling dose, stir evenly, staticly settle, filter, decompression filtrate recycling ethanol is to most.Other gets simple syrup 100ml, merges with above-mentioned medicinal liquid, adds above-mentioned volatile oil, Borneolum Syntheticum, tween 80 10ml again, mixing, and leave standstill adjust pH to 5.0～6.5, filters, and adds water to 1000ml, stir evenly, fill, sterilization, promptly.
Embodiment 2:Composition oral liquid quality detection method
As embodiment 1 preparation composition oral liquid, carry out quality testing with the following method:
Differentiate: a. gets this product 10ml, and water-bath is steamed near and done, and residue adds ethanol 10ml, and slight fever makes dissolving, filters, and filtrate is concentrated into 2ml, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains lmg, in contrast product solution; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, (40: 5: 10: 0.2) be developing solvent, expansion was taken out with chloroform-ethyl acetate-methanol-formic acid, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical bluish violet speckle;
B. get this product 10ml, add diethyl ether and extract 2 times, each 20ml merges ether extracted liquid, flings to ether, and residue adds ethyl acetate 2ml makes dissolving, as need testing solution.Other gets Radix Angelicae Sinensis, each 0.5g of Rhizoma Chuanxiong control medicinal material, mixes, and the 20ml that adds diethyl ether, supersound process 15 minutes filters, and filtrate low temperature is flung to ether, and residue adds ethyl acetate 2ml makes dissolving, in contrast medical material solution.According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with normal hexane-ethyl acetate (9: 1), launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show identical fluorescence speckle;
C. get this product 30ml, add liquor ammoniae fortis 5ml, shake up, add chloroform and extract 3 times, each 20ml, combined chloroform liquid reclaims chloroform, and residue adds ethanol 2ml makes dissolving, as need testing solution; Other gets the tetrahydropalmatine reference substance, adds ethanol and makes the solution that contains 1mg among every 1ml, in contrast product solution; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with cyclohexane extraction-acetone (7: 3), launch, take out, to dry, spray is with rare bismuth potassium iodide test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical orange-yellow speckle;
Assay: according to high performance liquid chromatography, be filler with octadecylsilane chemically bonded silica, 32: 68 methanol-water is mobile phase; The detection wavelength is 230nm; Theoretical cam curve is calculated by the peoniflorin peak should be not less than 3000; It is an amount of that precision takes by weighing the peoniflorin reference substance, adds mobile phase and make the solution that every 1ml contains peoniflorin 0.025mg, in contrast product solution; Precision is measured this product 5ml, puts in the 500ml measuring bottle, and thin up shakes up to scale, filters, and gets subsequent filtrate, promptly gets need testing solution; Accurate reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid respectively, measure, and the every ml of oral liquid contains peoniflorin (G
23H
28O
11), must not be less than 2.5mg.
Embodiment 3
Radix Angelicae Sinensis 150 weight portions, Chinese herbaceous peony 700 weight portions, Rhizoma Chuanxiong 160 weight portions, Rhizoma Corydalis (processed with vinegar) 350 weight portions, Herba Asari 40 weight portions, Borneolum Syntheticum 4 weight portions, Radix Glycyrrhizae Preparata 85 weight portions;
Get Radix Angelicae Sinensis, Rhizoma Chuanxiong, Herba Asari three flavors and add 4-10 times of water gaging and extracted volatile oil 3-8 hour, collect volatile oil; Aqueous solution after the distillation filters, and device is collected in addition; Other gets the Radix Paeoniae Alba, Rhizoma Corydalis, Radix Glycyrrhizae Preparata three flavor medical materials, adds 4-8 times of water gaging and decocts 2-4 time, and each 0.5-2 hour, collecting decoction filtered; Aqueous solution after filtrate and the distillation merges, and being concentrated into relative density is 25 ℃ of surveys 1.20, gets concentrated solution; Add suitable concentrated solution 1.5-3 and doubly measure ethanol, stir evenly, staticly settle; Filter, decompression filtrate recycling ethanol gets the precipitate with ethanol concentrated solution to the greatest extent; The precipitate with ethanol concentrated solution adds clinical acceptable auxiliary, granulates, and drying adds volatile oil, Borneolum Syntheticum, filled capsules.
Embodiment 4:
Radix Angelicae Sinensis 350 weight portions, the Radix Paeoniae Alba 550 weight portions, Rhizoma Chuanxiong 300 weight portions, Rhizoma Corydalis (processed with vinegar) 120 weight portions, Herba Asari 60 weight portions, Borneolum Syntheticum 3 weight portions, Radix Glycyrrhizae Preparata 120 weight portions;
Get Radix Angelicae Sinensis, Rhizoma Chuanxiong, Herba Asari three flavors and add 4-10 times of water gaging and extracted volatile oil 3-8 hour, collect volatile oil; Aqueous solution after the distillation filters, and device is collected in addition; Other gets the Radix Paeoniae Alba, Rhizoma Corydalis, Radix Glycyrrhizae Preparata three flavor medical materials, adds 4-8 times of water gaging and decocts 2-4 time, and each 0.5-2 hour, collecting decoction filtered; Aqueous solution after filtrate and the distillation merges, and being concentrated into relative density is 25 ℃ of surveys 1.20, gets concentrated solution; Add suitable concentrated solution 1.5-3 and doubly measure ethanol, stir evenly, staticly settle; Filter, decompression filtrate recycling ethanol gets the precipitate with ethanol concentrated solution to the greatest extent; Precipitate with ethanol concentrated solution drying adds adjuvant and volatile oil, Borneolum Syntheticum according to practice of pharmacy, makes drop pill.
Embodiment 5:
Radix Angelicae Sinensis 350 weight portions, the Radix Paeoniae Alba 550 weight portions, Rhizoma Chuanxiong 300 weight portions, Rhizoma Corydalis (processed with vinegar) 120 weight portions, Herba Asari 60 weight portions, Borneolum Syntheticum 3 weight portions, Radix Glycyrrhizae Preparata 120 weight portions;
Get Radix Angelicae Sinensis, Rhizoma Chuanxiong, Herba Asari three flavors and add 4-10 times of water gaging and extracted volatile oil 3-8 hour, collect volatile oil; Aqueous solution after the distillation filters, and device is collected in addition; Other gets the Radix Paeoniae Alba, Rhizoma Corydalis, Radix Glycyrrhizae Preparata three flavor medical materials, adds 4-8 times of water gaging and decocts 2-4 time, and each 0.5-2 hour, collecting decoction filtered; Aqueous solution after filtrate and the distillation merges, and being concentrated into relative density is 25 ℃ of surveys 1.20, gets concentrated solution; Add suitable concentrated solution 1.5-3 and doubly measure ethanol, stir evenly, staticly settle; Filter, decompression filtrate recycling ethanol gets the precipitate with ethanol concentrated solution to the greatest extent; The precipitate with ethanol concentrated solution adds volatile oil, Borneolum Syntheticum and clinical acceptable auxiliary according to practice of pharmacy, makes injection.
Embodiment 6:
Radix Angelicae Sinensis 300 weight portions, the Radix Paeoniae Alba 500 weight portions, Rhizoma Chuanxiong 150 weight portions, Rhizoma Corydalis (processed with vinegar) 250 weight portions, Herba Asari 40 weight portions, Borneolum Syntheticum 5 weight portions, Radix Glycyrrhizae Preparata 70 weight portions;
Get Radix Angelicae Sinensis, Rhizoma Chuanxiong, Herba Asari three flavors and add 4-10 times of water gaging and extracted volatile oil 3-8 hour, collect volatile oil; Aqueous solution after the distillation filters, and device is collected in addition; Other gets the Radix Paeoniae Alba, Rhizoma Corydalis, Radix Glycyrrhizae Preparata three flavor medical materials, adds 4-8 times of water gaging and decocts 2-4 time, and each 0.5-2 hour, collecting decoction filtered; Aqueous solution after filtrate and the distillation merges, and being concentrated into relative density is 25 ℃ of surveys 1.20, gets concentrated solution; Add suitable concentrated solution 1.5-3 and doubly measure ethanol, stir evenly, staticly settle; Filter, decompression filtrate recycling ethanol gets the precipitate with ethanol concentrated solution to the greatest extent; The precipitate with ethanol concentrated solution adds clinical acceptable auxiliary, makes oral liquid according to practice of pharmacy adding volatile oil, Borneolum Syntheticum.
Embodiment 7:
As embodiment 6 preparation composition oral liquid, carry out quality testing with the following method:
Differentiate: get this product 10ml, add diethyl ether and extract 2 times, each 20ml merges ether extracted liquid, flings to ether, and residue adds ethyl acetate 2ml makes dissolving, as need testing solution.Other gets Radix Angelicae Sinensis, each 0.5g of Rhizoma Chuanxiong control medicinal material, mixes, and the 20ml that adds diethyl ether, supersound process 15 minutes filters, and filtrate low temperature is flung to ether, and residue adds ethyl acetate 2ml makes dissolving, in contrast medical material solution.According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with normal hexane-ethyl acetate (9: 1), launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show identical fluorescence speckle;
Get this product 30ml, add liquor ammoniae fortis 5ml, shake up, add chloroform and extract 3 times, each 20ml, combined chloroform liquid reclaims chloroform, and residue adds ethanol 2ml makes dissolving, as need testing solution; Other gets the tetrahydropalmatine reference substance, adds ethanol and makes the solution that contains 1mg among every 1ml, in contrast product solution; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with cyclohexane extraction-acetone (7: 3), launch, take out, to dry, spray is with rare bismuth potassium iodide test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical orange-yellow speckle;
Assay: according to high performance liquid chromatography, be filler with octadecylsilane chemically bonded silica, 32: 68 methanol-water is mobile phase; The detection wavelength is 230nm; Theoretical cam curve is calculated by the peoniflorin peak should be not less than 3000; It is an amount of that precision takes by weighing the peoniflorin reference substance, adds mobile phase and make the solution that every 1ml contains peoniflorin 0.025mg, in contrast product solution; Precision is measured this product 5ml, puts in the 500ml measuring bottle, and thin up shakes up to scale, filters, and gets subsequent filtrate, promptly gets need testing solution; Accurate reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid respectively, measure, and the every ml of oral liquid contains peoniflorin (G
23H
28O
11) must not be less than 2.5mg.
Claims (10)
1. pharmaceutical composition is characterized in that the crude drug for preparing this pharmaceutical composition consists of:
Radix Angelicae Sinensis 100-400 weight portion Radix Paeoniae Alba 400-800 weight portion
Rhizoma Chuanxiong 100-400 weight portion Rhizoma Corydalis (processed with vinegar) 100-400 weight portion
Herba Asari 30-70 weight portion Borneolum Syntheticum 1-5 weight portion
Radix Glycyrrhizae Preparata 70-150 weight portion.
2. pharmaceutical composition as claimed in claim 1 is characterized in that the crude drug for preparing this pharmaceutical composition consists of:
Radix Angelicae Sinensis 200-300 weight portion Radix Paeoniae Alba 500-700 weight portion
Rhizoma Chuanxiong 150-250 weight portion Rhizoma Corydalis (processed with vinegar) 150-250 weight portion
Herba Asari 40-60 weight portion Borneolum Syntheticum 1-5 weight portion
Radix Glycyrrhizae Preparata 70-150 weight portion.
3. pharmaceutical composition as claimed in claim 1 is characterized in that the crude drug for preparing this pharmaceutical composition consists of:
The Radix Angelicae Sinensis 250 weight portion Radix Paeoniae Albas 600 weight portion Rhizoma Chuanxiongs 200 weight portions
Rhizoma Corydalis (processed with vinegar) 200 weight portion Herba Asaris 50 weight portion Borneolum Syntheticums 1 weight portion
Radix Glycyrrhizae Preparata 100 weight portions.
4. pharmaceutical composition as claimed in claim 1 is characterized in that the crude drug for preparing this pharmaceutical composition consists of:
The Radix Angelicae Sinensis 150 weight portion Radix Paeoniae Albas 700 weight portion Rhizoma Chuanxiongs 160 weight portions
Rhizoma Corydalis (processed with vinegar) 350 weight portion Herba Asaris 40 weight portion Borneolum Syntheticums 4 weight portions
Radix Glycyrrhizae Preparata 85 weight portions.
5. pharmaceutical composition as claimed in claim 1 is characterized in that the crude drug for preparing this pharmaceutical composition consists of:
The Radix Angelicae Sinensis 350 weight portion Radix Paeoniae Albas 550 weight portion Rhizoma Chuanxiongs 300 weight portions
Rhizoma Corydalis (processed with vinegar) 120 weight portion Herba Asaris 60 weight portion Borneolum Syntheticums 3 weight portions
Radix Glycyrrhizae Preparata 120 weight portions.
6. as claim 1,2,3,4 or 5 described preparation of drug combination methods, it is characterized in that this method is:
Get Radix Angelicae Sinensis, Rhizoma Chuanxiong, Herba Asari three flavors and add 4-10 times of water gaging and extracted volatile oil 3-8 hour, collect volatile oil; Aqueous solution after the distillation filters, and device is collected in addition; Other gets the Radix Paeoniae Alba, Rhizoma Corydalis, Radix Glycyrrhizae Preparata three flavor medical materials, adds 4-8 times of water gaging and decocts 2-4 time, and each 0.5-2 hour, collecting decoction filtered; Aqueous solution after filtrate and the distillation merges, and being concentrated into relative density is 25 ℃ of surveys 1.20, gets concentrated solution; Add suitable concentrated solution 1.5-3 and doubly measure ethanol, stir evenly, staticly settle; Filter, decompression filtrate recycling ethanol gets the precipitate with ethanol concentrated solution to the greatest extent; The precipitate with ethanol concentrated solution adds clinical acceptable auxiliary, according to practice of pharmacy and volatile oil, Borneolum Syntheticum mf mass pil, powder, capsule, soft capsule, tablet, granule, drop pill, oral liquid or injection.
7. as the quality determining method of the oral liquid of claim 1,2,3,4 or 5 described pharmaceutical compositions, it is characterized in that this method comprises one or more in following discriminating and/or the assay:
A. get the oral liquid 10ml of described pharmaceutical composition, water-bath is steamed near and is done, and residue adds ethanol 10ml, and slight fever makes dissolving, filters, and filtrate is concentrated into 2ml, as need testing solution; Other gets the peoniflorin reference substance, adds ethanol and makes the solution that every 1ml contains 1mg, in contrast product solution; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, with 40: 5: 10: 0.2 chloroform-ethyl acetate-methanol-formic acid was developing solvent, launched, and took out, dry, spray is with 5% vanillin sulfuric acid solution, and it is clear that hot blast blows to the speckle colour developing; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical bluish violet speckle;
B. get the oral liquid 10ml of described pharmaceutical composition, add diethyl ether and extract 2 times, each 20ml merges ether extracted liquid, flings to ether, and residue adds ethyl acetate 2ml makes dissolving, as need testing solution.Other gets Radix Angelicae Sinensis, each 0.5g of Rhizoma Chuanxiong control medicinal material, mixes, and the 20ml that adds diethyl ether, supersound process 15 minutes filters, and filtrate low temperature is flung to ether, and residue adds ethyl acetate 2ml makes dissolving, in contrast medical material solution.According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, put respectively on same silica gel g thin-layer plate, be developing solvent with 9: 1 normal hexane-ethyl acetates, launch, take out, dry, put under the 365nm ultra-violet lamp and inspect; In the test sample chromatograph, with the corresponding position of control medicinal material chromatograph on, show identical fluorescence speckle;
C. get the oral liquid 30ml of described pharmaceutical composition, add liquor ammoniae fortis 5ml, shake up, add chloroform and extract 3 times, each 20ml, combined chloroform liquid reclaims chloroform, and residue adds ethanol 2ml makes dissolving, as need testing solution; Other gets the tetrahydropalmatine reference substance, adds ethanol and makes the solution that contains 1mg among every 1ml, in contrast product solution; According to the thin layer chromatography test, draw each 5 μ l of above-mentioned two kinds of solution, on the same silica gel g thin-layer plate of idea, be developing solvent respectively with 7: 3 cyclohexane extraction-acetone, launch, take out, to dry, spray is with rare bismuth potassium iodide test solution; In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical orange-yellow speckle;
Assay comprises: according to high performance liquid chromatography, be filler with octadecylsilane chemically bonded silica, 32: 68 methanol-waters are mobile phase; The detection wavelength is 230nm; Theoretical cam curve is calculated by the peoniflorin peak should be not less than 3000; It is an amount of that precision takes by weighing the peoniflorin reference substance, adds mobile phase and make the solution that every 1ml contains peoniflorin 0.025mg, in contrast product solution; Precision is measured the oral liquid 5ml of described pharmaceutical composition, puts in the 500ml measuring bottle, and thin up shakes up to scale, filters, and gets subsequent filtrate, promptly gets need testing solution; Accurate reference substance solution and each 10 μ l of need testing solution of drawing inject chromatograph of liquid respectively, measure, and the every ml of oral liquid contains peoniflorin G
23H
28O
11Must not be less than 2.5mg.
8. as claim 1,2,3, the application of 4 or 5 described pharmaceutical compositions in the medicine of preparation treatment primary dysmenorrhea.
9. application as claimed in claim 8 is characterized in that treating primary dysmenorrhea and is meant that suppressing uterus muscle shrinks.
10. has application in the medicine of analgesic activity and antiinflammatory action as claim 1,2,3,4 or 5 described pharmaceutical compositions in preparation.
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100086573A CN100415253C (en) | 2005-03-01 | 2005-03-01 | Medicinal composition for treating dysmenorrhea and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2005100086573A CN100415253C (en) | 2005-03-01 | 2005-03-01 | Medicinal composition for treating dysmenorrhea and preparation method thereof |
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| CN100415253C true CN100415253C (en) | 2008-09-03 |
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| CN102353744A (en) * | 2011-06-15 | 2012-02-15 | 贵州弘康药业有限公司 | Method for detecting quality of Tong Jingning capsule |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1110600A (en) * | 1995-01-17 | 1995-10-25 | 河南省焦作市卫生材料厂 | Antalgic paster and its preparation method |
| CN1334121A (en) * | 2001-08-31 | 2002-02-06 | 石家庄以岭药业有限公司 | Medicinal composition for restoring cardiac collaterals and its application |
| CN1368336A (en) * | 2001-02-05 | 2002-09-11 | 杨孟君 | Nano medicine 'Tongjingning' and its preparing process |
| CN1422658A (en) * | 2002-12-12 | 2003-06-11 | 郭士全 | Medicine for treating menalgia |
| CN1456289A (en) * | 2003-04-10 | 2003-11-19 | 毛友昌 | Preparing method gynaecologic capsule for regulating menstruation |
| CN1456267A (en) * | 2003-02-21 | 2003-11-19 | 毛友昌 | Preparation of tablets against irregular manstruation |
| CN1565553A (en) * | 2003-06-18 | 2005-01-19 | 薛永新 | Dysmenorrhea treating Chinese traditional medicine |
-
2005
- 2005-03-01 CN CNB2005100086573A patent/CN100415253C/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1110600A (en) * | 1995-01-17 | 1995-10-25 | 河南省焦作市卫生材料厂 | Antalgic paster and its preparation method |
| CN1368336A (en) * | 2001-02-05 | 2002-09-11 | 杨孟君 | Nano medicine 'Tongjingning' and its preparing process |
| CN1334121A (en) * | 2001-08-31 | 2002-02-06 | 石家庄以岭药业有限公司 | Medicinal composition for restoring cardiac collaterals and its application |
| CN1422658A (en) * | 2002-12-12 | 2003-06-11 | 郭士全 | Medicine for treating menalgia |
| CN1456267A (en) * | 2003-02-21 | 2003-11-19 | 毛友昌 | Preparation of tablets against irregular manstruation |
| CN1456289A (en) * | 2003-04-10 | 2003-11-19 | 毛友昌 | Preparing method gynaecologic capsule for regulating menstruation |
| CN1565553A (en) * | 2003-06-18 | 2005-01-19 | 薛永新 | Dysmenorrhea treating Chinese traditional medicine |
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| CN1827131A (en) | 2006-09-06 |
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