CN100376284C - Proprietary Chinese traditional medicine with marked effect in treating hysteromyoma, process for preparing the same and quality controlling method thereof - Google Patents
Proprietary Chinese traditional medicine with marked effect in treating hysteromyoma, process for preparing the same and quality controlling method thereof Download PDFInfo
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Abstract
The present invention relates to a Chinese patent medicine mainly for curing hysteromyoma, and a preparation method and a quality control method thereof, which relates to a medicinal product containing Chinese medicinal materials used as raw materials. The Chinese patent medicine mainly for curing hysteromyoma is prepared from the following medicinal materials of weight percentages: 12.57% to 18.85% of danshen root, 4.18% to 6.28% of sanchi, 6.67% to 9.03% of common prism tuber, 4.45% to 6.01% of zedoary, 5.34% to 7.22% of peach seed, 4.45% to 6.01% of angelica, 6.07% to 9.03% of turtle shell, 11.13% to 15.05% of seaweed, 4.71% to 5.75% of salt-baked Cortex Eucommiae, 7.06% to 8.64% of fried largehead atractylodes rhizome, 14.14% to 17.28% of scutellariae barbatae and 4.24% to 5.18% of cassia twig, wherein ginsenoside Rg1 of a powder D, which is measured by a high performance liquid chromatograph scanning method or a thin-layer chromatography scanning method, is not less than 1.5 mg/g. The Chinese patent medicine mainly for curing hysteromyoma is a Chinese patent medicine which is used for curing hysteromyoma and pelvic inflammatory masses and has outstanding therapy effects and less side effect. The preparation method is suitable for industrial production, and the quality control method has strong practicality and operability.
Description
Technical field
The present invention relates to contain the pharmaceutical products that Chinese crude drug is a raw material and the method for quality control of preparation method and product, specifically relate to a kind of Chinese patent medicine for the treatment of hysteromyoma of gynecology and inflammatory masses of pelvic cavity disease.
Background technology
Hysteromyoma, pelvic inflammatory lump are the higher benign tumors of sickness rate, are gynecological's common frdquently encountered disease, belong to the medical science “ of motherland mass in the abdomen " category.According to the interrelated data statistical report, women about 25% has potential hysteromyoma more than 30 years old.To this type of treatment of diseases, many both at home and abroad at present employing operative treatments or hormonotherapy, but the former is not suitable for unmarried and the women of child-bearing age, and latter's side effect is obvious, and complication is many.In recent years, the tame Chinese medicine that adopts of many doctors has been done exploratory treatment to primary disease, not only exempted the hardship of operation, and toxic and side effects is little, and method is safe and simple, has obtained gratifying achievement.
But by Literature Consult and patent retrieval, discovery lays particular emphasis on the observation of clinical efficacy more to the treatment of primary disease, or single, test, the clinical verification of classical prescription, do not form one or more clinical efficacies medicine preferably, and, lack preferred and comparability because the various places case is selected, success rate is added up and curative effect determinate standard is inconsistent.Therefore, the basic research and the theoretic further discussion of utilization Chinese medicine primary disease are for it rare, and with strong points, the comparatively ideal clinical new drug of curative effect, and be still rare so far.At present, " 2005 editions one disclosed GUIZHI FULING JIAONANG of Chinese pharmacopoeia (ball) is made up of Ramulus Cinnamomi, Poria, Cortex Moutan, Semen Persicae, the Radix Paeoniae Alba (Radix Paeoniae Rubra), is applied to treat hysteromyoma of gynecology and chronic pelvic inflammatory disease enclosed mass clinically.Its prescription comes from " Medical Treasures of the Golden Chamber " classics side, and drug for invigorating blood circulation and eliminating stasis is less relatively, the merit of blood circulation promoting and blood stasis dispelling a little less than.According to document " Chinese-English tcm prescription handbook commonly used (Ou Ming chief editor, Guangdong science and technology publishing house, 1991,407) described in: Ramulus Cinnamomi Poria pill, Didang Tang, Xiayuxue Tang, Decoction for Dischanging Blood clots all have the effect of blood circulation promoting and blood stasis dispelling, all can be used for all diseases of stomachache due to the congestion retardance, but its effectiveness has the difference of power, wherein the Didang Tang effect is the highest suddenly, inferior is Xiayuxue Tang, Decoction for Dischanging Blood clots, is Ramulus Cinnamomi Poria pill once more.
Summary of the invention
The purpose of this invention is to provide a kind of reasonable recipe, toxic and side effects is little, is specifically designed to the hysteromyoma and the inflammatory masses of pelvic cavity of treatment caused by energy stagnation and blood stasis, be convenient to take with Chinese patent medicine easy to carry and the preparation method and the method for quality control of this Chinese patent medicine be provided.
Be to implement by the following technical programs to achieve the object of the present invention:
The said Chinese patent medicine that cures mainly hysteromyoma, inflammatory masses of pelvic cavity of the present invention, it is the oral formulations of being made by the Chinese crude drug of following weight percentage ratio and method,
Prescription:
Radix Salviae Miltiorrhizae 12.57～18.85% Radix Notoginseng 4.18～6.28% rhizoma sparganic 6.67～9.03%
Rhizoma Curcumae 4.45～6.01% Semen Persicae (peeled) 5.34～7.22% Radix Angelicae Sinensis 4.45～6.01%
Carapax Trionycis 6.07～9.03% Sargassums 11.13～15.05% Cortex Eucommiae (parched with salt) 4.71～5.75%
Rhizoma Atractylodis Macrocephalae (parched) 7.06～8.64% Herba Scutellariae Barbataes 14.14～17.28% Ramulus Cinnamomi 4.24～5.18%
Radix Notoginseng, rhizoma sparganic, Rhizoma Curcumae, Carapax Trionycis four Chinese medicine material pulverize separately are become fine powder; Radix Angelicae Sinensis, Rhizoma Atractylodis Macrocephalae (parched), Ramulus Cinnamomi three flavor medicinal material extract volatile oil; Radix Salviae Miltiorrhizae, Cortex Eucommiae (parched with salt) two flavor medical materials are condensed into extractum A with 60～95% alcoholic solution extraction, extracting solution; Medicinal residues after Radix Angelicae Sinensis, Rhizoma Atractylodis Macrocephalae (parched), Ramulus Cinnamomi extracted medicinal residues behind the volatile oil and Radix Salviae Miltiorrhizae, Cortex Eucommiae (parched with salt) alcoholic solution and extract add Semen Persicae (peeled), Sargassum, Herba Scutellariae Barbatae three flavor medical materials and use water extraction together, and the water intaking extract is condensed into extractum B; Merge extractum A and extractum B and continue to be condensed into thick paste C, after the volatile oil of the fine powder of adding Radix Notoginseng, rhizoma sparganic, Rhizoma Curcumae, Carapax Trionycis and Radix Angelicae Sinensis, Rhizoma Atractylodis Macrocephalae (parched), Ramulus Cinnamomi is mixed into medicated powder D, process of Chinese medicine preparation is made oral formulations routinely, with containing Radix Notoginseng with the ginsenoside Rg among high performance liquid chromatography or the tlc-scanning determination medicated powder D
1Meter must not be less than 1.50mg/g.
Chinese patent medicine of the present invention is prepared from by 12 flavor Chinese crude drugs, Radix Salviae Miltiorrhizae, pseudo-ginseng blood-circulation-invigovating blood stasis dispelling ， Xiao Disorder pain relieving " control all blood, mend all labor, broken stagnant blood is supported fresh blood Ji the Zhu mass in the abdomen " in the prescription." book on Chinese herbal medicine converge with speech " points out " Radix Salviae Miltiorrhizae is kind controls blood system, removes the tissue regeneration promoting that stagnates, a thing and the merit of four things is arranged, the hemopoietic merits and demerits of enriching blood are returned ground, regulating menstruation is held back Resina Draconis and born Radix Paeoniae, removing blood stasis tissue regeneration promoting times rhizome of chuanxiong Rong "; Radix Notoginseng " with battalion hemostasis, the clots absorbing of promoting blood circulation, clots absorbing blood and hold back fresh blood " has the characteristics of " hemostasis and do not stay the stasis of blood ".Two medicines share, promoting tissue regeneration by removing blood stasis, and merit is grand energetically, so be monarch drug.Rhizoma sparganic, Rhizoma Curcumae, removing blood stasis, promoting the circulation of QI to relieve pain, Zhang Xichun particularly praises highly, and points out " rhizoma sparganic, Rhizoma Curcumae are the key medicine of blood stasis dispelling blood, and to control women sub-mass in the abdomen, menstruation is obstructed, the non-very speed of fiercely making contributions of property ".Add " if opinion Xiao Mo mass in the abdomen, ten times of Rhizoma Cyperis are also not as good as rhizoma sparganic, Rhizoma Curcumae ".Semen Persicae " bitter to let out stagnant blood, sweet " with tissue regeneration promoting blood, kind blood-retention of attacking with the passing of time, broken hard hematochezia closes; Radix Angelicae Sinensis is enriched blood, blood enriching and dryness moistening, and the stasis of blood is dispelled and impairment of YIN blood not.Carapax Trionycis, Sargassum, hard masses softening and resolving, replenishing YIN and removing heat.With monarch drug mutually 5, both can impel blood stasis to get rid of, dissipate, can pin down the property of the warm-dryness syndrome of activating blood and removing stasis drug again.And Carapax Trionycis is assaulted fortified position and do not decrease gas " negative and positive have painful abdominal mass to stagnate not except that the person up and down, all should use it ".Six medicines share, and principal drug assistance blood stasis dispelling blood, tissue regeneration promoting blood ， Xiao mass in the abdomen are minister altogether altogether.Rhizoma Atractylodis Macrocephalae (parched), invigorating the spleen and benefiting QI, stomach function regulating in the accent and removing food stagnancy are as a means of the source of generating QI and blood day after tomorrow; The Cortex Eucommiae, and replenishing kidney, strengthening waist Gu Chong behind the parch to black are with solid the congenital foundation.The Cortex Eucommiae, the Rhizoma Atractylodis Macrocephalae one solid the congenital foundation, the monarch drug promoting tissue regeneration by removing blood stasis is assisted in the source of money day after tomorrow altogether, and regulating menstruation leak-stopping ， Shi Disorder repercussive is dispelled and is not just hindered.Herba Scutellariae Barbatae, heat-clearing and toxic substances removing, the anti-cancer and detumescence tumor is adjuvant drug altogether.Ramulus Cinnamomi, warming the meridian and promoting blood circulation and and nutrient blood, with Semen Persicae in the side with 5, not only can promote blood circulation and seek but also can strengthen the power of blood stasis removing and clots absorbing, and can handsome all medicines to reach disease institute, so be messenger drug.Make a general survey of full side, the method for learning something in history and the side of obstinately following tradition not, reinforcement and elimination in combination, activation and usefulness, promoting tissue regeneration by removing blood stasis Er Xiao Disorder, all medicines share, figure blood circulation promoting and blood stasis dispelling altogether, the effect of hard masses softening and resolving.
The said Chinese patent medicine the best of the present invention is to make prescription by the Chinese crude drug of following weight percentage ratio:
Radix Salviae Miltiorrhizae 15.71% Radix Notoginseng 5.23% rhizoma sparganic 7.85%
Rhizoma Curcumae 5.23% Semen Persicae (peeled) 6.28% Radix Angelicae Sinensis 5.23%
Carapax Trionycis 7.85% Sargassum 13.09% Cortex Eucommiae (parched with salt) 5.23%
Rhizoma Atractylodis Macrocephalae (parched) 7.85% Herba Scutellariae Barbatae 15.71% Ramulus Cinnamomi 4.71%.
In order to take with easy to carry, said oral formulations can be to make tablet, capsule, pill, granule etc.
For reaching another object of the present invention, provide a kind of preparation method of the Chinese patent medicine that cures mainly hysteromyoma, inflammatory masses of pelvic cavity as follows: (1) takes by weighing Radix Notoginseng, rhizoma sparganic, Rhizoma Curcumae, Carapax Trionycis pulverize separately by recipe quantity and becomes fine powder, sieves, and is standby; (2) taking by weighing Radix Angelicae Sinensis, Rhizoma Atractylodis Macrocephalae (parched), Ramulus Cinnamomi by recipe quantity, to extract volatile oil with steam distillation standby; (3) claim Radix Salviae Miltiorrhizae, Cortex Eucommiae (parched with salt) to be condensed into 60～95% alcoholic solution extraction, filtration, extracting solution that to measure relative density 70～80 ℃ the time be 1.05～1.25 extractum A by recipe quantity, standby, medicinal residues are deposited in addition; (4) with Radix Angelicae Sinensis, Rhizoma Atractylodis Macrocephalae (parched), Ramulus Cinnamomi extracts medicinal residues and the Radix Salviae Miltiorrhizae behind the volatile oil, medicinal residues after the Cortex Eucommiae (parched with salt) alcoholic solution extracts add Semen Persicae (peeled), Sargassum, Herba Scutellariae Barbatae is used water boiling and extraction 1～3 time together, merge the water extract, be condensed into extractum B, merge extractum A and extractum B and continue to be condensed into that to measure relative density in the time of 70～80 ℃ be 1.15～1.30 thick paste C, (5) thick paste C adds Radix Notoginseng, rhizoma sparganic, Rhizoma Curcumae, the fine powder mixing of Carapax Trionycis, dry, pulverize, add Radix Angelicae Sinensis again, Rhizoma Atractylodis Macrocephalae (parched), the volatile oil of Ramulus Cinnamomi, be mixed into medicated powder D, can add proper quantity of medicinal auxiliary material then, process of Chinese medicine preparation is made oral formulations routinely, and Chinese medicine preparation is made oral formulations routinely.
Get the medicated powder D behind the above-mentioned adding volatile oil, directly filled capsules promptly gets capsule;
Get the medicated powder D behind the above-mentioned adding volatile oil, add pharmaceutic adjuvants such as proper amount of lubricating agent, direct compression, in order to extend the shelf life, plain sheet is coating again, promptly gets coated tablet.
Get the medicated powder D behind the above-mentioned adding volatile oil, add the adjuvant that allows on the pharmaceutics, granulate, sieve, promptly get granule.
Get the medicated powder D behind the above-mentioned adding volatile oil, as adhesive, make pill, maybe can continue coating and obtain with water and/or Mel.
Also can adopt the above-mentioned thick paste C that makes to add the fine powder of Radix Notoginseng, rhizoma sparganic, Rhizoma Curcumae, Carapax Trionycis, behind the mixing, add proper quantity of medicinal auxiliary material, granulate, add the volatile oil of Radix Angelicae Sinensis, Rhizoma Atractylodis Macrocephalae (parched), Ramulus Cinnamomi again, make granule, or be pressed into tablet.
For reaching another object of the present invention, a kind of method of quality control that cures mainly the Chinese patent medicine of hysteromyoma that is provided is: (1) is with containing the ginsenoside Rg among the high effective liquid chromatography for measuring medicated powder D
1Content; 2) with containing the ginsenoside Rg among the tlc-scanning determination medicated powder D
1Content.
Do not adopt medical material Radix Angelicae Sinensis, Radix Salviae Miltiorrhizae, Radix Notoginseng, Rhizoma Curcumae to prepare in order to check to have in the product, can also test with (1) thin layer chromatography, silica gel G is made lamellae, normal hexane: the ethyl acetate volume ratio is that 9: 1 mixed solution is done developing solvent, put under the ultra-violet lamp 365nm wavelength and inspect, on the corresponding position of Radix Angelicae Sinensis control medicinal material chromatograph, show the fluorescence principal spot of same color; (2) with thin layer chromatography test, be reference substance with the tanshinone, silica gel G is made lamellae, and with benzene: the ethyl acetate volume ratio is that 19: 1 mixed solution is done developing solvent, on the corresponding position of chromatograph, shows identical bolarious speckle; (3) with the thin layer chromatography test, with the ginsenoside Rg
1, ginsenoside Rb
1, Panax Notoginseng saponin R
1Be reference substance, the thick silica gel G of 500 μ m is made lamellae, and with chloroform: methanol: water volume ratio is that 13: 7: 2 mixed solution is done developing solvent, and spray on the corresponding position of chromatograph, shows the speckle of same color with the colour developing of 10% ethanol solution of sulfuric acid; (4) test with thin layer chromatography, the silica gel G that with the sodium carboxymethyl cellulose is adhesive is made lamellae, with chloroform: ether: the volume ratio of formic acid is that 9: 1: 0.1 mixed solution is done developing solvent, spray develops the color with 5% vanillin concentrated sulfuric acid solution, with the Guangxi zedoary medical material on the corresponding position of chromatograph, show the principal spot of same color.
Contain Radix Notoginseng with content of ginsenoside among the described high effective liquid chromatography for measuring medicated powder D, can adopt following method when concrete operations: chromatographic condition is filler with the octadecylsilane chemically bonded silica, with acetonitrile: 4% methanol solution volume ratio is that 18: 82 solution is made mobile phase, the detection wavelength is 203nm, column temperature is 35 ℃, and theoretical cam curve is by the ginsenoside Rg
1The peak calculates should be not less than 4000.
The ginsenoside Rg is got in the preparation of reference substance solution
1Reference substance adds mobile phase and makes every 1ml and contain the ginsenoside Rg
10.5mg solution, promptly.
The preparation of the need testing solution powder D4g that gets it filled puts in the conical flask of tool plug, adds water-saturated n-butanol 50ml, claim to decide weight, close plug, placement is spent the night, supersound process 30 minutes is put coldly, claims to decide weight again, supply the weight that subtracts mistake with water saturated n-butyl alcohol, shake up, filter, precision is measured subsequent filtrate 25ml, puts in the separatory funnel, washs with ammonia solution, discard ammonia solution, n-butanol layer evaporate to dryness, the accurate water that adds 10ml of residue, claim to decide weight, about 5 minutes of supersound process is disperseed residue, claim to decide weight again, water is supplied the weight that subtracts mistake, shakes up, and filters, precision is measured subsequent filtrate 5ml, put in the 10ml volumetric flask, and add mobile phase, shake up to scale, filter with microporous filter membrane, promptly.
Accurate respectively above-mentioned reference substance solution and each the 20 μ l of need testing solution of drawing of algoscopy inject chromatograph of liquid, measure, promptly.
The operational approach that described TLC scanning method is concrete is as follows: according to TLC scanning method (2005 editions appendix VIB of Chinese Pharmacopoeia) test.
The preparation of the need testing solution powder D 4g that gets it filled accurately claims surely, puts in the tool plug conical flask, the accurate water-saturated n-butanol 50ml that adds claims to decide weight, and supersound process claims to decide weight again, add water-saturated n-butanol and supply the weight that subtracts mistake, shake up, filter, precision is measured subsequent filtrate 25ml, with the ammonia solution washing, gets n-butyl alcohol liquid evaporate to dryness, residue adds dissolve with methanol and is transferred in the 2ml measuring bottle, add methanol to scale, shake up, as need testing solution;
The preparation precision of reference substance solution takes by weighing the ginsenoside Rg
1Reference substance adds methanol and makes the solution that every 1ml contains 1mg, in contrast product solution;
The accurate need testing solution 1 μ l that draws of assay method, reference substance solution 1 μ l, 5 μ l, respectively the cross point in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with chloroform: methanol: water volume ratio is 13: 7: 2 a solution, lower floor's solution of placing 12 hours below 10 ℃ is developing solvent, launches below 10 ℃, takes out, dry, spray is with 10% ethanol solution of sulfuric acid, and it is clear to be heated to the speckle colour developing at 105 ℃, takes out, on lamellae, cover onesize glass plate, fixing.Scan wavelength according to thin layer chromatography: λ s=525nm, measure test sample trap integrated value and reference substance trap integrated value, calculate, promptly.
For proving that product provided by the present invention can be used for treating the hysteromyoma and the inflammatory masses of pelvic cavity of caused by energy stagnation and blood stasis, carry out main pharmacodynamics research and toxicological test with product provided by the present invention, the result shows that this product has antagonistic Serum estrogen and progesterone level effect, and the Cavia porcellus leiomyoma of uterus sample hypertrophy that estrogen is brought out has significant inhibitory effect; Microcirculation and hemorheology to the syndrome of blood stasis animal pattern have significant improvement effect; Isolated rat uterine smooth muscle shrinkage amplitude is not had obvious influence, and remarkable inhibitory action (P＜0.05 and 0.01) is arranged for contraction frequency and uterine motility; Can significantly shorten the mice docking bleeding time, and clotting time is not made significant difference; Foreign body inflammation and rat granuloma swell in xylol induced mice inflammation, the rat uterus the obvious suppression effect.
One, anti-leiomyoma of uterus sample proliferative effect test
(1) animal and grouping:
Select 60 of female adult unpregnancy Cavia porcelluss for use, body weight 350-400g is divided into the blank group at random, modeling group, Ramulus Cinnamomi Poria pill group (GZFLW group), test specimen small dose group (DBJN low dose), the heavy dose of group of test specimen (DBJN heavy dose), 12 every group.
(2) medicine and reagent
Estradiol benzoate injection (1mg/ml); Progesterone injection (10mg/ml); Test group sample: the medicated powder D of following embodiment 1; Ramulus Cinnamomi Poria pill, Linfen, Shanxi Province pharmaceutical factory of traditional Chinese medicine produces.
(3) experimental technique and index
Make leiomyoma of uterus sample model of hyperplasia with reference to the Li Shi legal system.
Blank group is conventional raises, and irritates stomach normal saline 2ml every day;
Four groups of modeling methods are: the intramuscular injection estradiol benzoate, and 0.2mg/, 3 times weekly, after continuous three months, add a Progesterone 1.5mg/ intramuscular injection, 2 times/week, continuous one month.In modeling simultaneously, model group is only irritated stomach normal saline 2ml/ every day, the Ramulus Cinnamomi Poria pill group is irritated stomach Ramulus Cinnamomi Siberian cocklebur ball 3g/kg (0.5g/ml every day, 2ml//day, be equivalent to 20 times of 60kg body weight adult conventional amount used approximately), the test specimen small dose group is irritated this medicine medicated powder of stomach 1.5g/kg every day, be equivalent to 15 times of 60kg body weight adult convention amount approximately), the heavy dose of group of test specimen is irritated this medicine of stomach 3g/kg/ day (approximately when measuring 30 times in the adult) every day.After four months, all animals are weighed, and cut open the belly and observe the uterus general form, weighing in the clip uterus, calculates uterus coefficient (uterus weight/100g body weight), measure the above and subangle uterus root transverse diameter of cervix uteri, be fixed in 10% neutral formalin then, the above same area crosscut of the uterus subangle 0.3mm that draws materials, paraffin embedding, HE dyeing, om observation uterine cancer cell form, every section is chosen 5 positions micro-micrometer under 10 * 10 times of mirrors and is measured smooth muscle thickness, averages.
(4) statistical method
The data MINITAB SOFTWARE statistical software carries out one factor analysis of variance Q check to be handled.
(5) result
1, uterus weight: the model group uterus weight increases, compare with matched group, difference highly significant meaning (P＜0.01), the heavy dose of group of test specimen uterus weight significantly alleviates (P＜0.05) than model group, the test specimen small dose group, Ramulus Cinnamomi Poria pill group uterus weight has the trend of alleviating (P＞0.05) than model group, sees Table 1.
The comparison of table 1 uterus weight (X ± SD)
| Grouping | N | Body weight W1 (g) | The heavy W2 (g) in uterus | Uterus coefficient W2/W1 * 100 |
| The low dose of DBJN heavy dose of blank group model group GZFLW group DBJN | 12 12 12 12 12 | 622.0±77.0 448.0±61.4 423.6±37.5 424.1±44.2 422.7±53.5 | 1.14±0.30 3.99±1.07** 3.12±0.52 3.10±0.61 2.90±0.80# | 0.188±0.006 0.837±0.197** 0.774±0.130 0.731±0.138 0.686±0.179# |
* and matched group be P＜0.01 relatively
# and model group be P＜0.05 relatively
2, the uterus transverse diameter changes: the result shows that the blank group of model group two virgin palace transverse diameters increases thick, and difference has highly significant meaning (P＜0.01), and treatment group transverse diameter is all less than model group, and difference significance (P＜0.05) sees Table 2.
Table 2 uterus transverse diameter is (unit: the cm of X ± SD) relatively
| Grouping | N | Under the subangle | The subangle root |
| The low dose of DBJN heavy dose of blank group model group GZFLW group DBJN | 12 12 12 12 12 | 0.54±0.09 1.37±0.09** 1.16±0.14# 1.15±0.10# 1.12±0.08# | 0.28±0.05 0.61±0.10** 0.45±0.06# 0.44±0.05# 0.43±0.04# |
* and matched group be P＜0.01 relatively
# and model group be P＜0.05 relatively
3, uterine cancer cell is learned metamorphosis: mirror is observed down, and modeling component silver coin palace root smooth muscle layer obviously is inhomogeneous thickening, and the smooth muscle cell arrangement disorder, wherein has 7 smooth muscle to arrange and is cirriform or weaving shape, and pathological changes is similar to tumor sample hypertrophy; Large and small dosage group of test specimen and Ramulus Cinnamomi Poria pill component silver coin palace smooth muscle layer are thinner than modeling group (P＜0.05), arrange regularly, and test specimen small dose group and Ramulus Cinnamomi Poria pill group respectively have 2, and tumor sample hypertrophy pathological changes appears in 4 individual areas.
4, uterine smooth muscle varied in thickness: the model group uterine smooth muscle obviously thickens (P＜0.01) than the blank group, and the large and small dosage group of Ramulus Cinnamomi Poria pill and test specimen uterine smooth muscle thickness sees Table 3 than model group thin (P＜0.05).
Table 3 uterine smooth muscle thickness is (measurement unit is micro-micrometer counting) relatively
| Grouping | N | X±SD |
| The low dose of DBJN low dose of blank group model group GZFLW group DBJN | 12 12 12 12 12 | 26.60±3.02 54.38±8.89** 34.76±9.56# 34.23±7.90# 34.04±7.89# |
* and matched group be P＜0.01 relatively
# and model group be P＜0.05 relatively
(6) conclusion
Long-term Cavia porcellus intramuscular injection estradiol benzoate and the Progesterone given can cause the Cavia porcellus uterus weight to increase, and smooth muscle thickens, and pathological changes such as tumor sample hypertrophy appear in smooth muscle cell arrangement disorder, most animals uterine smooth muscle; Irritate hello test specimen of the present invention and can significantly improve above-mentioned pathological change, illustrate that product of the present invention has significant inhibitory effect for the Cavia porcellus leiomyoma of uterus sample hypertrophy that estrogen brings out, for the clinical treatment leiomyoma of uterus provides experimental basis, point out this experimental result to cure mainly consistent simultaneously with this product clinical function.
Two, to the hemorheological influence test of syndrome of blood stasis animal pattern
Experiment material:
1, animal: 32 of healthy unpregnancy rabbit, body weight 2.5-3.0kg, male and female dual-purpose.
2, medicine and reagent:
1. test specimen: getting medicated powder D of the present invention, use 70% alcohol solution dipping, is 70%, 50%, 30%, 10% alcoholic solution percolation then successively with concentration, more several percolates merged, and the extracting solution of simmer down to 70%, standby.
2. Ramulus Cinnamomi Poria pill: Ramulus Cinnamomi Poria pill extracting solution method for making is with test specimen extracting solution method for making.
Method and result:
Get 32 of rabbit, quiet notes 10% high molecular dextran 5ml/kg, every day 2 times, 2d causes high viscosity syndrome of blood stasis model continuously.In the 2nd day, for the second time to 15min behind the high molecular dextran, heart extracting blood, anticoagulant heparin is measured the preceding hemorheological indexes of medication.Respectively organize laboratory animal behind the 5d respectively with 5ml/kg/ day normal saline (matched group), 6g/kg/ day Ramulus Cinnamomi Poria pill (GZFLW group), 6g/kg/ day test specimen (DBJN heavy dose), 3g/kg/ day test specimen (DBJN low dose) suspension oral gavage, for three days on end.Gave high molecular dextran when beginning was with medication from the 2nd day of administration as stated above.Behind the 3rd the administration 50min, hemorheological indexes after the medication of heart extracting blood mensuration.The results are shown in Table 4.
Table 4 is to the rheol influence of " syndrome of blood stasis " rabbit blood (X ± SD)
| Grouping | N | Before and after the medication | Whole blood contrast viscosity | Whole blood reduction ratio viscosity | Plasma viscosity | Erythrocyte electrophoretic time (sec) | ||
| Low cutting | Height is cut | Low cutting | Height is cut | |||||
| Matched group | 8 | Behind the medicine prodrug | 5.89±0.45 5.38±0.42 | 3.81±0.20 3.56±0.18 | 12.12±1.24 11.16±1.13 | 6.89±0.59 6.53±0.50 | 1.51±0.07 1.48±0.05 | 30.64±1.87 31.26±1.27 |
| The GZFLW group | 8 | Behind the medicine prodrug | 5.76±0.51 4.62±0.64** | 3.66±0.20 3.21±0.22* | 11.85±1.44 9.17±1.53* | 6.10±0.43 5.61±0.52** | 1.49±0.05 1.35±0.06** | 30.47±1.70 28.56±1.18* |
| The DBJN heavy dose | 8 | Behind the medicine prodrug | 5.48±0.47 4.11±0.52 | 3.88±0.40 3.42±0.27** | 11.91±0.93 9.02±0.84* | 7.05±0.77 5.82±0.75** | 1.50±0.03 1.33±0.06** | 30.87±1.40 27.61±1.38* |
| The DBJN low dose | 8 | Behind the medicine prodrug | 5.43±0.40 4.51±0.59* | 3.65±0.18 3.40±0.25* | 10.98±0.80 9.10±0.78* | 6.58±0.44 5.70±0.56* | 1.49±0.03 1.36±0.05** | 30.40±1.21 28.68±1.41* |
Compare * P＜0.05 * * P＜0.01 with matched group
The above results shows: product of the present invention can reduce the viscosity of the high viscosity blood of rabbit due to the high molecular dextran significantly, compare before whole blood contrast viscosity, whole blood reduction ratio viscosity, plasma viscosity and the administration, all have significantly or significant differences (P＜0.05 or P＜0.01); Compare before and after each medication group erythrocyte electrophoretic time administration of test specimen, significant difference (P＜0.05) is arranged, and compare there was no significant difference (P＞0.05) before and after the corresponding matched group administration.
Conclusion: product of the present invention can improve the rat mesentery microcirculation disturbance state that epinephrine causes, promotes microcirculatory recovery; Can obviously reduce the viscosity of the high viscosity blood of rabbit due to the high molecular dextran, increase erythrocyte electrophoresis speed, thereby change hemorheological property.
Prompting: these results are consistent with the clinical efficacy of this medicine, also are its importances that is used to prevent and treat the disease mechanisms of action such as hysteromyoma, pelvic inflammatory lump.
Three, toxicologic study: (1) acute toxicity test: irritate stomach mice 3 times with adult 1879 times of oral dose to 24 hours branches, observed 7 days, do not see an animal dead.(2) long term toxicity test: with 120 times and 60 times of amounts of adult's oral dose, respectively to rat successive administration 180 days, after the drug withdrawal 15 days, to its hemogram, liver, renal functioies etc. detect, all find no toxic and side effects, each internal organs organ is carried out histology's pathologic finding, not seeing has pathological change.Prompting this product toxic and side effects is little, safe and reliable.
Four, with product provided by the present invention (title: red Trionyx sinensis Wiegmann capsule 0.38g/ grain) carry out clinical verification.
Adopt randomized, double-blind, parallel control, the open method of part, with this prescription is the treatment group, " GUIZHI FULING JIAONANG " is matched group, observe syndrome of qi stagnation and blood stasis hysteromyoma, pelvic inflammatory lump totally 480 examples, wherein (120 examples are organized in treatment to hysteromyoma 240 examples, matched group 90 examples, open group 30 examples), pelvic inflammatory lump 240 examples (120 examples are organized in treatment, matched group 60 examples, open group 60 examples).Result of the test is as follows:
1. respectively organize items such as patient's age, the course of disease, the state of an illness, sign, tcm syndrome before will treating and made statistics, through X 2 test, every being evenly distributed, tool comparability.
2. clinical total effects analysis, the total effective rate of hysteromyoma treatment group comprehensive therapeutic effect, tcm syndrome curative effect and sign curative effect is respectively 87.5%, 92.5%, 64.17%, 93.55, and matched group is respectively 75.56%, 82.22%, 45.56%.Learn by statistics and handle, P has significant differences all less than 0.01, and the treatment group is better than matched group " GUIZHI FULING JIAONANG "; The total effective rate of pelvic inflammatory lump treatment group comprehensive therapeutic effect, tcm syndrome curative effect and sign curative effect is respectively 93.33%, 96.67%, 91.67%, and matched group " GUIZHI FULING JIAONANG " is respectively 86.67%, 91.67%, 80.00%.Learn by statistics and handle, P has significant differences all less than 0.01, and the treatment group is better than matched group.
3. tcm symptom improves the situation comparative analysis, all can obviously improve every tcm symptom (P＜0.01) after treatment group and the treatment of control group, compare for two groups, the treatment group is better than matched group (P＜0.01) to the curative effect of lower abdominal distention pain, and all other do not have significant difference (P＞0.05).
4. the treatment group has 2 routine patients to occur slight dizziness once in a while after taking medicine one month in the clinical trial process, disappears automatically later, does not influence the continuation medication, and all the other do not see obvious adverse reaction.Security inspection by to blood, urine, just routine inspection and electrocardiogram, liver, renal function detect, and do not find obvious toxic-side effects, clinical use is safer.
In addition clinical observation cyclomastopathy, endometriosis, ovarian cyst, each 100 example of menoxenia, effective percentage is respectively 93.55%, 78.51%, 91.28%, 92.32%.
5. clinical test results shows, this product has the function of blood circulation promoting and blood stasis dispelling, hard masses softening and resolving, cure mainly qi depression to blood stasis, blood stasis and stay De mass in the abdomen (hysteromyoma, pelvic inflammatory lump, endometriosis, ovarian cyst) and cyclomastopathy due to knot uterus and the lower abdomen, menoxenia, card is seen: lower abdominal distention pain, lumbosacral aching pain, profuse leukorrhea, rectal tenesmus, tongue secretly have speckle.
The invention has the beneficial effects as follows:
1, this product has the function of blood circulation promoting and blood stasis dispelling, hard masses softening and resolving, cure mainly qi depression to blood stasis, blood stasis and stay De mass in the abdomen (hysteromyoma, pelvic inflammatory lump, endometriosis, ovarian cyst) and cyclomastopathy due to knot uterus and the lower abdomen, menoxenia, card is seen: lower abdominal distention pain, lumbosacral aching pain, profuse leukorrhea, rectal tenesmus, tongue secretly have speckle.For treatment hysteromyoma, pelvic inflammatory lump, cyclomastopathy, endometriosis, ovarian cyst, menoxenia have increased a determined curative effect, Chinese patent medicine that toxic and side effects is little.
2, preparation method is fit to industrialized mass.
3, the method for quality control simple possible of product is workable, is convenient to guarantee the quality of product.
Description of drawings
Accompanying drawing 1, be the preparation method general flow chart that cures mainly the hysteromyoma Chinese patent medicine provided by the present invention.
Below in conjunction with embodiment technical scheme of the present invention is described in further detail:
Embodiment 1:
One, half-finished preparation
Prescription:
Radix Salviae Miltiorrhizae 2850g Radix Notoginseng 950g rhizoma sparganic 1425g
Rhizoma Curcumae 950g Semen Persicae (peeled) 1140g Radix Angelicae Sinensis 950g
Carapax Trionycis 1425g Sargassum 2375g Cortex Eucommiae (parched with salt) 950g
Rhizoma Atractylodis Macrocephalae (parched) 1425g Herba Scutellariae Barbatae 2850g Ramulus Cinnamomi 855g
Operational approach: see accompanying drawing 1
1. take by weighing Radix Notoginseng, rhizoma sparganic, Rhizoma Curcumae, Carapax Trionycis four Chinese medicine material, pulverize separately becomes fine powder, takes by weighing standby by recipe quantity.
2. by recipe quantity take by weighing Radix Salviae Miltiorrhizae, Cortex Eucommiae (parched with salt) is broken into 1cm with interior piece section, with 6 times of amount 90% alcohol reflux twice, each 1 hour, ethanol extract filtered, surveying when being condensed into 70 ℃ of relative densities is 1.20 extractum A, standby.Medicinal residues are deposited in addition.
3. take by weighing Radix Angelicae Sinensis, Rhizoma Atractylodis Macrocephalae (parched), Ramulus Cinnamomi by recipe quantity, extract volatile oil with steam distillation, standby.
4. the medicinal residues that extract medicinal residues behind the volatile oil and above-mentioned Radix Salviae Miltiorrhizae, Cortex Eucommiae (parched with salt) merge, add Sargassum, Semen Persicae (peeled), Herba Scutellariae Barbatae three flavor medical materials again, decoct 2 times with 12 times of water gagings, each 1.5 hours, after the water extract filters, be condensed into extractum B, add extractum A again, surveying when continuing to be concentrated into 70 ℃ of relative densities is 1.27 thick paste C.
5. thick paste C adds the fine powder of Radix Notoginseng, rhizoma sparganic, Rhizoma Curcumae and Carapax Trionycis, mixing, cold drying below 60 ℃ was ground into the medicated powder of 65 mesh sieves, added volatile oil, mixing, medicated powder D.With containing Radix Notoginseng with the ginsenoside Rg among the high effective liquid chromatography for measuring medicated powder D
1Meter is 4.060mg/g.
Two, the preparation of preparation
The hard capsule preparation
The powder D380g that gets it filled loads capsule, makes 1000, promptly.Every capsules is equipped with medicated powder 0.38g, contains Radix Notoginseng with the ginsenoside Rg with tlc-scanning determination
1Count the 1.54mg/ grain.
Preparation tablets
The powder D380g that gets it filled adds sodium carboxymethyl cellulose 3.8g, magnesium stearate 1.9g, and mix homogeneously is pressed into 1000, every heavy 0.38g, tlc-scanning determination contains Radix Notoginseng with the ginsenoside Rg
1Count the 1.52mg/ grain.
The granule preparation
The powder D 380g that gets it filled makes granule, is distributed into the heavy 1.9g of the every bag of 200 bags, promptly.Contain Radix Notoginseng with the ginsenoside Rg with tlc-scanning determination
1Count the 6.94mg/ bag.
The pill preparation
The powder D 380g that gets it filled adds suitable quantity of water, the general ball of making, and drying is made 2000 of the watered pills, every 0.19g, promptly.Contain Radix Notoginseng with the ginsenoside Rg with tlc-scanning determination
1Count 0.75mg/g.
Embodiment 2～6:
With the operation of embodiment 1, actual conditions is as follows:
Half-finished preparation
1. inventory
| The medical material title | Weight (g) | ||||
| Example 2 | Example 3 | Example 4 | Example 5 | Example 6 | |
| Radix Notoginseng | 38.00 | 285.00 | 213.75 | 475.00 | 522.50 |
| Radix Salviae Miltiorrhizae | 171.00 | 570.00 | 783.75 | 1425.00 | 1282.50 |
| Rhizoma sparganic | 60.57 | 391.87 | 320.63 | 712.50 | 748.13 |
| Rhizoma Curcumae | 54.62 | 213.75 | 249.38 | 475.00 | 451.25 |
| Radix Angelicae Sinensis | 45.13 | 249.38 | 225.63 | 475.00 | 546.25 |
| Carapax Trionycis | 74.81 | 338.44 | 409.68 | 712.50 | 605.63 |
| Semen Persicae (peeled) | 51.30 | 327.75 | 242.25 | 570.00 | 627.00 |
| Sargassum | 130.63 | 504.69 | 653.13 | 1187.50 | 1068.75 |
| Cortex Eucommiae (parched with salt) | 42.75 | 249.38 | 225.63 | 475.00 | 522.50 |
| Rhizoma Atractylodis Macrocephalae (parched) | 78.37 | 338.44 | 374.06 | 712.5 | 641.25 |
| Herba Scutellariae Barbatae | 149.63 | 641.25 | 676.88 | 1425 | 1567.5 |
| Ramulus Cinnamomi | 38.48 | 235.12 | 224.44 | 427.5 | 406.13 |
2. the extraction of volatile oil
Extract with steam distillation, each embodiment volatile oil extracted amount sees the following form.
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | |
| Volatile oil (ml) | 0.10 | 0.60 | 0.50 | 1.05 | 1.22 |
3. ethanol extraction
Each embodiment leaching process and related process parameter see the following form.
| Process conditions | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 |
| Concentration of alcohol (%) | 60 | 70 | 80 | 90 | 95 |
| Extraction time | 3 | 3 | 2 | 2 | 1 |
| Relative density | 1.05/76℃ | 1.20/73℃ | 1.25/75℃ | 1.23/75℃ | 1.20/78℃ |
| Extractum A weight (g) | 32.36 | 137.75 | 112.45 | 238.06 | 153.20 |
(4) water is carried
Each embodiment leaching process and related process parameter see the following form.
| Process conditions | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 |
| Extraction time | 1 | 2 | 2 | 2 | 3 |
| Relative density | 1.20/75℃ | 1.23/77℃ | 1.25/80℃ | 1.25/76℃ | 1.24/74℃ |
| Extractum B weight (g) | 200.71 | 1367.03 | 1415.36 | 2859.15 | 3336.18 |
(5) preparation of thick paste C
Each embodiment leaching process and related process parameter see the following form.
| Process conditions | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 |
| Relative density | 1.15/80℃ | 1.25/76℃ | 1.24/73℃ | 1.26/70℃ | 1.30/70℃ |
| Weight (g) | 215.83 | 1379.47 | 1412.89 | 2979.39 | 3048.16 |
(6) preparation of medicated powder D
Each embodiment leaching process and related process parameter see the following form.
| Process conditions | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 |
| Weight (g) | 331.46 | 1875.90 | 1862.49 | 3800.00 | 3795.63 |
| Moisture content (%) | 2.3 | 2.1 | 2.4 | 2.3 | 2.2 |
| Rg 1Content (mg/g) | 2.487 | 4.152 | 3.831 | 4.069 | 4.306 |
Claims (6)
1. a Chinese patent medicine that cures mainly hysteromyoma, inflammatory masses of pelvic cavity is characterized in that it being the oral formulations of being made by the Chinese crude drug and the method for following weight percentage ratio,
Prescription:
Radix Salviae Miltiorrhizae 12.57～18.85% Radix Notoginseng 4.18～6.28% rhizoma sparganic 6.67～9.03%
Rhizoma Curcumae 4.45～6.01% Semen Persicae (peeled) 5.34～7.22% Radix Angelicae Sinensis 4.45～6.01%
Carapax Trionycis 6.07～9.03% Sargassums 11.13～15.05% Cortex Eucommiae (parched with salt) 4.71～5.75%
Rhizoma Atractylodis Macrocephalae (parched) 7.06～8.64% Herba Scutellariae Barbataes 14.14～17.28% Ramulus Cinnamomi 4.24～5.18%
Radix Notoginseng, rhizoma sparganic, Rhizoma Curcumae, Carapax Trionycis pulverize separately are become fine powder; Radix Angelicae Sinensis, Rhizoma Atractylodis Macrocephalae (parched), Ramulus Cinnamomi extract volatile oil; Radix Salviae Miltiorrhizae, Cortex Eucommiae (parched with salt) are condensed into extractum A with 60～95% alcoholic solution extraction, extracting solution; Medicinal residues after Radix Angelicae Sinensis, Rhizoma Atractylodis Macrocephalae (parched), Ramulus Cinnamomi extracted medicinal residues behind the volatile oil and Radix Salviae Miltiorrhizae, Cortex Eucommiae (parched with salt) alcoholic solution and extract add Semen Persicae (peeled), Sargassum, Herba Scutellariae Barbatae and use water extraction together, and the water intaking extract is condensed into extractum B; Merge extractum A and extractum B and continue to be condensed into thick paste C, the volatile oil of the fine powder of adding Radix Notoginseng, rhizoma sparganic, Rhizoma Curcumae, Carapax Trionycis and Radix Angelicae Sinensis, Rhizoma Atractylodis Macrocephalae (parched), Ramulus Cinnamomi is mixed into medicated powder D, Chinese medicine preparation is made oral formulations routinely, with containing Radix Notoginseng with the ginsenoside Rg among high performance liquid chromatography or the tlc-scanning determination medicated powder D
1Meter must not be less than 1.50mg/g.
2. Chinese patent medicine as claimed in claim 1 is characterized in that said oral formulations is tablet, capsule, pill, granule.
3. one kind as the said hysteromyoma that cures mainly of claim 1, the preparation method of the Chinese patent medicine of inflammatory masses of pelvic cavity, it is characterized in that: (1) gets Radix Notoginseng, rhizoma sparganic, Rhizoma Curcumae, Carapax Trionycis four flavor raw material pulverize separately become fine powder, sieve, standby: (2) get Radix Angelicae Sinensis, Rhizoma Atractylodis Macrocephalae (parched), Ramulus Cinnamomi three flavor raw materials are standby with extracting volatile oil: (3) Radix Salviae Miltiorrhizae, Cortex Eucommiae (parched with salt) two flavor raw materials extract with 60～95% alcoholic solution, filter, extracting solution is condensed in the time of 70～80 ℃ and measures relative density is 1.05～1.25 extractum A, standby, medicinal residues are deposited in addition: (4) are with Radix Angelicae Sinensis, Rhizoma Atractylodis Macrocephalae (parched), Ramulus Cinnamomi extracts medicinal residues and the Radix Salviae Miltiorrhizae behind the volatile oil, medicinal residues after the Cortex Eucommiae (parched with salt) alcoholic solution extracts add Semen Persicae (peeled), Sargassum, Herba Scutellariae Barbatae three flavor raw materials are used water boiling and extraction 1～3 time together, merge the water extract, be condensed into extractum B, merge extractum A and extractum B and continue to be condensed into that to measure relative density in the time of 70～80 ℃ be 1.15～1.30 thick paste C, (5) thick paste C adds Radix Notoginseng, rhizoma sparganic, Rhizoma Curcumae, the fine powder of Carapax Trionycis, mixing, dry, pulverize, add Radix Angelicae Sinensis again, Rhizoma Atractylodis Macrocephalae (parched), the volatile oil of Ramulus Cinnamomi, be mixed into medicated powder D, process of Chinese medicine preparation is made oral formulations routinely.
4. one kind as the said method of quality control that cures mainly the Chinese patent medicine of hysteromyoma, inflammatory masses of pelvic cavity of claim 1, and it is characterized in that: (1) is with containing the ginsenoside Rg among the high effective liquid chromatography for measuring medicated powder D
1Content; (2) measure the content that contains the ginsenoside Rg1 among the medicated powder D with the tlc scanning method.
5. as the said method of quality control of claim 5, it is characterized in that the method for said high performance liquid chromatography is:
Chromatographic condition is filler with the octadecylsilane chemically bonded silica, and with acetonitrile: 4% methanol solution volume ratio is that 18: 82 solution is made mobile phase, and the detection wavelength is 203nm, and column temperature is 35 ℃, and theoretical cam curve is by the ginsenoside Rg
1The peak calculates should be not less than 4000;
The ginsenoside Rg is got in the preparation of reference substance solution
1Reference substance adds mobile phase and makes every 1ml and contain the ginsenoside Rg
10.5mg solution, promptly;
The preparation of the need testing solution powder D 4g that gets it filled puts in the conical flask of tool plug, adds water-saturated n-butanol 50ml, claims to decide weight, close plug, placement is spent the night, supersound process, put coldly, claim again to decide weight, supply the weight that subtracts mistake with water saturated n-butyl alcohol, shake up, filter, precision is measured subsequent filtrate 25ml, put in the separatory funnel,, discard ammonia solution with the ammonia solution washing, the n-butanol layer evaporate to dryness, the accurate water that adds 10ml of residue claims to decide weight, supersound process is disperseed residue, claims to decide weight again, water is supplied the weight that subtracts mistake, shakes up, and filters, precision is measured subsequent filtrate 5ml, puts in the 10ml volumetric flask, and adds mobile phase to scale, shake up, filter with microporous filter membrane, promptly.
6. as the said method of quality control of claim 5, it is characterized in that the method for said tlc scanning is:
The preparation of the need testing solution powder D 4g that gets it filled accurately claims surely, puts in the tool plug conical flask, the accurate water-saturated n-butanol 50ml that adds claims to decide weight, and supersound process claims to decide weight again, add saturated n-butyl alcohol and supply the weight that subtracts mistake, shake up, filter, precision is measured subsequent filtrate 25ml, with the ammonia solution washing, gets n-butyl alcohol liquid evaporate to dryness, residue adds dissolve with methanol and is transferred in the 2ml measuring bottle, add methanol to scale, shake up, as need testing solution;
The preparation precision of reference substance solution takes by weighing the ginsenoside Rg
1Reference substance adds methanol and makes the solution that 1ml contains 1mg, in contrast product solution;
The accurate need testing solution 1 μ l that draws of assay method, reference substance solution 1 μ l, 5 μ l, respectively the cross point in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, with chloroform: methanol: water volume ratio is 13: 7: 2 a solution, and lower floor's solution of placing 12 hours below 10 ℃ is developing solvent, launches below 10 ℃, take out, airing, spray be with 10% ethanol solution of sulfuric acid, and it is clear to be heated to speckle colour developing at 105 ℃, take out, on lamellae, cover onesize glass plate, fixing, scan according to thin layer chromatography, wavelength: go into s=525nm, measure test sample trap integrated value and reference substance trap integrated value, calculate, promptly.
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| CNB2005100364687A CN100376284C (en) | 2005-08-10 | 2005-08-10 | Proprietary Chinese traditional medicine with marked effect in treating hysteromyoma, process for preparing the same and quality controlling method thereof |
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| CN101406552B (en) * | 2008-11-14 | 2011-04-27 | 孙浩峰 | Medicament for treating hysteromyoma and preparation method thereof |
| CN102008680B (en) * | 2010-04-27 | 2011-12-28 | 泰一和浦（北京）中医药研究院有限公司 | Traditional Chinese medicine composition for treating abdominal mass and myoma and preparation method thereof |
| CN104189677A (en) * | 2014-09-20 | 2014-12-10 | 陈远征 | Medicine composition for treating uterine fibroid and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1318411A (en) * | 2001-04-20 | 2001-10-24 | 于子民 | Hysteromyoma capsule |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1318411A (en) * | 2001-04-20 | 2001-10-24 | 于子民 | Hysteromyoma capsule |
Non-Patent Citations (1)
| Title |
|---|
| 举元煎妇科临床应用. 刘胜利.陕西中医，第11卷第10期. 1990 * |
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