CN106110206B

CN106110206B - Traditional Chinese medicine preparation for treating endometriosis and preparation method thereof

Info

Publication number: CN106110206B
Application number: CN201610632470.9A
Authority: CN
Inventors: 靳凤云; 李德鑫; 姚鹏; 韩云霞; 唐秀胜
Original assignee: Guiyang College of Traditional Chinese Medicine
Current assignee: Guiyang College of Traditional Chinese Medicine
Priority date: 2016-08-04
Filing date: 2016-08-04
Publication date: 2021-03-09
Anticipated expiration: 2036-08-04
Also published as: CN106110206A

Abstract

The invention discloses a traditional Chinese medicine preparation for treating endometriosis and a preparation method thereof, wherein the traditional Chinese medicine preparation is prepared from the following raw material medicines in parts by weight: 53-198 parts of dragon's blood, 99-495 parts of rheum officinale, 198-396 parts of dogwood, 198-396 parts of angelica, 198-396 parts of moutan bark, 99-330 parts of elecampane, 99-330 parts of corydalis tuber, 198-396 parts of red paeony root, 293-495 parts of poria cocos, 173-297 parts of curcuma zedoary, 105-990 parts of polygonum perfoliatum, 99-330 parts of cassia twig and 165-330 parts of rhizoma sparganii. The traditional Chinese medicine preparation for treating endometriosis disclosed by the invention has the effects of activating blood circulation to dissipate blood stasis, tonifying kidney to arrest desertion, eliminating blotch and dispersing mass, and dredging collaterals to relieve pain, and has a good effect of treating endometriosis. The preparation process is simple, feasible and stable, the preparation conditions are mild and easy to control, the operation is simple, and the large-scale production is easy to realize.

Description

Traditional Chinese medicine preparation for treating endometriosis and preparation method thereof

Technical Field

The invention relates to a traditional Chinese medicine preparation for treating endometriosis and a preparation method thereof, belonging to the technical field of traditional Chinese medicines.

Background

Endometriosis is a gynecological disease in which endometrium with growth function covers other parts of body except uterine cavity and has recurrent and periodic bleeding. The ectopic intima can also produce obvious changes along with the change of estrogen level in function, and not only is surrounded by the glandular organ of the intima, but also is surrounded by the mesenchyme of the intima. Endometriosis mainly occurs in pelvic organs, cervical, vaginal, perineum and abdominal incisions, has strong transformation and growth capacity, and is a common gynecological disease. The common diseases of the female of childbearing age are usually seen in the female of childbearing age, and the incidence rate of the diseases is rapidly increased in recent years, wherein the number of the women of childbearing age is more than 10%, and the recurrence rate is extremely high. The clinical manifestations of the internal diseases are not necessarily strongly correlated with the degree of pathological changes, but may be severe when the pathological changes are mild or local, or severe when the pathological changes are large or even the pelvic anatomy is severely deformed. Statistically, about 70% of patients with endometriosis have typical clinical manifestations of secondary dysmenorrhea, menstrual changes, dyspareunia and infertility. When the endogenous disorder occurs in other specific sites, the resulting clinical manifestations may not be consistent with the disorder. The main symptom of most patients is secondary dysmenorrhea, which is often accompanied by progressive pain in the lower abdomen and back, and can be radiated to the legs. Pain usually begins two days before menstruation. When ectopic intimal bleeding occurs, the peak of menstruation is reached. Most patients experience pain relief during the menstrual period. However, in advanced patients, particularly in the pelvic cavity, there is widespread adhesions and pain persists. The typical age of patients with secondary dysmenorrhea is between 30 and 45 years. The focus of which can lead to retroversion of the uterus in patients. The longer the patient is affected, the more marked are symptoms of feelings of sexual disorder, dyspareunia, and the like, and endometriosis is associated with about one third of infertility of unknown origin. The infertility rate of patients with this condition is also as high as 40%. Changes in anatomy may be one of the causes of late stage severe patient infertility. The reasons of infertility of mild patients are greatly related to microenvironment factors in abdominal cavities, ovarian dysfunction and the like.

There is no record of endometriosis in the ancient literature of traditional Chinese medicine, but according to the main clinical manifestations of endometriosis, it can be ascribed to dysmenorrheal, abdominal mass, irregular menstruation and sterility. According to the research of traditional Chinese medicine gynecology on more systems of internal diseases in recent decades, the basic pathogenesis of the internal diseases is that blood stasis blocks uterus and any stroke is considered, and factors such as viscera function, blood and qi disorder, exogenous pathogenic factor invasion and the like are related to the formation of stasis. The diagnosis and treatment of "internal abnormal symptoms" in traditional Chinese medicine are based on syndrome differentiation as the fundamental feature, and the traditional Chinese medicine holds that the main syndrome of "internal abnormal symptoms" is blood stasis syndrome and runs through the whole process of the disease. In the early stage of the disease, excess syndrome is the main cause, and the disease damages the body resistance for a long time, and deficiency is caused by excess, and pure deficiency syndrome is rarely seen, which is mainly manifested as deficiency-excess mixed syndrome. For those with excess, dysmenorrhea before menstruation, severe pain during menstrual period and tenderness. Dysmenorrhea during menstrual period with intermingled deficiency and excess, and slightly mild pain after menstruation. Cold pain and colic caused by cold and stasis, and pain relieved by heat; burning pain, which is aggravated by heat, is caused by heat-induced stasis; distending and falling pain due to qi stagnation; stabbing pain is caused by severe blood stasis. For blood stasis due to qi stagnation or cold accumulation, the menstruation volume is small, the color is purple and dark, and there is blood clot. The blood stasis due to heat or damp-heat has a profuse menstruation volume, dark red color, thick texture and blood clots. The patients with qi deficiency and blood stasis also have more or less menstruation, dark color and thin and blood-stained blood clots. The syndrome is generally classified into qi stagnation and blood stasis syndrome, congealing cold and blood stasis syndrome, kidney deficiency and blood stasis syndrome, damp heat and blood stasis syndrome and the like through the dialectical symptoms of the traditional Chinese medicine.

The traditional Chinese medicine has unique advantages in treating endometriosis, especially the research pace of modern medicine on endometriosis is accelerated in recent decades, the knowledge and exploration of traditional Chinese medicine on endometriosis are deepened step by step, single curative effect is observed on symptoms, and in recent years, the effect of the traditional Chinese medicine on endometriosis is observed from microscopic indexes, so that an effective and appropriate traditional Chinese medicine treatment method is screened objectively. The traditional Chinese medicine not only plays a role in treating endometriosis, but also can better regulate multiple aspects of endocrine, immunity and the like of an organism. Therefore, the medicine is prepared by selecting the traditional Chinese medicine and adopting the modern preferred extraction process and preparation process, a new traditional Chinese medicine variety with a definite curative effect is provided for the treatment of endometriosis, and a new treatment medicine is provided for the patient.

Disclosure of Invention

In order to solve the defects of the prior art, the invention aims to provide a traditional Chinese medicine preparation for treating endometriosis and a preparation method thereof. The traditional Chinese medicine preparation for treating endometriosis provided by the invention has a good effect of treating endometriosis, and the preparation process is simple, feasible and stable.

In order to achieve the above object, the present invention adopts the following technical solutions:

a traditional Chinese medicine preparation for treating endometriosis is prepared from the following raw material medicines in parts by weight: 53-198 parts of dragon's blood, 99-495 parts of rheum officinale, 198-396 parts of dogwood, 198-396 parts of angelica, 198-396 parts of moutan bark, 99-330 parts of elecampane, 99-330 parts of corydalis tuber, 198-396 parts of red paeony root, 293-495 parts of poria cocos, 173-297 parts of curcuma zedoary, 105-990 parts of polygonum perfoliatum, 99-330 parts of cassia twig and 165-330 parts of rhizoma sparganii.

Further, the traditional Chinese medicine preparation for treating endometriosis is prepared from the following raw material medicines in parts by weight: 103 parts of dragon's blood, 412 parts of rhubarb, 343 parts of dogwood, 275 parts of angelica, 275 parts of tree peony bark, 175 parts of costustoot, 257 parts of corydalis tuber, 223 parts of red paeony root, 343 parts of tuckahoe, 223 parts of zedoary, 155 parts of polygonum perfoliatum, 223 parts of cassia twig and 223 parts of rhizoma sparganii.

The preparation is prepared into granules by using soluble starch as an excipient, 0.2 percent of aspartame as a flavoring agent and 90 percent of ethanol as a wetting agent.

The preparation method of the traditional Chinese medicine preparation for treating endometriosis comprises the following steps: weighing herba Polygoni Cymosi, Corni fructus, rhizoma corydalis and radix et rhizoma Rhei according to certain amount, adding ethanol, reflux extracting, and filtering to obtain ethanol extractive solution; weighing sanguis Draxonis, radix Angelicae sinensis, cortex moutan, radix aucklandiae, radix Paeoniae Rubra, Poria, Curcumae rhizoma, ramulus Cinnamomi and rhizoma Sparganii, adding water, decocting, filtering to obtain water extractive solution, concentrating under reduced pressure to obtain concentrated water extractive solution, adding ethanol, stirring, standing, removing precipitate to obtain supernatant of ethanol precipitation; mixing the ethanol extractive solution and the supernatant, concentrating under reduced pressure to obtain concentrated solution, vacuum drying the concentrated solution to obtain extract, pulverizing, sieving to obtain medicinal powder, adding adjuvants, and making into various preparations.

Specifically, the preparation method of the traditional Chinese medicine preparation for treating endometriosis comprises the following steps: weighing the polygonum perfoliatum, the dogwood, the corydalis tuber and the rhubarb according to the amount, adding 60-80% ethanol in an amount which is 6-10 times that of the polygonum perfoliatum, performing reflux extraction for 1-3 times, and filtering for 1-2 hours each time to obtain an ethanol extract for later use; weighing dragon's blood, Chinese angelica, tree peony bark, costustoot, red paeony root, Indian buead, zedoary, cassia twig and common burreed rhizome according to the amount, adding 6-10 times of water, decocting and extracting for 1-3 times, each time for 1-2 hours, filtering to obtain water extract, concentrating at 75 ℃ under reduced pressure until the density is 1.05 to obtain concentrated water extract, adding ethanol, uniformly stirring, controlling the concentration of the ethanol in the material liquid to be 40-60%, standing for 12 hours, removing precipitate to obtain ethanol precipitation supernatant for later use; mixing the ethanol extractive solution and the supernatant, concentrating under reduced pressure at 75 deg.C to density of 1.25 to obtain concentrated solution, vacuum drying at 60-80 deg.C for 72-42 h to obtain extract, pulverizing, sieving with No. 5 sieve to obtain medicinal powder, and adding adjuvants to make into various preparations.

Preferably, the preparation method of the traditional Chinese medicine preparation for treating endometriosis comprises the following steps: weighing herba Polygoni Cymosi, Corni fructus, rhizoma corydalis and radix et rhizoma Rhei, adding 9 times and 8 times of 80% ethanol respectively, reflux extracting for 2 times, each for 1 hr, and filtering to obtain ethanol extractive solution; weighing sanguis Draxonis, radix Angelicae sinensis, cortex moutan, radix aucklandiae, radix Paeoniae Rubra, Poria, Curcumae rhizoma, ramulus Cinnamomi and rhizoma Sparganii, adding 7 times and 6 times of water, decocting and extracting for 2 times, each time for 1 hr, filtering to obtain water extractive solution, concentrating at 75 deg.C under reduced pressure to density of 1.05 to obtain concentrated water extractive solution, adding ethanol, stirring, controlling ethanol concentration in the material liquid to 60%, standing for 12 hr, discarding precipitate to obtain ethanol precipitation supernatant; mixing the ethanol extractive solution and the supernatant, concentrating under reduced pressure at 75 deg.C to density of 1.25 to obtain concentrated solution, vacuum drying the concentrated solution at 70 deg.C for 60 hr to obtain extract, pulverizing, sieving with No. 5 sieve to obtain medicinal powder, adding adjuvants, and making into various preparations.

Further, the preparation method of the traditional Chinese medicine preparation for treating endometriosis comprises the steps of adding soluble starch into the medicinal powder according to the mass ratio of 1:1, using aspartame accounting for 0.2% of the total mass of the medicinal powder as a flavoring agent and 90% ethanol as a wetting agent for granulation, drying the granules at the temperature of 60-80 ℃, carrying out secondary granulation, sieving to remove large granules and removing fine powder, and obtaining the granules.

More specifically, the preparation method of the traditional Chinese medicine preparation for treating endometriosis comprises the steps of adding soluble starch into medicinal powder according to the mass ratio of 1:1, using aspartame accounting for 0.2% of the total mass of the medicinal powder as a flavoring agent and 90% ethanol as a wetting agent for granulation, gradually heating the granules at 60-80 ℃, drying, carrying out secondary granulation, sieving by a No. 1 sieve to remove large granules, and sieving by a No. 5 sieve to remove fine powder to obtain the granules.

The traditional Chinese medicine preparation for treating endometriosis takes polygonum perfoliatum and dragon's blood as monarch drugs, cortex moutan radicis, rhizoma corydalis and red paeony root as ministerial drugs, rhubarb, dogwood, costustoot, rhizoma zedoariae and rhizoma sparganii as adjuvant drugs, and angelica, cassia twig and poria cocos as conductant drugs.

In order to ensure the science, the reasonability and the feasibility of the scheme of the invention, the scheme of the invention is determined by carrying out a series of experimental researches and examinations.

Firstly, the raw material medicines are selected:

1. dragon's blood has sweet taste, salty taste and no toxicity, and has the functions of promoting blood circulation to disperse blood clots, relieving pain, arresting bleeding, promoting granulation and healing wound. Wherein the resin content is about 57.5%, and is flavonoid derivative. In recent years, many studies have been made on chemical components thereof. 6 fat-soluble compounds were isolated and identified in the study of their fat-soluble components. It has effects in promoting blood circulation, dispelling blood stasis, stopping bleeding, astringing, regulating, relieving inflammation and pain, and inhibiting bacteria.

2. Rhizoma sparganii is bitter in taste and neutral in nature, enters liver and spleen channels, has the effects of breaking blood and promoting qi circulation, removing food retention and relieving pain and the like, and is a commonly used traditional Chinese medicine for promoting blood circulation and removing blood stasis. Volatile oil, organic acid, steroid, flavonoid, phenylpropanoid and the like are main chemical components. Has effects in resisting platelet aggregation and thrombosis, influencing blood rheological property, and relieving pain.

3. Herba Polygoni Cymosi is aerial part of herba Polygoni Cymosi of Polygonaceae, also named as herba Polygoni Cymosi, herba Serpentis, herba seu radix Nothopanacis Delavayi, herba Damnacanthi, and herba Violae Japonicae, and is a perennial sprawl herb distributed all over the country with abundant resources. It is recorded in the section of pharmacopoeia of the people's republic of China (2010 edition) beginning in Wan Bingchun (Wan Bing Hui Chun). The medicine is sour, bitter and mild in nature, has the effects of clearing heat and removing toxicity, killing parasites and relieving itching, dispelling wind and arresting cough, and inducing diuresis to alleviate edema, is widely used for treating edema, jaundice, malaria, dysentery, pertussis, ulcer, erysipelas, eczema, herpes, mange, venomous snake bite and the like in folk, and has definite curative effect. Separating and identifying beta-sitosterol, trans-methyl p-hydroxycinnamate, quercetin-3-O-beta-D-glucoside, emodin, physcion, aloe-emodin and other compounds in the polygonum perfoliatum root. Contains phenols, organic acids, alkaloids, amino acids, tannin, flavone, anthraquinone, glycosides, saccharides, phytosterols, and triterpenes. The perfoliote knotweed herb medicinal material identifies flavonoids compounds such as kaempferol, quercetin, imporoside, quercetin-3-O-beta-D-glucuronic acid methyl ester, quercetin-3-beta-D-glucuronic acid n-butyl ester, kaempferol-3-O-rutinoside, rutin and the like. Herba Polygoni Cymosi has antiinflammatory, antibacterial, antitussive, expectorant, and antiviral effects.

4. The radix et rhizoma Rhei is dried root and rhizome of Rheum palmatum L, Rheum tanguticum Maxim. ex Balf. or Rheum officinale Baill. of Polygonaceae. The Chinese medicine rhubarb is one of Chinese special medicines, is bitter in taste and cold in nature, enters stomach, spleen, large intestine, liver and pericardium channels, and has the effects of purging heat, dredging intestine, cooling blood, removing toxicity, removing blood stasis, dredging channels and the like. The book of Shen nong Ben Cao Jing (Shen nong's herbal) has a main expression: 'Xieyu Xue, blood blocking cold and heat, breaking mass, staying food and drink, cleaning intestines and stomach, pushing old to cause novelty, smoothing water and removing food, regulating middle energizer and harmonizing five internal organs'. Compendium of materia Medica: "dysentery with reddish white stool, tenesmus and abdominal pain, dribbling urine, excess heat and dryness, tidal fever peaceful, jaundice, and various sores due to pathogenic fire". Anthraquinone derivatives are the main active ingredients in rhubarb. The anthraquinone derivatives include anthrone Emodin (Emodin), Rhein (Rhein), chrysophanol (Chrysophano1), Physcion (Physcion), Aloe-Emodin (Aloe-Emodin) and rhapontin (Chrysaron); the radix et rhizoma Rhei also contains glycosides and anthrones combined with glucose of anthraquinone derivatives, such as Sennoside A, B, C, D, E, F, etc., and other glycosides, tannin, polysaccharide compounds, organic compounds and inorganic substances. Radix et rhizoma Rhei has effects in stopping bleeding, reducing blood lipid, clearing away heat and toxic materials, resisting bacteria, relieving inflammation, protecting liver, and promoting bile flow.

5. Chinese angelica is a commonly used Chinese medicinal material with the functions of tonifying and regulating blood, regulating menstruation, stopping bleeding, moistening intestines and smoothing intestines. Can be used for treating blood deficiency, sallow complexion, giddiness, palpitation, menoxenia, amenorrhea, dysmenorrhea, abdominal pain due to deficiency cold, constipation due to intestinal dryness, and rheumatalgia. The research shows that the medicine contains various effective components such as volatile oil, polysaccharide and the like.

6. Zedoary is a common Chinese medicine with warm nature and pungent taste, and has the effects of promoting qi circulation, removing blood stasis, resolving food stagnation and relieving pain. Can be used for treating amenorrhea due to blood stasis, food stagnation, and abdominal distention. The research shows that the medicine has better functions of resisting tumor, thrombus, inflammation, virus, early pregnancy, bacteria, liver and fibrous tissue hyperplasia, etc. Is a clinically common medicament for promoting blood circulation and removing blood stasis. The active component of the medicine is volatile oil, and the modern pharmacological research shows that the medicine has better pharmacological effects of resisting tumor, thrombus, inflammation, virus, early pregnancy, bacteria, liver, psoriasis, fibrous tissue hyperplasia and the like.

7. Poria is a kind of fungus Chinese medicine. Sweet and bland in flavor. It enters heart, lung and kidney meridians. The modern pharmacological research proves that the traditional Chinese medicine composition has the effects of promoting urination, regulating immunity, tranquilizing, resisting tumors, protecting the liver and the like, is clinically used for treating symptoms such as edema, oliguria, phlegm and fluid retention, dizziness and palpitation, spleen deficiency, poor appetite, loose stool, diarrhea, uneasiness and the like, and is widely applied.

8. Cassia twig, recorded in Shen nong Ben Cao Jing for the earliest time, comes from Xin Xiu Ben Cao, has warm nature, pungent and sweet taste and twelve regular meridians. It has effects of inducing sweat to relieve exterior syndrome, supporting yang to regulate qi-flowing, and inducing sweat to relieve exterior syndrome, and contains volatile oil, benzyl formate, carnyl acetate, coumarin, and calamene. Has antiviral, antibacterial, antipyretic, analgesic, antiinflammatory, and antiallergic effects.

9. The cortex moutan is root bark of Paeonia suffruticosa Andr (Paenoina suffruticosa Andr) belonging to Paeonia of Ranunculaceae. Slightly cold in nature, bitter and pungent in flavor. It enters heart, liver and kidney meridians. Cortex moutan contains more components, and the main components include phenol and phenol glycosides, monoterpene and its glycosides, and triterpene, sterol and its glycosides, flavone, organic acid, coumarin, etc. The phenol and phenolic glycosides in cortex moutan are compounds with high content, and the phenol and phenolic glycosides separated from cortex moutan include paeonol, paeonol glycoside, paeonoloside, and paeonol neoside. It has effects in resisting atherosclerosis, lowering blood pressure, lowering blood sugar, relieving convulsion, regulating urinary system, regulating immunocyte, and resisting bacteria and inflammation.

10. Corni fructus has effects of invigorating liver and kidney, and arresting seminal emission, and can be used for treating giddiness, tinnitus, soreness of waist and knees, sexual impotence, nocturnal emission, enuresis, pollakisuria, leucorrhea hemorrhage, sweating, internal heat, diabetes, etc. Iridoid glycosides, pentacyclic triterpenic acid and esters, tannins and polysaccharides are main chemical components. Has effects in lowering blood sugar, inhibiting bacteria, relieving inflammation, and regulating immune system.

11. Corydalis tuber is pungent and bitter in flavor and warm in nature, and enters liver and spleen meridians; has effects in promoting blood circulation, activating qi-flowing, and relieving pain. The main chemical components are isoquinoline type alkaloids which are divided into two types according to the solubility in water, and the tertiary amine base is almost insoluble or insoluble in water; quaternary ammonium bases are more soluble in water. So far, more than 40 kinds of compounds have been separated from the raw materials and subjected to structural identification, and the compounds belong to protoberberine, apophenanthrene, protopine, isoquinoline benzimidazole, isoquinoline benzophenanthridine, bis-benzyl isoquinoline and the like. Has the functions of promoting blood circulation to disperse blood clots, promoting qi circulation to arrest pain, and has excellent pain relieving, tranquilizing, blood pressure lowering and arrhythmia resisting effects. Has effects in promoting blood circulation, activating qi-flowing, and relieving pain; has obvious protective effect on pyloric ligation and aspirin induced gastric ulcer, and can effectively inhibit gastric secretion; the total alkaloids also have protective effect on ischemic myocardium.

12. Radix Paeoniae Rubra is dry root of Paeonia lactiflora pall or Paeonia veitchii Lynch of Paeoniaceae, and has bitter taste, cold property, and liver meridian entered effect, and has effects of clearing heat, cooling blood, removing blood stasis, and relieving pain. Can be used for treating macula due to toxic heat, hematemesis, epistaxis, conjunctival congestion, swelling and pain, liver depression, hypochondriac pain, amenorrhea, dysmenorrhea, abdominal pain, traumatic injury, carbuncle, swelling, and pyocutaneous disease. The main effective components of radix Paeoniae Rubra mainly include glycosides represented by paeoniflorin, including paeoniflorin (paeoniflorin), oxypaeoniflorin (oxy-paeoniflorin), etc. It also contains dextro-catechuin (catechin) and volatile oil. Benzoic acid (benzoic acid) is the main component of the volatile oil, and 33 paeonol (paeonol) and other alcohol and phenol components are contained. Has antithrombotic, platelet aggregation inhibiting, blood lipid reducing, and arteriosclerosis resisting effects.

13. Radix aucklandiae enters spleen; the stomach; liver; the lung meridian is pungent and pungent; bitter; and (4) temperature. Has effects in regulating qi-flowing, eliminating dampness, eliminating phlegm, promoting qi circulation, and relieving pain; to regulate the middle energizer and remove food stagnation. Hypochondriac distention in the main cell is satisfied; abdominal distending pain; vomiting and diarrhea; severe after dysentery. Can be used for treating chest and abdominal pain, dysentery, diarrhea, dyspepsia, anorexia, and antibacterial effect. The pungent, warm and fragrant powder can ascend and descend, regulate qi of triple energizer, especially promote qi circulation of stomach and intestine to alleviate pain, and has the actions of invigorating spleen to promote digestion, so it is commonly used for all syndromes caused by qi stagnation of spleen, stomach and large intestine.

Secondly, determination of preparation process

1 decoction piece source

The decoction pieces are purchased from Guizhou Jiren Tang pharmaceutical industry Co., Ltd, and are identified to meet the relevant regulations of each medicinal material (decoction piece) item in the first part of the 2010 edition of Chinese pharmacopoeia and the 2003 edition of quality standards of Chinese medicinal materials and national medicinal materials in Guizhou province.

2 Process route determination, optimization

2.1 determination of extraction method

The extraction method of the traditional Chinese medicine preparation for treating endometriosis is designed according to the chemical component properties and modern pharmacological research of each medicine in a prescription and by combining factors such as industrial production practice and the like.

Dragon's blood contains very complicated chemical components. According to the structure of phenolic compounds, they can be roughly classified into polymers of chalcones, 2-hydrochalcone, flavanones, flavones, chromones, flavones and other phenolic compounds. 21 steroids and triterpenoids are separated at present. Other structural types of compounds exist, such as phenols, steroid saponins, and the like, as follows: alkanes, acids, esters, and the like. From the research summary about the chemical components, the main component of dragon's blood is phenolic compound, and the main part is flavonoid compound. According to the main function of the recipe, some of the ingredients are extracted by water extraction and alcohol precipitation.

The chemical components in rhizoma Sparganii mainly include volatile oil, organic acids, steroids, flavonoids, phenylpropanoids, etc. In recent years, new components and new activities have been discovered. At present, the total flavonoids have been proved to have the effects of resisting platelet aggregation, resisting thrombus and relieving pain. Can be extracted by water extraction and alcohol precipitation.

The herba Polygoni Cymosi chemical components include phenols, organic acids, alkaloids, amino acids, tannin, flavone, anthraquinone, glycosides, saccharides, phytosterol and triterpenes. Separating and identifying compounds such as beta-sitosterol, trans-methyl p-hydroxycinnamate, quercetin-3-O-beta-D-glucoside, emodin, physcion, aloe-emodin and the like in roots. The medicinal materials identify flavonoids such as kaempferol, quercetin, impoverine, quercetin-3-O-beta-D-glucuronic acid methyl ester, quercetin-3-beta-D-glucuronic acid n-butyl ester, kaempferol-3-O-rutinoside, rutin and the like. The effective components can be extracted to the maximum extent by ethanol extraction.

The main active component in the rhubarb is anthraquinone derivatives. The anthraquinone derivatives include anthrone emodin, rhein, chrysophanol, physcion, aloe-emodin, and rhapontigenin; the radix et rhizoma Rhei also contains glycosides and anthrones combined with glucose, such as sennosides A, B, C, D, E, F, etc., and other glycosides, tannin, polysaccharide compounds, organic compounds and inorganic substances, etc. The effective components can be extracted to the maximum extent by ethanol extraction.

The main pharmacological active ingredients in the angelica are volatile oil, polysaccharide and the like. Also contains sucrose, fructose, and glucose; vitamin a, vitamin B12, vitamin E; 17 amino acids, and more than 20 inorganic elements such as sodium, potassium, calcium, magnesium, etc. According to the main function of the recipe, some of the ingredients are extracted by water extraction and alcohol precipitation.

The active component of the zedoary is volatile oil with the content of 1.9-2.5 percent. In recent years, the components in the volatile oil are researched, and the main chemical components in the oil are various sesquiterpene substances. Also contains various trace elements such as zinc, iron, nickel, manganese, magnesium, cadmium, copper, molybdenum, cobalt, vanadium, phosphorus, calcium, gallium and the like. Can be extracted by water extraction and alcohol precipitation.

Poria contains polysaccharide (about 9.3% of dry weight) and triterpenes. Fatty acids such as caprylic acid, undecanoic acid, lauric acid, and palmitic acid are also included. In addition, ergosterol, gum, chitin, protein, fat, sterol, lecithin, D-glucose, adenine, histidine, choline, lipase, protease, etc. are included. According to the main function of the recipe, some of the ingredients are extracted by water extraction and alcohol precipitation.

The ramulus Cinnamomi contains volatile oil as main active component, with volatile oil content of 0.6%, benzyl formate, carnyl acetate, coumarin, and calamene. Can be extracted by water extraction and alcohol precipitation.

The components separated from cortex moutan are complex, but mainly comprise phenol and phenol glycosides, monoterpene and its glycosides, and also triterpene, sterol and its glycosides, flavone, organic acid, coumarin, etc. The content of phenol and phenolic glycoside compounds in cortex moutan is high, and the phenol and phenolic glycoside compounds separated from cortex moutan include paeonol, paeonol glycoside, paeonoloside, and paeonol neogenin. Can be extracted by water extraction and alcohol precipitation.

The main chemical components of Corni fructus are iridoid glycosides, pentacyclic triterpenic acid and its esters, tannins, and polysaccharides. The volatile components of the paint are as follows: palmitic acid, isobutanol, isoamyl alcohol, elemene, furfural, methyl eugenol, isoasarone, beta-phenethyl alcohol and the like. Glycosides and aglycones include: verbascoside, morroniside, swertiamarin, loganin, iridoid, glucose, fructose and sucrose. The effective components can be extracted to the maximum extent by ethanol extraction.

The main chemical components of the corydalis tuber are isoquinoline type alkaloids which can be divided into two types according to the solubility of the alkaloids in water, and the tertiary amine base is almost insoluble or hardly soluble in water; more water soluble quaternary ammonium bases. So far, more than 40 types of the existing ones are separated from the raw materials and subjected to structure identification, and the types of the existing ones respectively belong to protoberberine, apophenanthrene, protoopioid, isoquinoline benzimidazole, isoquinoline benzophenanthridine, bis-benzyl isoquinoline and the like. The effective components can be extracted to the maximum extent by ethanol extraction.

The main effective components of radix Paeoniae Rubra are glycosides represented by paeoniflorin, including paeoniflorin, oxidized paeoniflorin, etc. And contains dextro-catechin and volatile oil. The volatile oil mainly contains 33 of benzoic acid, paeonol and other alcohol and phenol components. Can be extracted by water extraction and alcohol precipitation, and the method is mature.

The oleum Linderae contains lactone chemical components 50%. Can be extracted by water extraction and alcohol precipitation.

2.2 Process route determination

According to the chemical component properties of each medicinal material in the prescription, combining the prescription functional indication and the analysis result of the extraction method, the medicinal materials of polygonum perfoliatum, dogwood, corydalis tuber and rhubarb in the prescription are extracted by adding ethanol and filtered to obtain ethanol extract for later use. Extracting the other 9 medicines in the prescription with water, filtering to obtain water extract, concentrating to obtain concentrated water extract, adding appropriate amount of ethanol for precipitation, removing precipitate to obtain supernatant of ethanol precipitation, and keeping. Mixing the ethanol extractive solution with the supernatant, and concentrating to obtain concentrated solution (recovering ethanol). Drying the concentrated solution to obtain extract, pulverizing, and sieving. Adding adjuvants, granulating, and grading. The process route is drawn as shown in fig. 1.

2.3 optimization of alcohol extraction Process conditions

2.3.1 investigation of the alcohol absorption Rate of the drug

Weighing three medicinal materials according to a prescription proportion, namely 4.5g of polygonum perfoliatum, 10g of dogwood, 7.5g of corydalis tuber and 12g of rhubarb, totaling 34g, adding 5 times of ethanol for soaking, observing the soaking condition every 30min until the medicine core is soaked, and obtaining the wet weight result according to the following formula, wherein the results are shown in table 1:

TABLE 1 investigation of alcohol absorption Rate of medicinal materials

As can be seen from table 1, when alcohol extraction is performed for the first time, 108% of alcohol absorption of the medicinal materials should be complemented, and for convenience of production calculation, when alcohol extraction is performed for the first time, one more time of ethanol is added to all alcohol-extracted medicinal materials, which is not much different from the ethanol to be added in the theoretical alcohol absorption, so that it is reasonable to add one more time of ethanol during alcohol extraction for the first time.

2.3.2 preference of ethanol concentration and other factors

(1) The preferred ethanol concentrations are as follows according to the quercetin component in polygonum perfoliatum: 80%, 70%, 60% for the screening.

(2) The extraction time is preferably considered in large-scale production, if the extraction time is too short, the effective components are difficult to extract completely, and if the extraction time is too long, the cost is increased, and the time is wasted, so the extraction time is selected to be three levels of 1h, 1.5h and 2 h.

(3) The extraction times are preferably selected according to a conventional method, and are respectively examined once, twice and three times.

(4) The solvent dosage is preferably 4 medicinal material decoction pieces, the medicinal materials can be immersed by adding 5 times of solvent, the solvent is wasted and the cost is increased due to too large amount of the solvent, and the solvent dosage is selected to be 6 times, 8 times and 10 times for investigation by considering the alcohol absorption rate of the medicinal materials.

2.3.3 methods and results

(1) The method is to find the optimal process conditions for ethanol extraction of herba Polygoni Cymosi, rhizoma corydalis and other 4 medicinal materials, and uses an orthogonal test table L9 (3)⁴) Orthogonal experiments were performed to determine the optimal ethanol extraction conditions. The orthogonal experimental table is shown in table 2.

TABLE 2L 9 (3)⁴) Orthogonality test factors and levels

The preparation of the sample solution takes 17g of medicinal materials with half prescription amount, an orthogonal table is selected according to a test scheme designed by the orthogonal table, and the obtained alcohol extract is filtered and concentrated to 100mL to obtain the product.

The selection of the index components takes quercetin and cream yield in polygonum perfoliatum as the index components, and the optimal extraction process of alcohol extraction is preferred.

Preparation of reference substance solution A proper amount of quercetin reference substance is precisely weighed, and methanol is added to prepare a solution containing 0.09mg of quercetin per 1 mL.

Preparing a sample solution, precisely weighing 10mL of a sample under the item of 'preparation of the sample solution', placing the sample in a beaker to volatilize, precisely adding 50mL of methanol, namely 4:1 hydrochloric acid solution, weighing, extracting in a water bath at 90 ℃ under reflux for 1h, cooling, weighing again, complementing the weight loss by using methanol, shaking up, filtering, and taking a subsequent filtrate to obtain the product.

The method comprises precisely measuring sample solution under the item of 'preparation of sample solution' of 50mL, concentrating to certain density, evaporating to dryness in water bath in an evaporation dish with constant weight, drying at 105 deg.C for 3h to constant weight, cooling in a drier for 30min, rapidly and precisely weighing its mass, and calculating to obtain dry extract rate.

W50mL weight of extract of 50mL sample solution

Total volume of sample

W medicinal materials with the weight of the medicinal materials

(2) Measurement result of Quercetin content

Chromatographic conditions Agela promosil C18(250 mm. times.4.6, 5 μm); methanol-0.4% phosphoric acid water solution 50:50 is taken as a mobile phase; the detection wavelength is 360 nm; flow rate: 1.0 mL/min; column temperature: 30 ℃; calculated by the theoretical plate number of the quercetin, is not less than 3000. As shown in fig. 2, 3 and 4.

And precisely weighing a proper amount of quercetin reference substance according to the standard curve, adding methanol to dissolve the quercetin reference substance to prepare a reference substance solution with the mass concentration of 90 mu g/mL, and injecting the reference substance solution into HPLC for determination according to a proposed chromatographic condition. The sample volume of quercetin is 0.1 μ L, 0.3 μ L, 0.5 μ L, 1 μ L, and 2 μ L, respectively. And performing linear regression on the sample introduction mass by using the peak area to obtain a regression equation, a correlation coefficient and a linear range of each measured component. The results are shown in table 3 and fig. 5: the mass concentration of the quercetin is in a good linear relation within the range of 0.009-0.180 mug.

TABLE 3

(3) Orthogonal experimental design and results

Weighing half the prescription amount of 17g, and mixing according to L9 (3)⁴) Orthogonal test conditions are respectively extracted, filtered and primarily concentrated to a certain amount to obtain test solution. Takes the content of quercetin and the cream collecting rate as indexesThe best process is obtained by using a comprehensive evaluation (comprehensive evaluation: quercetin content/maximum quercetin content x 80-cream collecting rate/maximum cream collecting rate x 20) as an index. The results are shown in tables 4, 5 and 6.

TABLE 4 results of orthogonal experiments

TABLE 5 analysis of variance in orthogonal tests

TABLE 6 results of comprehensive scoring in orthogonal experiments

As can be seen from the results of the orthogonal experiments in the table, the order of the alcohol extraction process influenced by various factors is extraction times > ethanol concentration > ethanol dosage > extraction time, wherein the extraction times C and the ethanol concentration a have significant (P <0.05) influence, so that according to the results of the orthogonal experiments, the extraction times C are selected from C2 optimally, and the ethanol concentration a is selected from A3 optimally; the ethanol dosage B and the extraction time D have no significant difference, and the optimal process condition is A3B2C2D1 in combination with mass production. The preparation method comprises extracting with 8 times of 80% ethanol solution for 2 times, each for 1 hr.

2.3.4 validation test

A total of 17g of half the prescribed amount of the drug materials were weighed out and subjected to a verification test according to the best protocol A3B2C2D1, as shown in Table 7, the results were consistent with the results of the orthogonal test. The process is stable and feasible. Therefore, the alcohol extraction process is determined as follows: reflux-extracting with 8 times of 80% ethanol solution for 2 times, each for 1 hr.

TABLE 7 alcohol extraction Process verification results

2.4 Water extraction Condition Process optimization

2.4.1 investigation of Water absorption of medicinal materials

Weighing three medicinal materials according to the proportion of a prescription, namely 8g of tree peony bark, 10g of tuckahoe, 6.5g of cassia twig, 8g of angelica, 6.5g of rhizoma sparganii, 6.5g of rhizoma zedoariae, 6.5g of red paeony root, 8g of costustoot and 3g of dragon's blood, adding 7 times of water for soaking, observing the soaking condition every 30min until the medicine core is soaked, and obtaining the wet weight result according to the following formula, wherein the results are shown in table 8:

TABLE 8 investigation of Water absorption of medicinal materials

As can be seen from Table 8, the water absorption of 102% of the crude drugs should be supplemented during the first water extraction, and for the convenience of production calculation, the water is added twice more than the total water-extracted crude drugs during the first water extraction, which is not much different from the water phase added by the theoretical water absorption, so that the water is reasonably added twice more during the first water extraction.

2.4.2 optimization of Water extraction factor levels

(1) Adding water into 9 medicinal material decoction pieces, and adding 5 times of water to immerse the medicinal materials, considering water absorption rate of the medicinal materials, so selecting water addition amount of 6 times, 8 times and 10 times.

2.4.3 methods and results

(1) The method is to find out the optimal process conditions for water extraction of 9 medicinal materials such as sanguis Draxonis, ramulus Cinnamomi, etc., and to use the orthogonal test table L9 (3)⁴) Orthogonal experiments were performed to determine the optimal water extraction conditions, as shown in table 9.

TABLE 9L 9 (3)⁴) Orthogonality test factors and levels

The preparation of the sample solution takes 31.5g of medicinal materials with half prescription amount, an orthogonal table is selected according to a test scheme designed by the orthogonal table, and the obtained water extract is filtered and concentrated to 100mL to obtain the product.

The selection of the index components takes paeoniflorin and the extraction rate of radix paeoniae rubra as indexes, and the optimal extraction process of water extraction is preferred.

Preparation of control solution A proper amount of paeoniflorin control is precisely weighed, and methanol is added to prepare solutions containing 257 mug of paeoniflorin per 1ml, respectively.

Precisely weighing 10mL of sample under the item of 'preparation of sample solution' for preparing test solution, placing in a beaker to volatilize, precisely adding 25mL of methanol solution, weighing, ultrasonically treating for 30min, cooling, weighing again, supplementing the lost weight with methanol, shaking up, filtering, and taking the subsequent filtrate.

The method comprises precisely measuring sample solution under the item of 'preparation of sample solution' of 50mL, concentrating to a certain density, evaporating to dryness in water bath in an evaporation dish with constant weight, drying at 105 deg.C for 3h to constant weight, cooling in a drier for 30min, rapidly and precisely weighing the weight, and calculating to obtain the dry extract rate.

W50mL weight of extract of 50mL sample solution

Total volume of sample

W medicinal materials with the weight of the medicinal materials

(2) Determination result of paeoniflorin content

Paeoniflorin chromatographic conditions Agela promosil C18(250 mm. times.4.6, 5 μm); methanol-0.5 mol/L potassium dihydrogen phosphate solution is 40:65 as a mobile phase; the detection wavelength is 230 nm; flow rate: 1.0 mL/min; column temperature: 30 ℃; the number of theoretical plates of paeoniflorin is not less than 3000. As shown in fig. 6, 7 and 8.

Accurately weighing appropriate amount of paeoniflorin reference substance, dissolving with methanol to obtain 257 μ g/ml reference substance solution, and injecting into HPLC for determination according to preset chromatographic conditions. The sample volume of paeoniflorin is 2.5 μ L, 5 μ L, 12.5 μ L, 20 μ L, and 25 μ L. And performing linear regression on the sample introduction mass by using the peak area to obtain a regression equation, a correlation coefficient and a linear range of each measured component. The results are shown in table 10 and fig. 9: the mass concentration of paeoniflorin is in good linear relation within the range of 0.64-6.42 mug.

Watch 10

Orthogonal experimental design and results

Weighing half the amount of medicinal materials 31.5g according to the prescription, and mixing according to L9 (3)⁴) Orthogonal test conditions are respectively extracted, filtered and primarily concentrated to a certain amount to obtain test solution. The best process is obtained by taking paeoniflorin content and dry extract rate as indexes and taking comprehensive evaluation (comprehensive evaluation is paeoniflorin content/maximum paeoniflorin content multiplied by 80-dry extract rate/maximum dry extract rate multiplied by 20) as an index. The results are shown in tables 11 to 13.

TABLE 11 results of orthogonal experiments

TABLE 12 analysis of variance in orthogonal experiments

TABLE 13 results of comprehensive scoring in orthogonal experiments

From the results of the orthogonal experiments in the table, it can be known that each factor influences the sequence in the water extraction process, namely extraction times > water addition > extraction time, wherein the extraction times a have significance (P <0.05), so according to the results of the orthogonal experiments, a2 is the best extraction times a; the ethanol dosage B and the extraction time C have no significant difference, and the optimal process condition is A2B1C1 by combining the large production requirement. It is extracted with 6 times of water for 2 times, each for 1 hr.

2.4.4 validation test

Half the prescription amount of 31.5g of the herbs was weighed out and tested according to best protocol A2B1C1, the results are shown in Table 14. The results were consistent with the results of the orthogonal experiments. The process is stable and feasible. Therefore, the water extraction process is determined to be 6 times of water extraction for 2 times, and each time is 1 h.

Table 14 water extraction process validation results

2.5 aqueous extract impurity removal Process optimization

After the traditional Chinese medicinal materials are extracted with water, the liquid of the traditional Chinese medicinal materials often contains starch, polysaccharide, protein, pectin and the like, so that the final prepared solid preparation has an overlarge administration dosage, and therefore, the extracting solution is generally purified, the content of irrelevant components in the preparation is reduced, and the administration dosage is reduced. Alcohol precipitation and impurity removal processes are mostly adopted in the production.

2.5.1 different alcohol precipitation concentrations are preferred

Respectively weighing 3 parts of a medicinal material 63g according to the prescription amount, adding 6 times of water for extraction twice, each time for 1 hour, obtaining a water extraction solution for concentration, adding a certain amount of ethanol, respectively controlling the ethanol concentration of the material liquid to be 40%, 50% and 60% for ethanol precipitation, standing for 12 hours to obtain an ethanol precipitation solution, concentrating, decompressing and drying to respectively obtain 3 parts of dry paste, wherein the results are shown in table 15.

TABLE 15 comparison of ethanol concentration in water extraction and ethanol precipitation

From the results, it was found that the purification effect of 40% or 50% was inferior to that of 60% ethanol, and the final dose was still large. The 60% ethanol concentration of the feed liquid has a good purification effect, the dosage is effectively reduced, the ethanol concentration of the feed liquid is lower than 65%, the effective components such as polysaccharide and the like in a prescription can be effectively preserved, and the change of the alcohol precipitation concentration has little influence on the paeoniflorin content, so that the ethanol concentration of the feed liquid purified by alcohol precipitation of the water extract is determined to be 60%.

2.6 concentration and drying Process optimization

The ingredients and properties of the traditional Chinese medicine in the traditional Chinese medicine extracting solution are complex, and in the process of concentration and drying, due to long heating time, certain active ingredients contained in the traditional Chinese medicine extracting solution can be damaged to different degrees, so that the content of the active ingredients is reduced, and the clinical curative effect of the preparation is influenced. Concentration and drying are important links of the production of the traditional Chinese medicine preparation, different concentration and drying modes are selected, the content, moisture content, appearance, color, granularity, solubility, sanitary requirements and the like of active ingredients of a finished product are influenced, and the concentration and drying process must be comprehensively considered by combining the production scale and the production capacity of the finished product. The currently used concentration drying methods are divided into four types, and there are various forms such as a normal pressure concentration drying method, a reduced pressure concentration drying method, a spray drying method, a microwave drying method and the like. The reduced pressure concentration has the advantages of preventing the decomposition of effective components, having high benefit, short time consumption, saving energy consumption and the like, and the process selects reduced pressure concentration by combining the consideration of mass production in the future. The transfer rates of quercetin, paeonol and paeoniflorin are used as evaluation indexes, and the normal pressure and vacuum drying and drying processes under different temperature conditions are examined.

2.6.1 different drying methods are preferred

Weighing 48.5g of half prescription amount of medicinal materials, respectively carrying out alcohol extraction and water extraction according to an optimal scheme, mixing extracting solutions, concentrating under reduced pressure to a certain density, drying under normal pressure, drying under reduced pressure in different drying modes, and determining the optimal drying mode by inspecting the factors of the content of quercetin, paeonol and paeoniflorin, such as comparison before and after drying, crispness, color, drying time and the like. The results are shown in Table 16.

TABLE 16 Effect of different drying modes

As can be seen from table 16, the optimum drying method was selected for vacuum drying based on comprehensive consideration of content comparison, crispness, color, and drying time before and after drying of quercetin, paeonol, and paeoniflorin.

2.6.2 Effect of different temperatures on vacuum drying

Weighing 48.5g of half prescription amount of medicinal materials, respectively performing alcohol extraction and water extraction according to the optimal scheme, mixing the extracting solutions, concentrating under reduced pressure to a certain density, and comparing the drying temperature of vacuum drying at 80 ℃, 70 ℃ and 60 ℃. The results are shown in Table 17.

TABLE 17 Effect of different vacuum drying times

As can be seen from table 17, in consideration of the drying efficiency, the transfer rates of quercetin, paeonol, and paeoniflorin decreased with increasing temperature. Although the drying time at 80 ℃ is short, the content is greatly different. The content difference between 60 ℃ and 70 ℃ is small, but the drying efficiency at 60 ℃ is lower than that at 70 ℃, and the vacuum drying at 70 ℃ is determined from the efficiency of mass production.

In the preliminary experiments, the content of paeoniflorin in a red paeony root medicinal material and the content of quercetin in a polygonum perfoliatum medicinal material in the experiments are determined and calculated (according to the requirements of Chinese pharmacopoeia 2010 edition), and are respectively 19mg/g and 1.55 mg/g. The preparation is preferably extracted, purified, concentrated and dried to finally obtain dry extract powder of the preparation. In the target components selected by the preparation, the transfer rates of paeoniflorin in the red paeony root and quercetin in the polygonum perfoliatum are measured and calculated to respectively reach 76% and 61%, which indicates that the selected extraction, purification, concentration and drying processes are stable and feasible.

2.7 determination of Molding Process

2.7.1 dosage forms

The prescription amount of the traditional Chinese medicine preparation for treating endometriosis is 97g, and the traditional Chinese medicine preparation is decoction used clinically and has obvious curative effect. In order to increase the clinical adaptability of the traditional Chinese medicine, the prescription is processed into a certain dosage form according to the prescription amount by modern theory, technology and method under the guidance of the traditional Chinese medicine theory. According to the physicochemical properties of the components contained in the medicinal materials, the research results of modern pharmacology and the characteristics of various dosage forms, the preparation is considered to have poor stability and inconvenient storage and transportation if the preparation is prepared into a liquid preparation. The invention once considers that the prescription is made into capsules, but the clinical application prescription amount is 97g, the total paste yield is generally 15% after water extraction, alcohol precipitation and alcohol extraction, 0.5g of No. 0 capsules are filled, and 30 capsules are needed to be taken every day under the condition of not adding auxiliary materials, so the medicine taking burden of a patient is increased. Therefore, the prescription is made into granules, so that the adaptability of taking the granules by a patient is improved, the granules are quickly disintegrated in the gastrointestinal tract of a human body, are quickly absorbed, are convenient to transport, carry and take, the stability is improved under the condition of ensuring the curative effect of the prescription, and the modernization and the economic and social values of the prescription are realized.

2.7.2 method of granulating

The granulation can be divided into dry extract granulation and thick paste granulation according to the granulation methods of different raw materials. In the experiment, the ethanol extraction solution and the water extraction solution are concentrated to the relative density of 1.30-1.35, and the auxiliary materials are added for granulation which is 3-5 times of the extract, so that the dosage of the medicine is increased, and dry paste granulation is selected in the experiment.

2.7.3 preference of auxiliary materials

(1) The moisture absorption resisting agent and excipient are suitable auxiliary materials for the reason that dry paste powder of the traditional Chinese medicine granules for treating endometriosis is easy to absorb moisture in the storage process. The invention intends to select dextrin, soluble starch and lactose as excipients, when the soluble starch is used as a moisture-absorbing resistant agent and an excipient in a preliminary experiment, the viscosity of a soft material is low, the forming and the fluidity of particles are better, the moisture-absorbing resistant capability is strong, and the soluble starch is insoluble in water and ethanol, is very stable in the air, absorbs moisture and is not deliquesced. The chemical property of the soluble starch is stable, and the soluble starch does not act with most medicines, and is low in price.

(2) The taste-modifying agent is selected because the traditional Chinese medicine granules for treating endometriosis are bitter and astringent after being extracted by alcohol and water to obtain dry paste powder, and are difficult to be directly orally taken, so a certain taste-modifying agent is considered to be added to improve the unpleasant smell. The added flavoring agents are considered to be 0.2 percent of aspartame, 0.5 percent of sodium cyclamate or sucrose directly used for replacing part of soluble starch as auxiliary materials. Preliminary experiments show that the bitter taste can be effectively improved by adding 0.2 percent of aspartame.

2.7.4 ratio of excipient to powder

The powder and soluble starch were granulated at different mass ratios of 3:4, 1:1, 4:3, 2:1, and the granulation effect, hygroscopicity and appearance were observed, and the results are shown in table 18:

TABLE 18 examination of the ratio of soluble starch to powder

As can be seen from Table 18, when the mass ratio of the powder to the soluble starch is 1:1, the granules do not absorb moisture, have the best effect, and have a high molding rate, so that the optimal mass ratio of the powder to the soluble starch is determined to be 1: 1.

2.7.5 preference for wetting agent

To better ensure the stability of the formulation and its forming rate, the experiment was conducted with 80%, 85%, 90%, 95% ethanol for granulation, and the results are shown in table 19:

TABLE 19 granulation of different wetting agents

The results show that 90% ethanol is used as the wetting agent for granulation, the prepared soft material has moderate viscosity and is easy to granulate, the obtained granules are uniform and moderate, and the forming effect is good, so 90% ethanol is selected as the wetting agent.

2.7.6 Performance criteria of the pellets

(1) Bulk density measurement 2g of the powder was weighed (sieved through a sieve of four), placed in a 10mL measuring cylinder, dropped several times at a constant height (conditions were kept as consistent as possible) to adjust the degree of tightness, and the bulk density was calculated by weight and volume, where the bulk density is weight (g)/volume (mL). The results are shown in Table 20:

TABLE 20 bulk Density measurements of three samples

(2) The angle of repose was determined by placing the funnel on a horizontally placed drawing paper, the distance of the lower mouth of the funnel from the drawing paper was H, pouring the granules into the funnel until the outlet of the funnel contacted the tip of the canister, measuring the cone bottom diameter (2R) and the cone height (H), and calculating θ from tan θ H/R. The results are shown in Table 21:

TABLE 21 results of angle of repose measurements for three samples

The results show that the average angle of repose of the granules is 28.17 degrees, indicating that the flowability of the granules is better.

2.7.7 critical relative humidity of the particles

The critical relative humidity is the critical value of whether the drug absorbs moisture or not, and the environmental humidity during production can be determined according to the critical relative humidity. Saturated solutions of sulfuric acid or different salts with different concentrations are prepared respectively and are placed in a constant-temperature (25 ℃) dryer for 96 hours respectively, so that the internal humidity is balanced to form environments with different relative humidity, and the results are shown in a table 22:

TABLE 22 relative humidity of supersaturated solutions of sulfuric acid or different salts at different concentrations at 25 deg.C

Drying the prepared powder to constant weight, placing particles with the thickness of about 2mm at the bottom of a weighing bottle with the constant weight, accurately weighing the particles, placing the particles in a dryer (with a weighing bottle cap opened) which is listed in the table and respectively contains supersaturated solutions of 6 sulfuric acids or different salts with different concentrations, absorbing moisture in a constant-temperature incubator at 25 ℃ to constant weight, precisely weighing, and calculating the moisture absorption percentage. The results are shown in Table 22.

The moisture absorption curve is plotted with the relative humidity as the abscissa and the moisture absorption rate as the ordinate, as shown in fig. 10. The two ends of the moisture absorption curve are tangent lines of the curve, the abscissa of the intersection point of the two curves is Critical Relative Humidity (CRH), the critical relative humidity is 60 percent, therefore, the relative humidity is controlled to be less than 60 percent in the environment of crushing, granulating, packaging and storing, and the moisture-proof packaging is adopted.

Third, pilot scale production

The raw materials are fed according to the unit amount of 1000 preparations, the preparation is carried out according to the optimal process, three batches of pilot-scale finished products are pilot-produced, and the detection is carried out according to the quality standard and the requirements under the item of the drug granules, and the results are shown in tables 23 and 24.

Raw material input of formula amount of 231000 preparations in Table

TABLE 24 Pilot plant test product inspection data

From the pilot production research results in the table, the molding rate of the product can reach 90% by adopting the optimized molding process, the molding rates of the three batches of finished products are basically consistent, multiple indexes of the finished products are detected, and the transfer rates of paeoniflorin in the red paeony root and quercetin in the polygonum perfoliatum are calculated to respectively reach 71% and 52%, so that the process is simple, feasible and stable.

The preparation formula is used for clinical trial research, and the research is as follows:

4.1, clinical data

4.1.1 general data

126 patients, mean age (33.5 ± 6.3) years.

4.1.2, diagnostic criteria

Refer to the revised standard of the third academic conference of the gynaecology and obstetrics professional committee of the Chinese medical society of western and Chinese medicine. All cases were diagnosed with clinical gynecological examination and type B ultrasonography, and some cases were diagnosed with endometriosis by CT, MRI, CA125 value, laparoscopy and postoperative pathology.

The main clinical symptoms and signs 126 patients had lumbosacral pain, dysmenorrhea 86 cases, irregular menstruation 43 cases and infertility 15 cases. 71 cases of obvious painful nodules are detected in gynecological examination, 41 cases of uterine adenomatosis are suggested by B ultrasonic, 34 cases of ovarian chocolate cysts are detected in the gynecological examination, and 16 cases of the gynecological examination and the maximum diameter of the cysts is 8.7 cm.

4.2 methods of treatment and visualization

4.2.1 methods of treatment

(1) Treatment of

When clinical curative effect is observed, decoction is adopted. The compound longdan decoction is used as follows: 3g of dragon blood, 12g of rhubarb, 10g of dogwood, 8g of angelica, 8g of tree peony bark, 8g of costustoot, 8g of corydalis tuber, 6g of red paeony root, 10g of tuckahoe, 6g of zedoary, 5g of perfoliate knotweed, 5g of cassia twig and 5g of common burreed rhizome, 1 dose per day. For convenient administration, 10 doses of the above medicinal materials are decocted together for 3 times, the obtained medicinal liquid is concentrated to 1000mL, stored in refrigerator at 4 deg.C, 2 times daily, 50mL each time, and heated for oral administration.

(2) The treatment course is 6 months for 1 treatment course.

4.2.2 Observation indicators and methods

(1) The main clinical symptoms and physical signs are that symptoms such as lumbosacral pain, dysmenorrheal, irregular menstruation and the like are graded according to the degree of severity, and 0 is scored for asymptomatic patients; mild case 1 score; 2 points for moderate symptoms; severe disease was divided into 3 points. According to the gynecologic double-diagnosis and triple-diagnosis, the pathological changes are classified into mild, moderate and severe according to the physical signs of painful nodules, intimal cysts, pelvic adhesions and the like obtained by B-ultrasonic examination. 0 point for patients without obvious physical signs; mild degree 1 score; medium 2 points; the gravity was 3 points. In the course of taking medicine, gynecological examination is performed for 1 time every 4 weeks, B-ultrasonic examination is performed for 1 time every 8 weeks, and the degree of improvement of clinical symptoms and physical signs of 2 groups of cases is dynamically observed.

(2) The side effect condition of the medicine, the pregnancy follow-up and the relapse condition are observed.

4.3 therapeutic results

4.3.1, standard of therapeutic effect

According to the therapeutic effect standard established by the third academic conference of the special Committee of obstetrics and gynecology of the Chinese medical and western medicine Union, the first is to heal that the symptoms are completely disappeared, the local physical signs such as pelvic cavity mass and the like are basically disappeared, and the infertility patient is pregnant or fertile within 3 years; secondly, the effect is shown, wherein symptoms basically disappear, the pelvic cavity mass is reduced, or although local signs exist, the patients with infertility can be pregnant; thirdly, the medicine is effective, the symptoms are relieved, the pelvic cavity mass is not enlarged or slightly reduced, and the symptoms are not aggravated within 3 months after the medicine is stopped; fourthly, the Chinese medicinal composition is ineffective, the main symptoms are unchanged or worsened, and the local lesion has the tendency of aggravation.

4.3.2, results

The statistics of the clinical data of 126 cases of non-operative treatment of internal diseases indicate that the total effective rate is 90.48 percent, wherein 35 cases (29.36 percent), 48 cases (38.09 percent) and 31 cases (24.60 percent) are cured, and the curative effect is obvious.

The invention has the advantages that: the traditional Chinese medicine preparation for treating endometriosis has the effects of promoting blood circulation to remove blood stasis, tonifying kidney to arrest desertion, eliminating blotches, dispersing masses, dredging collaterals and relieving pain. Is used for treating abdominal mass for women, kidney deficiency and blood stasis, or menstrual disorder caused by qi stagnation and blood stasis, abdominal distention and pain before menstruation, menstrual pain, lumbosacral pain, tenderness, pudendum depression, or menstrual disorder, hypomenorrhea, scanty menstruation or dripping, dark blood, blood clot, pain relieving under lump, or breast distending pain, headache, insomnia, hyposexuality, purple tongue dark, or ecchymosis on the edge, thin tongue fur, deep and thready pulse or wiry pulse; endometriosis and uterine fibroids are seen in the above-mentioned cases. The treatment effect is remarkable, and the total effective rate is 90.48% according to statistics of clinical data of 126 cases of non-operative treatment internal abnormal symptoms, wherein 35 cases (29.36%) are cured, 48 cases (38.09%) are remarkably effective, and 31 cases (24.60%) are effective. The traditional Chinese medicine preparation for treating endometriosis has a good effect of treating endometriosis. The composition medicines of the invention are common medicines carried by pharmacopoeia and landmarks, and the resources are rich. The traditional Chinese medicine preparation for treating endometriosis is preferably granules, is convenient for patients to take, really achieves three or five stools, and realizes modernization of traditional Chinese medicine. Through the research on the extraction and preparation processes of the preparation, more reasonable extraction process conditions and preparation process conditions are preferably selected. The preparation process is simple, feasible and stable, the preparation conditions are mild and easy to control, the operation is simple, and the large-scale production is easy to realize.

Drawings

FIG. 1 is a process flow diagram of the present invention;

FIG. 2 is a chromatogram of an alcohol extract sample in an alcohol extraction preferred process;

FIG. 3 is a chromatogram of a polygonum perfoliatum-deficient negative sample in an alcohol extraction and optimization process;

FIG. 4 is a chromatogram of a quercetin control in an alcohol extraction preferred process;

FIG. 5 is a graph of the standard curve of quercetin in the alcohol extraction optimization process;

FIG. 6 is a chromatogram of a sample of aqueous extract from a preferred aqueous extraction process;

FIG. 7 is a chromatogram of a negative sample lacking red peony root in a preferred water extraction process;

FIG. 8 is a chromatogram of a paeoniflorin control in a water extraction preferred process;

FIG. 9 is a standard profile of paeoniflorin in a preferred water extraction process;

fig. 10 is the moisture absorption curve of the intermediate of the traditional Chinese medicine granule for treating endometriosis.

Detailed Description

The invention is further described with reference to specific examples.

Example 1

A traditional Chinese medicine preparation for treating endometriosis is prepared from the following raw material medicines: 53g of dragon blood, 99g of rheum officinale, 198g of dogwood, 198g of angelica, 198g of moutan bark, 99g of costustoot, 99g of corydalis tuber, 198g of red paeony root, 293g of poria cocos, 173g of curcuma zedoary, 105g of polygonum perfoliatum, 99g of cassia twig and 165g of rhizoma sparganii. The preparation method comprises the following steps: weighing the polygonum perfoliatum, the dogwood, the corydalis tuber and the rhubarb according to the amount, adding 60-80% ethanol in an amount which is 6-10 times that of the polygonum perfoliatum, performing reflux extraction for 1-3 times, and filtering for 1-2 hours each time to obtain an ethanol extract for later use; weighing dragon's blood, Chinese angelica, tree peony bark, costustoot, red paeony root, Indian buead, zedoary, cassia twig and common burreed rhizome according to the amount, adding 6-10 times of water, decocting and extracting for 1-3 times, each time for 1-2 hours, filtering to obtain water extract, concentrating at 75 ℃ under reduced pressure until the density is 1.05 to obtain concentrated water extract, adding ethanol, uniformly stirring, controlling the concentration of the ethanol in the material liquid to be 40-60%, standing for 12 hours, removing precipitate to obtain ethanol precipitation supernatant for later use; mixing the ethanol extractive solution and the supernatant, concentrating under reduced pressure at 75 deg.C to density of 1.25 to obtain concentrated solution, vacuum drying at 60-80 deg.C for 42-72 hr to obtain extract, pulverizing, sieving with No. 5 sieve to obtain powder, and adding adjuvants to make into various pharmaceutical preparations.

Example 2

A traditional Chinese medicine preparation for treating endometriosis is prepared from the following raw material medicines: 198g of dragon blood, 495g of rhubarb, 396g of dogwood, 396g of angelica, 396g of tree peony bark, 330g of costustoot, 330g of corydalis tuber, 396g of red paeony root, 495g of tuckahoe, 297g of zedoary, 990g of polygonum perfoliatum, 330g of cassia twig and 330g of common burreed rhizome. The preparation method comprises the following steps: weighing herba Polygoni Cymosi, Corni fructus, rhizoma corydalis and radix et rhizoma Rhei according to the amount, adding 6 times of 60% ethanol, reflux extracting for 1 time, each time for 2 hr, and filtering to obtain ethanol extractive solution; weighing sanguis Draxonis, radix Angelicae sinensis, cortex moutan, radix aucklandiae, radix Paeoniae Rubra, Poria, Curcumae rhizoma, ramulus Cinnamomi and rhizoma Sparganii according to a certain amount, decocting with 8 times of water for 1 time, decocting with 7 times of water for 2 times, each time for 1.5 hr, filtering to obtain water extractive solution, concentrating at 75 deg.C under reduced pressure to density of 1.05 to obtain concentrated water extractive solution, adding ethanol, stirring well, controlling ethanol concentration in the material liquid to 40%, standing for 12 hr, discarding precipitate to obtain ethanol precipitation supernatant; mixing the alcohol extract and the alcohol precipitation supernatant, concentrating under reduced pressure at 75 ℃ until the density is 1.25 to obtain a concentrated solution, drying the concentrated solution under vacuum at 60 ℃ for 57 hours to obtain an extract, crushing and sieving by a No. 5 sieve to obtain medicinal powder, adding soluble starch into the medicinal powder according to the mass ratio of 1:1, taking aspartame accounting for 0.2 percent of the total mass of the medicinal powder as a flavoring agent, taking 90 percent of ethanol as a wetting agent for granulation, drying the granules at 60-80 ℃, performing secondary granulation, sieving by the No. 1 sieve to remove large granules, and sieving by the No. 5 sieve to remove fine powder to obtain granules. The preparation is administered after mixing with boiling water. Two bags at a time and three times a day. Each bag is 5 g.

Example 3

A traditional Chinese medicine preparation for treating endometriosis is prepared from the following raw material medicines: 103g of dragon blood, 412g of rhubarb, 343g of dogwood fruit, 275g of angelica, 275g of tree peony bark, 175g of costustoot, 257g of corydalis tuber, 223g of red paeony root, 343g of tuckahoe, 223g of zedoary, 155g of polygonum perfoliatum, 223g of cassia twig and 223g of rhizoma sparganii. The preparation method comprises the following steps: weighing herba Polygoni Cymosi, Corni fructus, rhizoma corydalis and radix et rhizoma Rhei, adding 9 times and 8 times of 80% ethanol respectively, reflux extracting for 2 times, each for 1 hr, and filtering to obtain ethanol extractive solution; weighing sanguis Draxonis, radix Angelicae sinensis, cortex moutan, radix aucklandiae, radix Paeoniae Rubra, Poria, Curcumae rhizoma, ramulus Cinnamomi and rhizoma Sparganii, adding 7 times and 6 times of water, decocting and extracting for 2 times, each time for 1 hr, filtering to obtain water extractive solution, concentrating at 75 deg.C under reduced pressure to density of 1.05 to obtain concentrated water extractive solution, adding ethanol, stirring, controlling ethanol concentration in the material liquid to 60%, standing for 12 hr, discarding precipitate to obtain ethanol precipitation supernatant; mixing the alcohol extract and the alcohol precipitation supernatant, concentrating under reduced pressure at 75 ℃ until the density is 1.25 to obtain a concentrated solution, drying the concentrated solution under vacuum at 70 ℃ for 60 hours to obtain an extract, crushing and sieving by a No. 5 sieve to obtain medicinal powder, adding soluble starch into the medicinal powder according to the mass ratio of 1:1, taking aspartame accounting for 0.2 percent of the total mass of the medicinal powder as a flavoring agent, taking 90 percent of ethanol as a wetting agent for granulation, drying the granules at the temperature of 60-80 ℃ gradually, granulating for the second time, sieving by the No. 1 sieve to remove large granules, and sieving by the No. 5 sieve to remove fine powder to obtain granules. The preparation is administered after mixing with boiling water. Two bags at a time and three times a day. Each bag is 5 g.

Example 4

A traditional Chinese medicine preparation for treating endometriosis is prepared from the following raw material medicines: 150g of dragon's blood, 350g of rheum officinale, 220g of dogwood, 230g of angelica, 300g of moutan bark, 250g of costustoot, 240g of corydalis tuber, 260g of red paeony root, 310g of poria cocos, 200g of curcuma zedoary, 800g of polygonum perfoliatum, 260g of cassia twig and 210g of rhizoma sparganii. The preparation method comprises the following steps: weighing herba Polygoni Cymosi, Corni fructus, rhizoma corydalis and radix et rhizoma Rhei according to the amount, adding 10 times of 70% ethanol, reflux-extracting for 1 time, adding 9 times of 70% ethanol, reflux-extracting for 2 times, each time for 1.5 hr, and filtering to obtain ethanol extractive solution; weighing sanguis Draxonis, radix Angelicae sinensis, cortex moutan, radix aucklandiae, radix Paeoniae Rubra, Poria, Curcumae rhizoma, ramulus Cinnamomi and rhizoma Sparganii according to a certain amount, adding 10 times of water, decocting and extracting for 1 time, each time for 2h, filtering to obtain water extract, concentrating at 75 deg.C under reduced pressure to density of 1.05 to obtain concentrated water extract, adding ethanol, stirring, controlling ethanol concentration in the material liquid to 50%, standing for 12h, discarding precipitate to obtain ethanol precipitation supernatant; mixing the alcohol extract and the alcohol precipitation supernatant, concentrating under reduced pressure at 75 ℃ until the density is 1.25 to obtain a concentrated solution, drying the concentrated solution at 80 ℃ for 42 hours in vacuum to obtain an extract, crushing and sieving by a No. 5 sieve to obtain medicinal powder, adding soluble starch into the medicinal powder according to the mass ratio of 1:1, granulating by using aspartame accounting for 0.2 percent of the total mass of the medicinal powder as a flavoring agent and 90 percent of ethanol as a wetting agent, drying the granules at 60-80 ℃, granulating for the second time, sieving by the No. 1 sieve to remove large granules, and sieving by the No. 5 sieve to remove fine powder to obtain the granules. The preparation is administered after mixing with boiling water. Two bags at a time and three times a day. Each bag is 5 g.

Example 5

A traditional Chinese medicine preparation for treating endometriosis is prepared from the following raw material medicines: 80g of dragon's blood, 150g of rheum officinale, 330g of dogwood, 305g of angelica, 350g of moutan bark, 180g of costustoot, 120g of corydalis tuber, 360g of red paeony root, 390g of poria cocos, 210g of curcuma zedoary, 500g of polygonum perfoliatum, 120g of cassia twig and 300g of rhizoma sparganii. The preparation method comprises the following steps: weighing herba Polygoni Cymosi, Corni fructus, rhizoma corydalis and radix et rhizoma Rhei, adding 8 times and 7 times of 75% ethanol respectively, reflux extracting for 2 times, each for 1.5 hr, and filtering to obtain ethanol extractive solution; weighing sanguis Draxonis, radix Angelicae sinensis, cortex moutan, radix aucklandiae, radix Paeoniae Rubra, Poria, Curcumae rhizoma, ramulus Cinnamomi and rhizoma Sparganii, adding 9 times and 8 times of water, decocting and extracting for 2 times, each time for 2 hr, filtering to obtain water extractive solution, concentrating at 75 deg.C under reduced pressure to density of 1.05 to obtain concentrated water extractive solution, adding ethanol, stirring, controlling ethanol concentration in the material liquid to 60%, standing for 12 hr, discarding precipitate to obtain ethanol precipitation supernatant; mixing the alcohol extract and the alcohol precipitation supernatant, concentrating under reduced pressure at 75 ℃ until the density is 1.25 to obtain a concentrated solution, drying the concentrated solution under vacuum at 60 ℃ for 72 hours to obtain an extract, crushing and sieving by a No. 5 sieve to obtain medicinal powder, adding soluble starch into the medicinal powder according to the mass ratio of 1:1, taking aspartame accounting for 0.2 percent of the total mass of the medicinal powder as a flavoring agent, taking 90 percent of ethanol as a wetting agent for granulation, drying the granules at the temperature of 60-80 ℃ gradually, granulating for the second time, sieving by the No. 1 sieve to remove large granules, and sieving by the No. 5 sieve to remove fine powder to obtain granules. The preparation is administered after mixing with boiling water. Two bags at a time and three times a day. Each bag is 5 g.

Example 6

A traditional Chinese medicine preparation for treating endometriosis is prepared from the following raw material medicines: 135g of dragon's blood, 480g of rheum officinale, 270g of dogwood, 380g of angelica, 225g of moutan bark, 210g of elecampane, 300g of corydalis tuber, 300g of red paeony root, 370g of poria cocos, 190g of curcuma zedoary, 200g of polygonum perfoliatum, 190g of cassia twig and 180g of rhizoma sparganii. The preparation method comprises the following steps: weighing herba Polygoni Cymosi, Corni fructus, rhizoma corydalis and radix et rhizoma Rhei according to the amount, reflux-extracting with 9 times of 65% ethanol for 1 time, reflux-extracting with 8 times of 65% ethanol for 2 times, each for 2 hr, and filtering to obtain ethanol extractive solution; weighing dragon's blood, Chinese angelica, tree peony bark, costustoot, red paeony root, Indian buead, zedoary, cassia twig and common burreed rhizome according to the amount, firstly adding 7 times of water for decocting for 1 time, then adding 6 times of water for decocting and extracting for 2 times, wherein each time is 1 hour, filtering to obtain water extract, concentrating at 75 ℃ under reduced pressure until the density is 1.05 to obtain concentrated water extract, then adding ethanol, uniformly stirring, controlling the concentration of the ethanol in the material liquid to be 40-60 percent, standing for 12 hours, removing precipitate to obtain ethanol precipitation supernatant for later use; mixing the alcohol extract and the alcohol precipitation supernatant, concentrating under reduced pressure at 75 ℃ until the density is 1.25 to obtain a concentrated solution, drying the concentrated solution under vacuum at 70 ℃ for 72 hours to obtain an extract, crushing and sieving by a No. 5 sieve to obtain medicinal powder, adding soluble starch into the medicinal powder according to the mass ratio of 1:1, taking aspartame accounting for 0.2 percent of the total mass of the medicinal powder as a flavoring agent, taking 90 percent of ethanol as a wetting agent for granulation, drying the granules at the temperature of 60-80 ℃ gradually, granulating for the second time, sieving by the No. 1 sieve to remove large granules, and sieving by the No. 5 sieve to remove fine powder to obtain granules. The preparation is administered after mixing with boiling water. Two bags at a time and three times a day. Each bag is 5 g.

Claims

1. A traditional Chinese medicine preparation for treating endometriosis is characterized in that: the traditional Chinese medicine composition is prepared from the following raw material medicines in parts by weight: 53-198 parts of dragon's blood, 99-495 parts of rheum officinale, 198-396 parts of dogwood, 198-396 parts of angelica, 198-396 parts of moutan bark, 99-330 parts of elecampane, 99-330 parts of corydalis tuber, 198-396 parts of red paeony root, 293-495 parts of poria cocos, 173-297 parts of curcuma zedoary, 105-990 parts of polygonum perfoliatum, 99-330 parts of cassia twig and 165-330 parts of rhizoma sparganii.

2. The traditional Chinese medicine preparation for treating endometriosis according to claim 1, wherein: the traditional Chinese medicine composition is prepared from the following raw material medicines in parts by weight: 103 parts of dragon's blood, 412 parts of rhubarb, 343 parts of dogwood, 275 parts of angelica, 275 parts of tree peony bark, 175 parts of costustoot, 257 parts of corydalis tuber, 223 parts of red paeony root, 343 parts of tuckahoe, 223 parts of zedoary, 155 parts of polygonum perfoliatum, 223 parts of cassia twig and 223 parts of rhizoma sparganii.

3. The traditional Chinese medicine preparation for treating endometriosis according to claim 1 or 2, wherein: the preparation is a granule prepared by using soluble starch as an excipient, 0.2 percent of aspartame as a flavoring agent and 90 percent of ethanol as a wetting agent.

4. The method for preparing a Chinese medicinal preparation for treating endometriosis according to claim 1 or 2, wherein: weighing the polygonum perfoliatum, the dogwood, the corydalis tuber and the rhubarb according to the amount, adding 60-80% ethanol in an amount which is 6-10 times that of the polygonum perfoliatum, performing reflux extraction for 1-3 times, and filtering for 1-2 hours each time to obtain an ethanol extract for later use; weighing dragon's blood, Chinese angelica, tree peony bark, costustoot, red paeony root, Indian buead, zedoary, cassia twig and common burreed rhizome according to the amount, adding 6-10 times of water, decocting and extracting for 1-3 times, each time for 1-2 hours, filtering to obtain water extract, concentrating at 75 ℃ under reduced pressure until the density is 1.05 to obtain concentrated water extract, adding ethanol, uniformly stirring, controlling the concentration of the ethanol in the material liquid to be 40-60%, standing for 12 hours, removing precipitate to obtain ethanol precipitation supernatant for later use; mixing the ethanol extractive solution and the supernatant, concentrating under reduced pressure at 75 deg.C to density of 1.25 to obtain concentrated solution, vacuum drying at 60-80 deg.C for 72-42 h to obtain extract, pulverizing, sieving with No. 5 sieve to obtain medicinal powder, and adding adjuvants to make into various preparations.

5. The method for preparing a Chinese medicinal preparation for treating endometriosis according to claim 4, wherein: weighing herba Polygoni Cymosi, Corni fructus, rhizoma corydalis and radix et rhizoma Rhei, adding 9 times and 8 times of 80% ethanol respectively, reflux extracting for 2 times, each for 1 hr, and filtering to obtain ethanol extractive solution; weighing sanguis Draxonis, radix Angelicae sinensis, cortex moutan, radix aucklandiae, radix Paeoniae Rubra, Poria, Curcumae rhizoma, ramulus Cinnamomi and rhizoma Sparganii, adding 7 times and 6 times of water, decocting and extracting for 2 times, each time for 1 hr, filtering to obtain water extractive solution, concentrating at 75 deg.C under reduced pressure to density of 1.05 to obtain concentrated water extractive solution, adding ethanol, stirring, controlling ethanol concentration in the material liquid to 60%, standing for 12 hr, discarding precipitate to obtain ethanol precipitation supernatant; mixing the ethanol extractive solution and the supernatant, concentrating under reduced pressure at 75 deg.C to density of 1.25 to obtain concentrated solution, vacuum drying the concentrated solution at 70 deg.C for 60 hr to obtain extract, pulverizing, sieving with No. 5 sieve to obtain medicinal powder, adding adjuvants, and making into various preparations.

6. The method for preparing a Chinese medicinal preparation for treating endometriosis according to claim 4, wherein: adding soluble starch into the medicinal powder according to the mass ratio of 1:1, taking aspartame accounting for 0.2 percent of the total mass of the medicinal powder as a flavoring agent and 90 percent ethanol as a wetting agent for granulation, drying the granules at 60-80 ℃, performing secondary granulation, sieving to remove large granules and fine powder, and obtaining the granules.

7. The method for preparing a Chinese medicinal preparation for treating endometriosis according to claim 6, wherein: adding soluble starch into the medicinal powder according to the mass ratio of 1:1, taking aspartame accounting for 0.2 percent of the total mass of the medicinal powder as a flavoring agent and 90 percent ethanol as a wetting agent for granulation, gradually heating the granules at 60-80 ℃ for drying, performing secondary granulation, sieving by a No. 1 sieve to remove large granules, and sieving by a No. 5 sieve to remove fine powder to obtain the granules.