CN106110206A - A kind of Chinese medicine preparation treating endometriosis and preparation method thereof - Google Patents

Abstract

The invention discloses a kind of Chinese medicine preparation treating endometriosis and preparation method thereof, count by weight, be made up of following crude drug: Sanguis Draxonis 53～198 parts, Radix Et Rhizoma Rhei 99～495 parts, Fructus Corni 198～396 parts, Radix Angelicae Sinensis 198～396 parts, Cortex Moutan 198～396 parts, the Radix Aucklandiae 99～330 parts, Rhizoma Corydalis 99～330 parts, Radix Paeoniae Rubra 198～396 parts, Poria 293～495 parts, Rhizoma Curcumae 173～297 parts, Herba Polygoni cymosi 105～990 parts, Ramulus Cinnamomi 99～330 parts and Rhizoma Sparganii 165～330 parts.The Chinese medicine preparation of the treatment endometriosis of the present invention, blood circulation promoting and blood stasis dispelling, the kidney invigorating takes off admittedly, and dissipate knot, removing obstruction in the collateral to relieve pain, has the effect of good treatment endometriosis.The preparation technology of the present invention is simple, feasible, stable, and preparation condition gentleness is easy to control, simple to operate, it is easy to large-scale production.

Description

A kind of Chinese medicine preparation treating endometriosis and preparation method thereof

Technical field

The present invention relates to a kind of Chinese medicine preparation treating endometriosis and preparation method thereof, belong to traditional Chinese medicine technology neck Territory.

Background technology

Endometriosis refers to the endometrium with growth function, is covered in other portions of the health beyond cavity of uterus , there is a kind of gynaecopathia of cyclic hemorrhage repeatedly simultaneously in position.Ectopic Endometrium functionally can be along with the change of estrogen level Change, also can produce significantly change, not only have the body of gland of inner membrance, also have inner membrance interstitial around.Endometriosis is main Occurring at pelvic organ, cervix uteri, vagina, perineum and abdominal incision are likely to there will be, and have the strongest transformation and business growth ability, for Common gynecological disease disease.Gynecopathy is common in the women of child-bearing age more, and its sickness rate ascendant trend in recent years is very fast, the wherein women of child-bearing age Account for more than 10%, and relapse rate is high.The clinical manifestation of gynecopathy not necessarily has the strongest phase with the degree of pathological changes sometimes Guan Xing, when the lesion degree of patient lighter or local, its clinical manifestation may be very serious, and when the extent of disease of patient Pelvic Anatomy structure gross distortion even occur relatively greatly, its clinical manifestation is the lightest.According to statistics, there are about the intrauterine of 70% Endometriosis patient has typical secondary dysmenorrhea, change in menstrual cycle characteristics, the clinical manifestations such as sexual intercourse is unhappy and infertile.When gynecopathy occurs When other privileged sites, its clinical manifestation produced may not correspond with this disease.And Most patients cardinal symptom is for continuing The property sent out dysmenorrhea, is often accompanied by the Progressive symmetric erythrokeratodermia pain at hypogastric region and back, can be radiated to leg.Generally a few days ago start pain in menstruation Bitterly.When Ectopic Endometrium is hemorrhage, menstruation reaches summit.The Most patients pain in menstrual period is eased.But late In patient, especially having the adhesion of popularity in pelvic cavity, its pain may proceed to exist.Typical secondary dysmenorrhea patient age base These are between 30～45 years old.Its focus can cause the retroversion of patient.The sick time of patient is the longest, its dyspareunia, property Handing over pain, the symptom such as dyspareunia is the most obvious, and endometriosis and about 1/3rd unknown causes is infertile relevant.Should The incidence of infertility of condition subject is also up to 40%.The change of anatomical structure is probably one of infertile reason of severe patient in late period.Gently The reason that degree patient is infertile has the biggest contacting with intraperitoneal microenvironment factor, ovarian function exception etc..

Without the record of " endometriosis " name of disease in Chinese medicine ancient documents, but according to gynecopathy main clinical manifestation, Can belong among the disease such as " dysmenorrhea ", " abdominal mass ", " menoxenia ", " infertile ".The most different according to Gynecology of Chinese Medicine in recent decades The more systematic research of disease, it is believed that " stagnation of blood stasis uterus, punching " is its basic pathogenesis occurred, and function and vim and vigour Imbalance, the factor such as exopathogen invasion is relevant to the formation of the stasis of blood.The diagnoses and treatment of " gynecopathy " is by Chinese medicine Its fundamental characteristic, Chinese medicine thinks, the main symptom of " gynecopathy " is syndrome of blood stasis, and through the whole process of disease.The disease initial stage with Excess syndrome is main, and just, because of the real void that causes, rare pure deficiency syndrome, master shows as simulataneous insufficiency and excessive disease to sick long wound.True person, premenstrual dysmenorrhea, menstrual period Sharp ache, tenderness.Simulataneous insufficiency and excessive person, menstrual period dysmenorrhea, through after pain gesture the most slow.Because trembling with fear and stasis of blood person, for cold type of pain, angor, obtain burning pain Subtract；Because of thermic stasis of blood person, for causalgia, obtain burning pain and increase；Because of stagnation of QI person, swollen pendant is had a pain；Blood stasis notably, for twinge.Because of the stagnation of QI or cold coagulation Causing stasis of blood person, hypomenorrhea, color is purple dark, has clot.Because of hot or damp and hot and stasis of blood person, many through amount, color depth is red, and matter is thick clot.Deficiency of vital energy blood Stasis of blood person, also many also few through amount, color is light dim, matter dilute folder clot.By dialectical to this disease of the traditional Chinese medical science, be generally divided into syndrome of qi stagnation and blood stasis, The type such as cold blood stasis card, blood stasis due to renal deficiency card, damp and hot syndrome of blood stasis.

Chinese medicine has modern medicine pair between its original advantage, particularly recent decades on treatment endometriosis Endometriosis research steps is accelerated, and understanding and the exploration of endometriosis are the most progressively deepened, no by Chinese medicine It is only in symptom, observe single curative effect, observes Chinese medicine to endometriosis effect from Microscopic Indexes more simultaneously Action effect, thus more objectively screen effective and suitable treatment by Chinese herbs method.Chinese medicine is to endometriosis not Only play its therapeutical effect, also can preferably regulate the many aspects such as endocrine and immunity of body simultaneously.Therefore select Chinese medicine, takes modern preferably extraction process and preparation technology, prepares medicine, the treatment for endometriosis provided One true medicable Chinese medicine new varieties, provides new medicine for this patient.

Summary of the invention

For solving the deficiencies in the prior art, it is an object of the invention to provide a kind of Chinese medicine treating endometriosis Preparation and preparation method thereof.The Chinese medicine preparation of the treatment endometriosis that the present invention provides has good treatment intrauterine The effect of endometriosis, preparation technology is simple, feasible, stable.

In order to realize above-mentioned target, the present invention adopts the following technical scheme that:

A kind of Chinese medicine preparation treating endometriosis, counts by weight, is made up of following crude drug: Sanguis Draxonis 53～198 parts, Radix Et Rhizoma Rhei 99～495 parts, Fructus Corni 198～396 parts, Radix Angelicae Sinensis 198～396 parts, Cortex Moutan 198～396 parts, the Radix Aucklandiae 99～330 parts, Rhizoma Corydalis 99～330 parts, Radix Paeoniae Rubra 198～396 parts, Poria 293～495 parts, Rhizoma Curcumae 173～297 parts, Herba Polygoni cymosi 105～990 parts, Ramulus Cinnamomi 99～330 parts and Rhizoma Sparganii 165～330 parts.

Further, the Chinese medicine preparation for the treatment of endometriosis is counted by weight, is made up of following crude drug: dragon Sanguis Draxonis 103 parts, Radix Et Rhizoma Rhei 412 parts, Fructus Corni 343 parts, Radix Angelicae Sinensis 275 parts, Cortex Moutan 275 parts, the Radix Aucklandiae 175 parts, Rhizoma Corydalis 257 parts, Radix Paeoniae Rubra 223 parts, 343 parts of Poria, Rhizoma Curcumae 223 parts, Herba Polygoni cymosi 155 parts, Ramulus Cinnamomi 223 parts and Rhizoma Sparganii 223 parts.

Previous formulations be make excipient with soluble starch, 0.2% aspartame makees correctives, wetting agent made by 90% ethanol The granule made.

The preparation method of the Chinese medicine preparation for the treatment of endometriosis, comprises the following steps: weigh Herba Polygoni cymosi, mountain according to quantity The Fructus Evodiae, Rhizoma Corydalis and rhubarb medicinal material, add ethanol, reflux, extract, filter, obtain alcohol extract, standby；Weigh according to quantity Sanguis Draxonis, Radix Angelicae Sinensis, Cortex Moutan, the Radix Aucklandiae, Radix Paeoniae Rubra, Poria, Rhizoma Curcumae, Ramulus Cinnamomi and Rhizoma Sparganii, add water, and decocts and extracts, and filters, obtains Aqueous extracts, through concentrating under reduced pressure, Obtain condensed water extract, add ethanol, stir, stand, discard precipitation, obtain precipitate with ethanol supernatant, standby；Alcohol extract and precipitate with ethanol Supernatant mixes, concentrating under reduced pressure, obtains concentrated solution, and concentrated solution is vacuum dried, and obtains extractum extract, pulverizes and sieves, obtains medicated powder, then Add adjuvant and make various pharmaceutical preparation.

Specifically, the preparation method of the Chinese medicine preparation of aforementioned therapies endometriosis, comprise the following steps: claim according to quantity Take Herba Polygoni cymosi, Fructus Corni, Rhizoma Corydalis and rhubarb medicinal material, add 6～10 times amount 60%～80% ethanol, reflux, extract, 1～3 times, often Secondary 1～2h, filter, obtain alcohol extract, standby；Weigh Sanguis Draxonis, Radix Angelicae Sinensis, Cortex Moutan, the Radix Aucklandiae, Radix Paeoniae Rubra, Poria, Rhizoma Curcumae, osmanthus according to quantity Branch and Rhizoma Sparganii, add 6～10 times amount water, decocts and extracts 1～3 time, and each 1～2h filter, obtain Aqueous extracts, through 75 DEG C of concentrating under reduced pressure Being 1.05 to density, obtain condensed water extract, add ethanol, stir, controlling concentration of alcohol in feed liquid is 40%～60%, Stand 12h, discard precipitation, obtain precipitate with ethanol supernatant, standby；Alcohol extract mixes with precipitate with ethanol supernatant, and 75 DEG C are evaporated to density It is 1.25, obtains concentrated solution, concentrated solution 60 DEG C～80 DEG C vacuum drying 72～42h, obtain extractum extract, pulverized No. 5 sieves, and obtained Medicated powder, adds adjuvant and makes various pharmaceutical preparation.

Preferably, the preparation method of the Chinese medicine preparation of aforementioned therapies endometriosis, comprise the following steps: claim according to quantity Take Herba Polygoni cymosi, Fructus Corni, Rhizoma Corydalis and rhubarb medicinal material, add 9 times amount, 8 times amount 80% ethanol respectively, reflux, extract, 2 times, every time 1h, filters, obtains alcohol extract, standby；Weigh Sanguis Draxonis, Radix Angelicae Sinensis, Cortex Moutan, the Radix Aucklandiae, Radix Paeoniae Rubra, Poria, Rhizoma Curcumae, Ramulus Cinnamomi and three according to quantity Rib, adds 7 times amount, 6 times amount water respectively, decocts and extracts 2 times, and each 1h filters, obtains Aqueous extracts, be evaporated to density through 75 DEG C Being 1.05, obtain condensed water extract, add ethanol, stir, controlling concentration of alcohol in feed liquid is 60%, stands 12h, discards Precipitation, obtains precipitate with ethanol supernatant, standby；Alcohol extract mixes with precipitate with ethanol supernatant, and 75 DEG C are evaporated to density is 1.25, obtains concentration Liquid, concentrated solution 70 DEG C vacuum drying 60h, obtain extractum extract, pulverized No. 5 sieves, and obtained medicated powder, and added adjuvant and make various Pharmaceutical preparation.

Further, the preparation method of the Chinese medicine preparation of aforementioned therapies endometriosis, is by the mass ratio of 1:1 Adding soluble starch in medicated powder, the aspartame accounting for medicated powder gross mass 0.2% with consumption makees correctives, and 90% ethanol is made to moisten Humectant is pelletized, and granule is dried in 60 DEG C～80 DEG C, and secondary is pelletized, and crosses and screens out bulky grain and except fine powder, obtains granule.

More specifically, the preparation method of the Chinese medicine preparation of aforementioned therapies endometriosis, it is by the mass ratio of 1:1 Adding soluble starch in medicated powder, the aspartame accounting for medicated powder gross mass 0.2% with consumption makees correctives, and 90% ethanol is made to moisten Humectant is pelletized, and granule gradually rises warming middle-JIAO at 60 DEG C～80 DEG C and is dried, and secondary is pelletized, and crosses No. 1 and screens out bulky grain, crosses No. 5 and screens out thin Powder, obtains granule.

The Chinese medicine preparation of the treatment endometriosis of the present invention, with Herba Polygoni cymosi and Sanguis Draxonis as monarch drug, Cortex Moutan, prolongs Rhizoma Corydalis and Radix Paeoniae Rubra are ministerial drug, and Radix Et Rhizoma Rhei, Fructus Corni, the Radix Aucklandiae, Rhizoma Curcumae and Rhizoma Sparganii are adjuvant drug, and Radix Angelicae Sinensis, Ramulus Cinnamomi and Poria are for making medicine.

In order to ensure the science, reasonable, feasible of the present invention program, by carrying out series of experimental research and investigation, thus Determine the solution of the present invention.

One, the selection of crude drug in the present invention:

1, Sanguis Draxonis nature and flavor are sweet, salty flat, nontoxic, have effect of promoting blood circulation to remove blood stasis, pain relieving, hemostasis, promoting tissue regeneration and ulcer healing.Wherein contain Resin about 57.5%, for the derivant of flavonoid.More to its chemical constitution study in recent years.Its liposoluble constituent is studied Middle separation also identifies 6 fat-soluble compounds.It has blood circulation promoting and blood stasis dispelling and hemostasis convergence two-ways regulation, anti-inflammatory and antalgic, antibacterial Deng effect.

2, Rhizoma Sparganii bitter in the mouth, property are put down, and enter liver, spleen channel, have the effect such as removing blood stasis circulation of qi promoting, removing food stagnancy pain relieving, be conventional invigorating blood circulation Stasis of blood Chinese medicine.Volatile oil, organic acid, steroid, flavonoid, Phenylpropanoid Glycosides class etc. are its main chemical compositions.There is anti-blood little Plate coagulation and antithrombotic, on effects such as the impact of hemorheological property, analgesias.

3, Herba Polygoni cymosi, for the aerial parts of polygonaceae plant Herba Polygoni cymosi, have another name called pass through leaf knotweed, Herba Lespedezae Cuneatae, Herba Polygoni cymosi, Herba Damnacanthi, Plough point grass etc., all herbal medicine, for perennial climing property draft, all there is distribution all parts of the country, aboundresources.Begin to be loaded in " ten thousand sick times Spring ", now record the Pharmacopoeia of the People's Republic of China one (version in 2010).Property acid, bitter, flat, there is heat-clearing and toxic substances removing, parasite killing only Itch, effect of dispelling wind stopping cough, inducing diuresis to remove edema, the treatment edema that is widely used among the people, jaundice, malaria, dysentery, pertussis, ulcer, red Poison, eczema, herpes, scabies and venom etc., determined curative effect.In Herba Polygoni cymosi root isolation identification go out cupreol, trans-to hydroxyl Base methyl cinnamate, Quercetin, Quercetin-3-O-β-D-glucopyranoside, rheum emodin, physcione and aloe-emodin etc. are changed Compound.Containing phenols, organic acid, alkaloid, aminoacid, tannin, flavone, anthraquinone, glycoside, saccharide, plant sterol and triterpenes Etc. chemical composition.Herba Polygoni cymosi Med Mat Appreciation kaempferol, Quercetin, storage glycosides, Quercetin-3-O-β-D-Glucose aldehydic acid methyl ester, The flavone compounds such as Quercetin-3-β-D-Glucose aldehydic acid N-butyl, KAEMPFEROL-3-O-RUTINOSIDE, rutin.Herba Polygoni cymosi has There are the effects such as antiinflammatory antibacterial, eliminating phlegm and stopping cough, antiviral.

4, Radix Et Rhizoma Rhei is polygonum rheum palmatum (Rheum palmatum L.), Rheum tanguticum (Rheum TanguticumMaxim.ex Balf.) or the dry root and rhizome of Rheum officinale (Rheum officinale Baill.).In Medicine Radix Et Rhizoma Rhei is one of special product of China medicine, and bitter in the mouth is cold in nature, returns stomach, spleen, large intestine, liver, pericardium channel, has purging heat and dredging bowels, removing heat from blood solution The effects such as poison, eliminating blood stasis and inducing menstruation.Shennong's Herbal is said: " lower blood stasis, blood closes cold and heat, broken abdominal mass accumulation, and prolonged fluid-retention dyspepsia cleanses intestinal Stomach, pushes away Chen Zhixin, tonneau water paddy, relieving dyspepsia in tune, peace and the five internal organs ".Compendium of Material Medica: " dysentery is red in vain, and pain in the abdomen is suffered from abdominal pain, urine leaching Drip, excess-heat dryness accumulated in the stomach and intestine, the quiet language of hectic fever, yellow cellulitis, all burn ".Anthraquinone derivatives is active component main in Radix Et Rhizoma Rhei.Anthraquinones spreads out Biology includes anthrone class rheum emodin (Emodin), chrysophanic acid (Rhein), chrysophanol (Chrysophano1), physcione (Physcion), the effective ingredient such as aloe-emodin (Aloe-emodin) and chrysaron (Chrysaron)；Radix Et Rhizoma Rhei possibly together with Glycoside that Radix Et Rhizoma Rhei anthraquinone analog derivative and glucose are combined into and anthrone class, such as sennoside (Sennoside) A, B, C, D, E, F Deng, and other glycosides, tannin, compound of polysaccharide, organic compound and inorganic matter etc..Radix Et Rhizoma Rhei has blood and metabolic system Impact, hemostasis, blood fat reducing, rush down under, heat-clearing and toxic substances removing, anti-inflammation, hepatic cholagogic effect.

5, Radix Angelicae Sinensis has benefiting blood and regulating blood circulation, regulating menstruation, hemostasis, effect of intestine moistening laxation, for parts of generic medicinal plants.Can be used for blood deficiency to wither The treatment of Huang, dizziness cardiopalmus, menoxenia, amenorrhea dysmenorrhea, asthenia cold abdominalgia, dryness of the intestine constipation, rheumatic arthralgia etc..Research shows, its Comprise the multiple active ingredient such as volatile oil, polysaccharide.

6, Rhizoma Curcumae is conventional Chinese medicine, its acrid in the mouth warm in nature, has circulation of qi promoting removing blood stasis, effect of removing food stagnancy pain relieving.For blood stasis amenorrhea, Dyspeptic abdominal distention etc..Research show to have preferable antitumor, antithrombotic, antiinflammatory, antiviral, antiearly pregnancy, antibacterial, protect the liver, anti-fibre Dimensional tissue hypertrophy etc. act on.It it is the activating blood and removing stasis drug the most more commonly used.Its active component is volatile oil, modern pharmacology Research shows, its have preferable antitumor, antithrombotic, antiinflammatory, antiviral, antiearly pregnancy, antibacterial, protect the liver, anti-psoriasis, anti-fibre The multiple pharmacological effect such as dimensional tissue hypertrophy.

7, Poria is a kind of Mycophyta Chinese medicine.Sweet in the mouth, light flat.GUIXIN, lung, kidney channel.There are promoting diuresis to eliminate damp pathogen, spleen invigorating, calm the nerves Effect modern pharmacological research proves, it has diuresis, regulation immunity, calmness, antitumor, protects the liver etc. and to act on, and is clinically used for edema The treatment of the cards such as oliguria, phlegm retention vertigo and palpitation, insufficiency of the spleen lack of appetite, loose stool are had loose bowels, irritability, is widely used.

8, Ramulus Cinnamomi is recorded in Shennong's Herbal the earliest, comes from " Newly Revised Canon of Materia Medica ", property of medicine temperature, acrid-sweet flavor, current 12 warps. GUIXIN, lung, bladder warp, have relieving the exterior syndrome by diaphoresis, supporing yang activating QI, effect of relieving the exterior syndrome by diaphoresis, and it is contained within volatile oil, also the benzyl in formic acid Ester, acetic acid meat ester, coumarin, Rhizoma Acori Graminei alkene etc..There is the effect such as antiviral, antibacterial, antipyretic-antalgic, antiinflammatory, antiallergic.

9, the root bark of Cortex Moutan system Ranunculaceae Paeonia plant Paeonia suffruticosa (Paenoina SuffruticosaAndr).Property is micro- Cold, bitter in the mouth, pungent.GUIXIN, liver, kidney channel.Cortex Moutan is divided into part more, is mainly composed of phenol and phenolic glycoside class, monoterpene and glycoside thereof, Also have triterpene, sterol and glycoside, flavone, organic acid, coumarin etc..In Cortex Moutan, phenol and phenolic glycoside class are the classes that content is higher Compound, the phenol therefrom separated and phenolic glycoside compounds have: paeonol, Cortex Moutan phenolic glycoside, the former glycosides of paeonol, paeonol are new.Its tool There are the regulation of atherosclerosis, blood pressure lowering, blood sugar lowering, convulsion, urinary system, regulation immunocyte, antibacterial and anti-inflammation functions.

10, Fructus Corni has the effect such as liver and kidney tonifying, essence astringing and desertion stemming, is usually used in dizziness, tinnitus, soreness of waist and knee joint, sexual impotence, loses Essence, the enuresis, frequent micturition, leucorrhoea hemorrhage, profuse sweating collapses, and interior-heat such as is quenched one's thirst the disease.Iridoid glycosides, Pentacyclic triterpenic acid and esters thereof, Tannin class, polysaccharide are the chemical composition that it is main.There is blood sugar lowering, antibacterial, antiinflammatory, and immune system can be affected.

11, Rhizoma Corydalis acrid in the mouth, hardship, warm in nature, returns liver, spleen channel；Have invigorate blood circulation, promoting the circulation of QI, effect of pain relieving.Main chemical compositions For isoquinoline type alkaloid, being divided into two kinds by the dissolubility in water, tertiary amine base is the most insoluble or is insoluble in water；Quaternary amine alkali is easier to It is dissolved in water.Up to now, therefrom separate and through the existing kind more than 40 of Structural Identification, adhere to separately proto-berberine, aporphine, former Ah Sheet bases, isoquinolin benzyl imidazoles, isoquinolin benzo phenanthridines class, double benzyl different beautiful jade class etc..There are blood circulation promoting and blood stasis dispelling, promoting the circulation of QI to relieve pain Effect, modern experimental proves that it has well analgesia, calm, blood pressure lowering and antiarrhythmic effect.Have invigorate blood circulation, circulation of qi promoting, The effect of pain relieving；For pylorus ligation and the gastric ulcer of aspirin-induced, there is significant protective effect, and can effectively suppress right Gastric secretion；Its total alkaloids also has protective effect to ischemic myocardial.

12, Radix Paeoniae Rubra is Paeoniaceae plant peony (Paeonia Lacti floraPall.) or river Radix Paeoniae Rubra (P.veit chii Lynch) dry root, nature and flavor are bitter, are slightly cold, return Liver Channel, have effect of clearing away heat and cooling blood, eliminating stasis to stop pain.For maculae caused by violent heat pathogen, tell Blood epistaxis, conjunctival congestion and swelling pain, hypochondriac pain due to stagnation of liverQI, amenorrhea dysmenorrhea, lump in the abdomen stomachache, injury from falling down, carbuncle skin infection.The main of Radix Paeoniae Rubra effectively becomes Divide the methods of glycosides mainly with peoniflorin as representative, including paeoniflorin (paeoniflorin), oxypaeoniflorin (oxy- Paeoniflorin) etc..Again containing dextrorotation cachou extract (catechin) and volatile oil.Benzoic acid (benzoic acid) is volatile oil Main component, paeonol (paeonol) and other alcohols and phenols component totally 33.Tool antithrombus formation, antiplatelet aggregation, Blood fat reducing and arteriosclerosis effect.

13, the Radix Aucklandiae returns spleen；Stomach；Liver；The pungent acrid in the mouth of lung meridian；Bitter；Warm in nature.Have and regulate the flow of vital energy in tune, drying dampness to eliminate phlegm promoting the circulation of QI to relieve pain；Adjust Middle intestinal stasis relieving.Main born of the same parents coerce distension foot；Abdominal distention；Tell and have loose bowels；Weight after dysentery.After breast gastral cavity distending pain, dysentery, weight, food stagnation are not Disappear, anorexia, there is antibacterial action.Its pungent temperature is fragrant to be dissipated, and can rise and can drop, lead to the gas managing three Jiao, especially benefaction gastrointestinal gas and Pain relieving, has the merit of strengthening the spleen to promote digestion concurrently, is usually used in all cards caused by all taste QI stagnation of the large intestine.

Two, the determination of preparation technology

1 decoction pieces source

Decoction pieces used is purchased from Guizhou Ji Rentang pharmaceutcal corporation, Ltd, identified meets " Chinese Pharmacopoeia " version one in 2010 Relevant regulations under portion and " Guizhou Province's Chinese crude drug, Ethnic crude drugs quality standard " version each medical material (decoction pieces) item in 2003.

2 process routes determine, preferably

The determination of 2.1 extracting method

The Chinese medicine preparation extracting method for the treatment of endometriosis is based on the chemical composition character of each flavour of a drug in prescription Study with modern pharmacology, and combine the factor designs such as industrialized production reality.

Containing sufficiently complex chemical composition in Sanguis Draxonis.According to the structure of phenolic compound, chalcone derivative can be roughly divided into, The polymer of 2-hydrogen chalcone derivative, flavanone, flavone, flavonoid, chromone class, flavone compound and other phenolic compound.Mesh Front separated to steroidal, triterpene substance 21 kinds.Outside including the compound such as phenols, steroidal saponin, there is also other structure The compound of type, such as: alkane, acids, esters etc..Can obtain from the current research overview about its chemical composition, Sanguis Draxonis master Wanting composition is phenoloid, is wherein main status with flavone compound.Cure mainly according to we's function, take its water extract-alcohol precipitation Fractions.

Chemical composition in Rhizoma Sparganii is mainly volatile oil, organic acid, steroid, flavonoid, Phenylpropanoid Glycosides class etc..In recent years Come, constantly have new component, new activity to be found.At present, it has therefore proved that its total flavones has antiplatelet aggregation, antithrombotic, analgesia Effect.Available water extract-alcohol precipitation extracts.

Herba Polygoni cymosi chemical composition has phenols, organic acid, alkaloid, aminoacid, tannin, flavone, anthraquinone, glycoside, saccharide, plants Thing sterol and triterpenes etc..In root isolation identification go out cupreol, trans-p-Coumaric Acid methyl ester, Quercetin, Quercetin- The compounds such as 3-O-β-D-Glucose glycoside, rheum emodin, physcione and aloe-emodin.Med Mat Appreciation kaempferol, Cortex querci dentatae Element, storage glycosides, Quercetin-3-O-β-D-Glucose aldehydic acid methyl ester, Quercetin-3-β-D-Glucose aldehydic acid N-butyl, kaempferol-3- The flavone compounds such as O-rutinoside, rutin.Effective ingredient can be proposed to greatest extent with ethanol extraction.

Active component main in Radix Et Rhizoma Rhei is anthraquinone derivatives.Anthraquinone derivatives includes anthrone class rheum emodin, Radix Et Rhizoma Rhei Acid, chrysophanol, physcione, aloe-emodin and chrysaron etc.；Radix Et Rhizoma Rhei is possibly together with Radix Et Rhizoma Rhei anthraquinone analog derivative and Fructus Vitis viniferae Glycoside that sugar is combined into and anthrone class, such as Sennoside A, B, C, D, E, F etc., and other glycosides, tannin, compound of polysaccharide, organic Compound and inorganic matter etc..Effective ingredient can be proposed to greatest extent with ethanol extraction.

Pharmacological component main in Radix Angelicae Sinensis is volatile oil, polysaccharide etc..Possibly together with sucrose, fructose, glucose；Vitamin A, vitamin B12, vitamin E；17 kinds of aminoacid and sodium, potassium, calcium, magnesium etc. more than 20 plant inorganic elements.According to we function master Control, take its water extract-alcohol precipitation fractions.

The active component of Rhizoma Curcumae is volatile oil, and content is 1.9%～2.5%.In recent years the composition in volatile oil was carried out Research, in oil, main chemical compositions is multiple sesquiterpenoids material.Possibly together with zinc, ferrum, nickel, manganese, magnesium, cadmium, copper, molybdenum, cobalt, The various trace elements such as vanadium, phosphorus, calcium, gallium.Available water extract-alcohol precipitation extracts.

Poria is mainly composed of polysaccharide, accounts for the 9.3% of dry weight, in addition possibly together with triterpenoid compound.Also containing fat Fat acid, such as octanoic acid, undecanoic acid, lauric acid, lauric acid/dodecanoic acid and Palmic acid.Additionally, also ergosterol, natural gum, chitin, albumen Matter, fat, sterol, lecithin, D-glucose, adenine, histidine, choline, lipase, protease etc..According to we's merit Can cure mainly, take its water extract-alcohol precipitation fractions.

Ramulus Cinnamomi main active is volatile oil, and volatile oil content reaches 0.6%, additionally containing benzyl formate, acetic acid meat ester, Coumarin, Rhizoma Acori Graminei alkene etc..Available water extract-alcohol precipitation extracts.

The composition being separated in Cortex Moutan is more complicated, but main with phenol and phenolic glycoside class, monoterpene and glycoside thereof, and other also have three Terpene, sterol and glycoside thereof, flavone, organic acid, coumarin etc..Phenol and phenolic glycoside class phenol and phenolic glycoside compounds content in Cortex Moutan Higher, the phenol and the phenolic glycoside compounds that are separated to from Cortex Moutan have: paeonol, Cortex Moutan phenolic glycoside, the former glycosides of paeonol, paeonol Newly.Available water extract-alcohol precipitation extracts.

The main chemical compositions of Fructus Corni is iridoid glycosides, Pentacyclic triterpenic acid and esters thereof, tannin class, polysaccharide. Its volatile ingredient mainly has: Palmic acid, isobutanol, isoamyl alcohol, elemicin, furfural, methyleugenol, different asarone, β- Phenethanol etc..Glucoside and glycoside unit include: venbenalin, morroniside, swertianolin, Semen Strychni glycoside, iridoids, Fructus Vitis viniferae Sugar, fructose and sucrose.Effective ingredient can be proposed to greatest extent with ethanol extraction.

The main chemical compositions of Rhizoma Corydalis is isoquinoline type alkaloid, can be divided into two kinds according to its dissolubility in water, Tertiary amine base is the most insoluble or the person that is insoluble in water；Person more soluble in water belongs to quaternary amine alkali.Up to the present, therefrom isolate and pass through knot The existing kind more than 40 that structure is identified, its type is belonging respectively to again proto-berberine, aporphine, protopine class, isoquinolin benzyl miaow Azole, isoquinolin benzo phenanthridines class, double benzyl different beautiful jade class etc..Effective ingredient can be carried to greatest extent with ethanol extraction Go out.

The principle active component of Radix Paeoniae Rubra is that the methods of glycosides with peoniflorin as representative is containing paeoniflorin, oxypaeoniflorin etc..Again Containing dextrorotation cachou extract and volatile oil.Volatile oil is mainly containing benzoic acid, paeonol and other alcohols and phenols component totally 33.Available Decoction and alcohol sedimentation technique extracts, and method is more ripe.

Costus root oil master chemical composition Han lactone, content reaches 50%.Available water extract-alcohol precipitation extracts.

2.2 process routes determine

According to the chemical composition character of each flavour of a drug in prescription, cure mainly in conjunction with prescription function and said extracted methods analyst knot Really, intend Herba Polygoni cymosi, Fructus Corni, Rhizoma Corydalis, rhubarb medicinal material in prescription are added ethanol extraction, filter, obtain alcohol extract, standby.Prescription In remaining 9 taste medicine extracting in water, filter, obtain Aqueous extracts, concentrate, obtain condensed water extract, add ethanol in proper amount precipitate with ethanol, it is heavy to discard Form sediment, obtain precipitate with ethanol supernatant, standby.Alcohol extract mixes with precipitate with ethanol supernatant and is concentrated to give concentrated solution (recovery ethanol).Concentrated solution is dried, Obtain extractum extract, pulverize and sieve.Add adjuvant to pelletize, granulate, to obtain final product.Draft process route as shown in Figure 1.

2.3 alcohol extraction process conditions are preferred

2.3.1 the investigation of alcohol rate inhaled by medical material

Medical material three parts, Herba Polygoni cymosi 4.5g, Fructus Corni 10g, Rhizoma Corydalis 7.5g and Radix Et Rhizoma Rhei is weighed by a prescription proportional quantities 12g, altogether 34g, add the soak with ethanol of 5 times amount, observes every 30min and once soaks situation, till being impregnated with medicated core, presses Formula tries to achieve weight in wet base result, and result is as shown in table 1:

The investigation of alcohol rate inhaled by table 1 medical material

As shown in Table 1, when adding alcohol extraction first, the suction alcohol amount of medical material 108% should be supplied, for convenience of production calculation, first When adding alcohol extraction, adding a times amount ethanol with whole alcohol extraction medical materials, the ethanol inhaling alcohol amount to be added with theory is more or less the same, therefore The ethanol adding a times amount first during alcohol extraction is that comparison is rational.

2.3.2 concentration of alcohol and other factors is preferred

(1) concentration of alcohol preferably select the concentration of ethanol to be respectively as follows: 80% according to quercetin component in Herba Polygoni cymosi, 70%, 60% carries out investigating screening.

(2) if extraction time when preferably consideration produces greatly of extraction time is the shortest, effective ingredient is relatively difficult to extract completely, And the extraction time long cost that can improve, and lose time, therefore extraction time is chosen as tri-kinds of levels of 1h, 1.5h, 2h and investigates.

(3) extraction time the most according to a conventional method, selective extraction number of times be respectively the most once, twice, three times investigate.

(4) quantity of solvent preferably weighs 4 taste pharmaceutical decocting pieces, add the solvent of 5 times amount just can submergence medical material, and solubilization dosage is too Greatly not only waste solvent, and cause cost to increase, in conjunction with considering the suction alcohol rate of medical material, therefore to select quantity of solvent be 6 times, 8 times, 10 Times amount is investigated.

2.3.3 method and result

(1) method is to seek 4 optimum process condition of ethanol extraction of taste medical material such as Herba Polygoni cymosi, Rhizoma Corydalis, intends with orthogonal Test table L9 (3⁴) carry out orthogonal test, so that it is determined that optimal ethanol extraction condition.Orthogonal design table is as shown in table 2.

Table 2 L9 (3⁴) orthogonal test factor and level

The preparation of sample solution takes the medical material 17g altogether of half recipe quantity, selects orthogonal table to press the test side of orthogonal trial Case is carried out, and the alcohol extract of gained, through filtering, being concentrated into 100mL, to obtain final product.

Index components selected with Quercetin in Herba Polygoni cymosi and paste-forming rate as index components, preferably alcohol extraction optimum extraction work Skill.

Reference substance solution is prepared precision and is weighed Quercetin reference substance in right amount, adds methanol and makes every 1mL 0.09mg Han Quercetin Solution, to obtain final product.

Need testing solution is prepared precision and is measured sample 10mL under " preparation of sample solution " item, puts in beaker and volatilizes, accurate Addition 50mL methanol: hydrochloric acid=4:1 solution, weighed weight, 90 DEG C of water-bath reflux, extract, 1h, lets cool, more weighed weight, uses methanol Supply the weight of less loss, shake up, filter, take subsequent filtrate, to obtain final product.

Dry cream rate measures precision and measures sample solution under 50mL " preparation of sample solution " item, is concentrated into certain density, puts Water bath method in the evaporating dish of constant weight, 105 DEG C of dry 3h, to constant weight, put cooling 30min, its matter the most accurately weighed in exsiccator Amount, calculates the rate that gets dry extract.

The extractum weight of W50mL:50mL sample solution

V is total: population of samples amasss

W medical material: medical material weight

(2) quercetin content measurement result

Chromatographic condition Agela promosil C18 (250mm × 4.6,5 μm)；With methanol-0.4% phosphate aqueous solution= 50:50 is flowing phase；Detection wavelength is 360nm；Flow velocity: 1.0mL/min；Column temperature: 30 DEG C；In terms of Quercetin theoretical cam curve not Less than 3000.As shown in Figure 2, Figure 3 and Figure 4.

It is appropriate that standard curve precision weighs Quercetin reference substance, and add methanol dissolving making mass concentration is the right of 90 μ g/mL According to product solution, inject HPLC by the chromatographic condition drafted and measure.Quercetin sample size is respectively 0.1 μ L, 0.3 μ L, 0.5 μ L, 1 μ L、2μL.With peak area, sample introduction quality is carried out linear regression, obtain the regression equation of each tested composition, correlation coefficient and linear model Enclose.Result is as shown in table 3 and Fig. 5: Quercetin mass concentration in 0.009～0.180 μ g range in good linear relation.

Table 3

(3) Orthogonal Experiment and Design and result

The medical material 17g altogether of half recipe quantity is weighed, by L9 (3 by prescription⁴) orthogonal test condition extracts respectively, filter, just Step is concentrated into a certain amount of, obtains test liquid.With quercetin content, receipts cream rate as index, use overall merit (overall merit=Cortex querci dentatae Cellulose content/Quercetin maximum level × 80-receives cream rate/maximum and receives cream rate × 20) it is index, obtain optimised process.Result such as table 4, Shown in table 5 and table 6.

Table 4 orthogonal experiments

Table 5 orthogonal test variance analysis

Table 6 orthogonal experiment comprehensive grading result

From table, Orthogonal experiment results understands, and it is extraction time that each factor affects the order of alcohol extraction technique > concentration of alcohol > Ethanol consumption>extraction time, wherein extraction time C, concentration of alcohol A have significance (P<0.05) to affect, therefore, according to orthogonal examination Testing result, extraction time C most preferably selects C2, concentration of alcohol A most preferably to select A3；And ethanol consumption B, extraction time D there was no significant difference, Producing in conjunction with big, preferably optimum process condition is A3B2C2D1.The ethanol solution i.e. adding 8 times amount 80% extracts 2 times, each 1h.

2.3.4 test is verified

Weigh the medical material 17g altogether of half recipe quantity, carry out checking test, as shown in table 7, knot by preferred plan A3B2C2D1 Fruit coincide with orthogonal experiments.Illustrate that this process stabilizing is feasible.It is thus determined that alcohol extraction process is: the ethanol of 8 times amount 80% is molten Liquid reflux, extract, 2 times, each 1h.

Table 7 alcohol extraction process the result

2.4 abstract methods techniques are preferred

2.4.1 the investigation of medical material water absorption rate

Medical material three parts, Cortex Moutan 8g, Poria 10g, Ramulus Cinnamomi 6.5g, Radix Angelicae Sinensis 8g, Rhizoma Sparganii 6.5g, cowherb is weighed by prescription proportional quantities Art 6.5g, Radix Paeoniae Rubra 6.5g, Radix Aucklandiae 8g and Sanguis Draxonis 3g, 63g altogether, add the water soaking of 7 times amount, observe every 30min and once soak Bubble situation, till being impregnated with medicated core, tries to achieve weight in wet base result as the following formula, and result is as shown in table 8:

The investigation of table 8 medical material water absorption rate

As shown in Table 8, first during extracting in water, the water absorption of medical material 102% should be supplied, for convenience of production calculation, first During extracting in water, carrying medical material with whole water and add a times amount water, the water to be added with theoretical water absorption is more or less the same, first The water adding a times amount when water puies forward is that comparison is rational.

2.4.2 water carries the preferred of factor level

(1) amount of water selects to weigh 9 taste pharmaceutical decocting pieces, add the water of 5 times amount just can submergence medical material, take medical material into consideration Water absorption rate, therefore selecting amount of water is 6 times, 8 times, 10 times amount investigations.

(2) if extraction time when preferably consideration produces greatly of extraction time is the shortest, effective ingredient is relatively difficult to extract completely, And the extraction time long cost that can improve, and lose time, therefore extraction time is chosen as tri-kinds of levels of 1h, 1.5h, 2h and investigates.

(3) extraction time the most according to a conventional method, selective extraction number of times be respectively the most once, twice, three times investigate.

2.4.3 method and result

(1) method is to seek 9 optimum process condition of water extraction of taste medical material such as Sanguis Draxonis, Ramulus Cinnamomi, intends with orthogonal test Table L9 (3⁴) carry out orthogonal test, so that it is determined that optimal water extraction condition, as shown in table 9.

Table 9 L9 (3⁴) orthogonal test factor and level

The preparation of sample solution takes the medical material 31.5g altogether of half recipe quantity, selects orthogonal table to press the test of orthogonal trial Scheme is carried out, and the Aqueous extracts of gained, through filtering, being concentrated into 100mL, to obtain final product.

Index components selected with peoniflorin in Radix Paeoniae Rubra and paste-forming rate as index, preferably water carries optimum extraction process.

Reference substance solution is prepared precision and is weighed peoniflorin reference substance in right amount, adds methanol and is respectively prepared every 1ml containing peoniflorin 257 The solution of μ g, to obtain final product.

Need testing solution is prepared precision and is measured sample 10mL under " preparation of sample solution " item, puts in beaker and volatilizes, accurate Add 25mL methanol solution, weighed weight, supersound process 30min, let cool, more weighed weight, the weight of less loss is supplied with methanol, Shake up, filter, take subsequent filtrate, to obtain final product.

Dry cream rate measures precision and measures sample solution under 50mL " preparation of sample solution " item, is concentrated into certain density, puts Water bath method in the evaporating dish of constant weight, 105 DEG C of dry 3h, to constant weight, put in exsiccator cooling 30min, and the most accurately weighed it is heavy Quality, calculates the rate that gets dry extract.

The extractum weight of W50mL:50mL sample solution

V is total: population of samples amasss

W medical material: medical material weight

(2) paeoniflorin content measurement result

Peoniflorin chromatographic condition Agela promosil C18 (250mm × 4.6,5 μm)；With methanol-0.5mol/L phosphoric acid Potassium dihydrogen solution=40:65 is flowing phase；Detection wavelength is 230nm；Flow velocity: 1.0mL/min；Column temperature: 30 DEG C；Manage with peoniflorin Opinion number of plates meter is not less than 3000.As shown in Fig. 6, Fig. 7 and Fig. 8.

It is appropriate that standard curve precision weighs peoniflorin reference substance, adds methanol dissolving and makes mass concentration 257 μ g/ml's respectively Reference substance solution, injects HPLC by the chromatographic condition drafted and measures.Peoniflorin sample size be respectively 2.5 μ L, 5 μ L, 12.5 μ L, 20 μL、25μL.With peak area, sample introduction quality is carried out linear regression, obtain the regression equation of each tested composition, correlation coefficient and linear Scope.Result is as shown in table 10 and Fig. 9: peoniflorin mass concentration in 0.64～6.42 μ g range in good linear relation.

Table 10

Orthogonal Experiment and Design and result

The medical material 31.5g altogether of half recipe quantity is weighed, by L9 (3 by prescription⁴) orthogonal test condition extracts respectively, filter, Initial concentration, to a certain amount of, obtains test liquid.With paeoniflorin content and dry cream rate as index, use overall merit (overall merit= Paeoniflorin content/maximum paeoniflorin content × 80-dry cream rate/maximum dry cream rate × 20) it is index, obtain optimised process.Result is such as Shown in table 11～table 13.

Table 11 Orthogonal experiment results

Table 12 orthogonal experiment variance analysis

Table 13 orthogonal experiment comprehensive grading result

From table, Orthogonal experiment results understands, and it is extraction time that each factor affects the order in water extraction process > amount of water > Extraction time, wherein extraction time A has significance (P < 0.05) to affect, and therefore according to orthogonal experiments, extraction time A is optimal Select A2；And ethanol consumption B, extraction time C there was no significant difference, in conjunction with big Production requirement, preferably optimum process condition it is A2B1C1.I.e. add 6 times amount water extraction 2 times, each 1h.

2.4.4 test is verified

Weigh the medical material 31.5g altogether of half recipe quantity, carry out checking test, result such as table 14 institute by preferred plan A2B1C1 Show.Result is coincide with orthogonal experiments.Illustrate that this process stabilizing is feasible.It is thus determined that it is 6 times amount water extraction 2 that water put forward work to add skill Secondary, each 1h.

Table 14 extraction process by water the result

2.5 Aqueous extracts impurity removal process are preferred

Chinese crude drug is after water carries, and often containing starch, polysaccharide, protein, pectin etc. in its liquid, causes final prepared consolidating Body preparation taking dose is excessive, is purified so generally dealing with extracting solution, reduces the content of unrelated composition in preparation, reduces clothes Use dosage.In production, the certain density alcohol of many employings carries out precipitate with ethanol impurity removal process.

2.5.1 different alcohol precipitation concentrations are preferred

Weigh the medical material 63g of 3 parts of recipe quantities respectively, add 6 times amount water extraction secondaries, each 1 hour, obtain Aqueous extracts Concentrating, add a certain amount of ethanol, controlling feed liquid concentration of alcohol respectively is 40%, 50%, 60% precipitate with ethanol, after standing 12 hours Obtaining alcohol deposit fluid, reconcentration drying under reduced pressure obtains 3 parts of dry cream respectively, and result is as shown in Table 15.

Table 15 water extract-alcohol precipitation concentration of alcohol comparative result

By found that the purification effect feed liquid concentration of alcohol compared with 60% of 40%, 50% is poor, final dosage is still Bigger.The feed liquid concentration of alcohol purification effect of 60% is preferable, effectively reduces dosage, and the concentration of alcohol of feed liquid is less than 65%, can effectively preserve the effective ingredient such as polysaccharide of prescription, alcohol precipitation concentration to change the impact on paeoniflorin content little, therefore really The feed liquid concentration of alcohol determining Aqueous extracts precipitate with ethanol purification is 60%.

2.6 concentrations and drying process are preferred

Composition and the character of Chinese medicine extraction liquid Chinese medicine are complex, in concentration, dry run, due to heated time relatively Long, its some effective ingredient contained may be destroyed to some extent, and makes its active constituent content reduce, and have impact on preparation Clinical efficacy.Concentrate drying is the important step that Chinese medicine preparation produces, and selects different concentrate drying modes, will affect finished product Active constituent content, water capacity, outward appearance, color and luster, granularity, dissolubility and hygienic requirements thereof etc. and it is necessary to combine its produce Scale and production capacity consider concentrate drying technique.The most conventional concentrate drying method is divided into four kinds, has normal pressure to concentrate Seasoning, concentrating under reduced pressure seasoning, the various ways such as spray drying method and micro-wave drying method.Concentrating under reduced pressure has and prevents from effectively becoming Point decompose, high efficiency, the shortest, the advantage of energy efficient etc., the big consideration produced after combining, therefore this process choice reduces pressure dense Contracting.With the rate of transform of Quercetin, paeonol and peoniflorin as evaluation index, to normal pressure and vacuum drying with in condition of different temperatures Under drying process investigated.

2.6.1 different drying modes are preferred

Weigh the medical material 48.5g altogether of half recipe quantity, carry out alcohol by preferred plan respectively and mention that water carries, remix extracting solution Concentrating under reduced pressure, to certain density, compares constant pressure and dry, drying under reduced pressure difference drying mode, by investigate Quercetin, paeonol and The content of peoniflorin be dried before and after contrast, fragitity, color, drying time etc., factor, determined optimum drying mode.Result is such as Shown in table 16.

The impact of the different drying mode of table 16

As shown in Table 16, consider Quercetin, paeonol and peoniflorin be dried before and after content balance, fragitity, face Color, on the basis of drying time, selects vacuum drying for optimum drying mode.

2.6.2 different temperatures is on vacuum drying impact

Weigh the medical material 48.5g altogether of half recipe quantity, carry out alcohol by preferred plan respectively and mention that water carries, remix extracting solution Concentrating under reduced pressure, to certain density, compares and is vacuum dried 80 DEG C, 70 DEG C, the baking temperature of 60 DEG C.Result is as shown in table 17.

The impact of table 17 different vacuum drying time

As shown in Table 17, it is considered to drying efficiency, Quercetin, paeonol, the rate of transform of peoniflorin raise with temperature and reduce. Although the drying time of 80 DEG C is shorter, but content has larger difference.The content difference of 60 DEG C and 70 DEG C is less, but 60 DEG C are dried effect Rate is low compared with 70 DEG C, considers from the big efficiency produced, determines that 70 DEG C of vacuum is dried.

(by version " Chinese Pharmacopoeia " requirement in 2010) is calculated after measured, Radix Paeoniae Rubra medical material Radix Paeoniae in test in early stage preliminary experiment Glycosides content is 19mg/g, and Herba Polygoni cymosi medical material quercetin content is 1.55mg/g.By to the extraction of preparation, purification, concentrate and dry Drying process is investigated preferably, finally gives the dry plaster powder of preparation.In the target component that preparation is selected, calculate after measured in Radix Paeoniae Rubra The rate of transform of the Quercetin in peoniflorin and Herba Polygoni cymosi respectively reaches 76% and 61%, illustrate selected extraction, purification, concentration and Drying process is stable, feasible.

2.7 moulding processs determine

2.7.1 dosage form is preferred

The Chinese medicine preparation recipe quantity for the treatment of endometriosis is 97g, the most once with decoction, evident in efficacy.For Increase its clinical adaptability, by this prescription under the guidance of Chinese medical theory, use the theory of modernization, technology, method to press It is processed into certain dosage form according to recipe quantity.Physicochemical property according to each medical material ingredient and modern pharmacological research result and each dose The feature of type, it is believed that if making liquid preparation, the then poor stability of preparation, preserve, transport inconvenience.The present invention once considered by Capsule made by this prescription, but is 97g according to the recipe quantity of its clinical application, according to the rate of extract total after its water extract-alcohol precipitation and alcohol extraction Generally 15%, fill No. 0 capsule, every 0.5g, in the case of being not added with adjuvant, need every day to take 30, which adds The burden of taking medicine of patient.Therefore consider to make this prescription granule, and increasing the adaptability that patient takes, granule is at human body the intestines and stomach In road, disintegrate is rapid, absorbs fast, and is readily transported, carries and takes, and in the case of the curative effect ensureing this prescription, adds steady Qualitative, it is achieved the modernization of this prescription and economic society are worth.

The method of granule the most processed is preferred

Granule processed dry extract can be divided into pelletize according to the method for granulating of different material and thick paste is pelletized.This experiment considers alcohol Carry solution and water carries solution and is concentrated into relative density 1.30～1.35, add 3～5 times of granulations that adjuvant amount is extractum, result in The dose of medicine increases, therefore the dry cream of this experimental selection is pelletized.

2.7.3 adjuvant is preferred

(1) anti-moisture absorption agent and excipient are because the dried cream powder of the Chinese medicine granules for the treatment of endometriosis is in the process of preservation In the easily moisture absorption, therefore consider to select suitable adjuvant as anti-moisture absorption agent and excipient.The present invention intends selecting dextrin, solubility to form sediment Powder, lactose are as excipient, and when in preliminary experiment, soluble starch is cooked anti-moisture absorption agent and excipient, the viscosity of soft material is low, granule Molding and mobility are all preferable, and anti-moisture absorption capacity is strong, and soluble starch is water insoluble and ethanol, the most stable, Moisture absorption and not deliquescence.The chemical property of soluble starch is the most stable, inoperative with most medicine, cheap.

(2) correctives select due to treatment endometriosis Chinese medicine granules raise dried cream powder through alcohol extraction and water After, its bitter and puckery flavor, it is more difficult in directly oral, therefore consider that adding certain correctives improves its bad smell.Consider that add rectifys Taste agent has 0.2% aspartame, 0.5% cyclamate or directly replaces part soluble starch as adjuvant with sucrose.Preliminary experiment Show that adding 0.2% aspartame can be effectively improved the taste of its bitterness.

2.7.4 excipient and medicated powder ratio

Medicated powder is pelletized by different mass ratio 3:4,1:1,4:3,2:1 from soluble starch, observes its granulating efficiency, suction Moist and outward appearance, the results are shown in Table 18:

Table 18 soluble starch investigates result with medicated powder ratio

From table 18, when the mass ratio of medicated powder Yu soluble starch is 1:1, granule is nonhygroscopic, effect is best, becomes Type rate is high, therefore determines that medicated powder is 1:1 with the best in quality ratio of soluble starch.

2.7.5 wetting agent is preferred

In order to better ensure that stability and its ratio of briquetting of preparation, this experiment is intended with 80%, 85%, 90%, 95% Ethanol carries out research of pelletizing, and the results are shown in Table 19:

Table 19 different wetting agent granulation situation

The above results shows, pelletizes with 90% ethanol for wetting agent, soft material moderate viscosity processed, it is easy to pelletize, gained granule The most moderate, good forming effect, therefore select to make wetting agent with the ethanol of 90%.

2.7.6 the performance indications of granule

(1) bulk density measures and weighs 2g medicated powder (crossing No. four sieves), loads in 10mL graduated cylinder, falls for several times with certain altitude (keeping consistent), make degree of tightness suitable, with weight and calculation of capacity bulk density, bulk density=weight (g)/volume as far as possible (mL).The results are shown in Table 20:

Table 20 3 batch sample bulk density measurement result

(2) angle of repose, funnel was drawn a circle to approve on the diagram paper of horizontal positioned by mensuration, and the funnel end opening distance away from diagram paper is H, pours funnel into granule until the outlet of funnel and round can nib contacts, measures cone base diameter (2R) and circular cone is high (H), θ is calculated according to tan θ=H/R.The results are shown in Table 21:

Table 21 3 batch sample measurement result angle of repose

Result shows that the average angle of repose of granule is 28.17 degree, illustrates that the mobility of granule is preferable.

2.7.7 the critical relative humidity of granule

Critical relative humidity is medicine moisture absorption whether marginal value, simultaneously can also be according to it is determined that environmental wet when producing Degree.Prepare sulphuric acid or the saturated solution of different salt of variable concentrations respectively, be respectively placed in 96h in constant temperature (25 DEG C) exsiccator, make Its interior humidity balance constitutes the environment of different relative humiditys, the results are shown in Table 22:

The sulphuric acid of table 22 variable concentrations or the supersaturated solution of the different salt relative humidity when 25 DEG C

The powder prepared is dried to constant weight, bottom the weighing botle of constant weight, puts into the granule of thick about 2mm, accurately The exsiccator weighing the supersaturated solution being placed on the sulphuric acid filling 6 kinds of variable concentrations respectively listed by table or different salt (claims Measuring bottle lid is opened), in 25 DEG C of constant incubators, moisture absorption is to constant weight, precision weighing, calculates its Moisture percentage.The results are shown in Table 22。

With relative humidity as abscissa, hydroscopicity is vertical coordinate, draws sucting wet curve, sees Figure 10.By sucting wet curve straight line This curve tangent line is done at two ends, and two intersections of complex curve abscissas are critical relative humidity (CRH), and critical relative humidity is 60%, because of This should control relative humidity at the environment pulverized, pelletize, pack and store and be less than 60%, and uses moistureproof good packaging.

Three, scale up test

Feed intake by 1000 preparation unit amount times raw materials, prepare by above-mentioned optimised process, manufacture experimently three batch pilot scale finished products, and Detect by the requirement under quality standard and medicine granule item, the results are shown in Table 23,24.

The raw material input amount of 23 1000 preparation prescription amounts of table

Table 24 pilot scale finished product detection data

From scale up test result of study in table, use the moulding process optimized, its ratio of briquetting up to 90%, and three batches The ratio of briquetting of finished product is basically identical, have detected the many index of finished product simultaneously, is computed in Radix Paeoniae Rubra Mongolian oak in peoniflorin and Herba Polygoni cymosi The rate of transform of Pi Su respectively reaches 71% and 52%, shows that this technique is simple, feasible, stable.

Four, this preparation prescription is used for clinical experimental study, and its research is as follows:

4.1, clinical data

4.1.1, physical data

126 example patients, year mean age (33.5 ± 6.3).

4.1.2, diagnostic criteria

With reference to the 3rd academic conference revised standard of department of obstetrics and gynecology Professional Committee of CAIM (Chinese Association Of Integrative Medicine).All cases All combine clinical gynecologial examination, B-type ultrasonography diagnosis, some cases combine CT, MRI, CA125 value, laparoscopy and Postoperative pathological examination inspection is diagnosed as endometriosis.

Waist and sacrum pain, dysmenorrhea 86 example in main clinic symptoms and sign 126 example patient, menoxenia 43 example, infertile 15 Example.Gynecologial examination has obvious painful tubercles 71 example, B ultrasonic prompting myometrial gland tumor 41 example, chocolate cyst of ovary 34 example, Qi Zhongshuan Side person 16 example, cyst maximum gauge is 8.7cm.

4.2, treatment and observational technique

4.2.1, Therapeutic Method

(1) treatment

When observing clinical efficacy, use decoction.Compound recipe dragon pellet decoction use: Sanguis Draxonis 3g, Radix Et Rhizoma Rhei 12g, Fructus Corni 10g, when Return 8g, Cortex Moutan 8g, Radix Aucklandiae 8g, Rhizoma Corydalis 8g, Radix Paeoniae Rubra 6g, Poria 10g, Rhizoma Curcumae 6g, Herba Polygoni cymosi 5g, Ramulus Cinnamomi 5g and Rhizoma Sparganii 5g, Every day 1 dose.For ease of taking, by 10 agent medicines with decocting 3 times, gained concentration of liquid medicine becomes 1000mL, 4 DEG C of Refrigerator stores, every day 2 Secondary, each 50mL, heats when taking oral.

(2) course for the treatment of was 1 course for the treatment of with 6 months.

4.2.2, observation index and method

(1) main clinic symptoms and sign: the symptoms such as waist and sacrum pain, dysmenorrhea, menoxenia are pressed light and heavy degree marking, Asymptomatic person 0 point；Mild 1 point；Medium disease 2 points；Serious symptom 3 points.Examine, obtained by ultrasound diagnosis according to gynecological's bimanual examination, three conjunctions The sign such as painful tubercles, endometrial cyst and pelvic adhesion pathological changes is divided into gently, in, severe.Without obvious sign person 0 point；Slight 1 Point；Moderate 2 points；Severe 3 points.Gynecologial examination in every 4 weeks 1 time in drug administration process, ultrasound diagnosis 1 time in every 8 weeks, dynamically observe 2 groups of cases Clinical symptoms and the degree of improvement of sign.

(2) observe drug side effect situation, follow up a case by regular visits to gestation and recurrence.

4.3, therapeutic outcome

4.3.1, criterion of therapeutical effect

The criterion of therapeutical effect formulated according to the 3rd academic conference of department of obstetrics and gynecology Professional Committee of CAIM (Chinese Association Of Integrative Medicine), 1. Recovery from illness: symptom all disappears, the local such as pelvic lump sign disappears substantially, and Sterility patient is gestation or fertility in 3 years；2. show Effect: symptom disappears substantially, and pelvic lump reduces, though or local sign exist, but infertile patient is become pregnant；The most effective: symptom Alleviating, pelvic lump is without increasing or slightly reducing, and in drug withdrawal 3 months, symptom does not increases the weight of；The most invalid: cardinal symptom is unchanged or dislikes Changing, local patholoic change has and increases the weight of trend.

4.3.2, result

The clinical data statistics of 126 example non-operative treatment gynecopathies, its total effective rate is 90.48%, 35 examples of wherein fully recovering (29.36%), effective 48 examples (38.09%), effective 31 examples (24.60%).

The invention have benefit that: the Chinese medicine preparation of the treatment endometriosis of the present invention, there is invigorating blood circulation The stasis of blood, the kidney invigorating takes off admittedly, and dissipate knot, effect of removing obstruction in the collateral to relieve pain.For married woman place block, silt resistance of suffering from a deficiency of the kidney, or caused by energy stagnation and blood stasis Menoxenia, premenstrual inferior belly gas pain, acute through row pain, pain draws waist sacrum, tenderness, and pudendum sky falls, or blockage of menstruation, hypomenorrhea or pouring Drenching endless, color is dark, has held clot under the arm, alleviation of pain under block, or with distending pain of the breast, headache and insomnia, hyposexuality, body of the tongue purple is dim, or While there is ecchymosis, thin fur, all cards such as deep-thready pulse or string；Endometriosis, hysteromyoma is shown in above-mentioned all card persons.Its therapeutic effect shows Writing, the clinical data statistics of 126 example non-operative treatment gynecopathies, its total effective rate is 90.48%, 35 examples of wherein fully recovering (29.36%), effective 48 examples (38.09%), effective 31 examples (24.60%).In the treatment endometriosis of the present invention Medicine preparation has the effect of good treatment endometriosis.The composition medicine of the present invention, is pharmacopeia and terrestrial reference is contained Common medicine, its aboundresources.The Chinese medicine preparation of the treatment endometriosis of the present invention is preferably granule, facilitates patient Take, real meaning accomplish " three little five just ", it is achieved the modernization of Chinese medicine.By to the extraction of this preparation, Study on Preparation, Excellent have selected relatively reasonable extracting factor and preparation process condition.The preparation technology of the present invention is simple, feasible, stable, Preparation condition gentleness is easy to control, simple to operate, it is easy to large-scale production.

Accompanying drawing explanation

Fig. 1 is the process chart of the present invention；

Fig. 2 is alcohol extract sample chromatogram figure in alcohol extraction selection process；

Fig. 3 is to lack Herba Polygoni cymosi negative sample chromatogram in alcohol extraction selection process；

Fig. 4 is Quercetin reference substance chromatogram in alcohol extraction selection process；

Fig. 5 is Quercetin canonical plotting in alcohol extraction selection process；

Fig. 6 is that water carries Aqueous extracts sample chromatogram figure in selection process；

Fig. 7 is that water carries scarce Radix Paeoniae Rubra negative sample chromatogram in selection process；

Fig. 8 is that water carries peoniflorin reference substance chromatogram in selection process；

Fig. 9 is that water carries peoniflorin canonical plotting in selection process；

Figure 10 is the intermediate sucting wet curve of the Chinese medicine granules for the treatment of endometriosis.

Detailed description of the invention

Below in conjunction with specific embodiment, the present invention is further introduced.

Embodiment 1

A kind of Chinese medicine preparation treating endometriosis, is made up of following crude drug: Sanguis Draxonis 53g, Radix Et Rhizoma Rhei 99g, Fructus Corni 198g, Radix Angelicae Sinensis 198g, Cortex Moutan 198g, Radix Aucklandiae 99g, Rhizoma Corydalis 99g, Radix Paeoniae Rubra 198g, Poria 293g, Rhizoma Curcumae 173g, Herba Polygoni cymosi 105g, Ramulus Cinnamomi 99g and Rhizoma Sparganii 165g.Prepare according to following steps: weigh according to quantity Herba Polygoni cymosi, Fructus Corni, Rhizoma Corydalis and Rhubarb medicinal material, adds 6～10 times amount 60%～80% ethanol, reflux, extract, 1～3 times, each 1～2h, filters, obtains alcohol extract, standby With；Weigh Sanguis Draxonis, Radix Angelicae Sinensis, Cortex Moutan, the Radix Aucklandiae, Radix Paeoniae Rubra, Poria, Rhizoma Curcumae, Ramulus Cinnamomi and Rhizoma Sparganii according to quantity, add 6～10 times amount water, decoct Boiling extraction 1～3 time, each 1～2h, filter, obtain Aqueous extracts, being evaporated to density through 75 DEG C is 1.05, obtains condensed water extract, Adding ethanol, stir, controlling concentration of alcohol in feed liquid is 40%～60%, stands 12h, discards precipitation, obtain on precipitate with ethanol Clear liquid, standby；Alcohol extract mixes with precipitate with ethanol supernatant, and 75 DEG C are evaporated to density is 1.25, obtains concentrated solution, concentrated solution 60 DEG C ～80 DEG C of vacuum drying 42～72h, obtain extractum extract, pulverized No. 5 sieves, and obtained powder, and added adjuvant and make various medicine Thing preparation.

Embodiment 2

A kind of Chinese medicine preparation treating endometriosis, is made up of following crude drug: Sanguis Draxonis 198g, Radix Et Rhizoma Rhei 495g, Fructus Corni 396g, Radix Angelicae Sinensis 396g, Cortex Moutan 396g, Radix Aucklandiae 330g, Rhizoma Corydalis 330g, Radix Paeoniae Rubra 396g, Poria 495g, cowherb Art 297g, Herba Polygoni cymosi 990g, Ramulus Cinnamomi 330g and Rhizoma Sparganii 330g.Prepare according to following steps: weigh according to quantity Herba Polygoni cymosi, Fructus Corni, Rhizoma Corydalis and rhubarb medicinal material, add 6 times amount 60% ethanol, reflux, extract, 1 time, each 2h, filter, obtain alcohol extract, standby；Claim according to quantity Take Sanguis Draxonis, Radix Angelicae Sinensis, Cortex Moutan, the Radix Aucklandiae, Radix Paeoniae Rubra, Poria, Rhizoma Curcumae, Ramulus Cinnamomi and Rhizoma Sparganii, first add 8 times amount water boiling and extraction 1 time, then With 7 times amount water boiling and extraction 2 times, each 1.5h, filtering, obtain Aqueous extracts, being evaporated to density through 75 DEG C is 1.05, obtains concentration Aqueous extracts, adds ethanol, stirs, and controlling concentration of alcohol in feed liquid is 40%, stands 12h, discards precipitation, obtain on precipitate with ethanol Clear liquid, standby；Alcohol extract mixes with precipitate with ethanol supernatant, and 75 DEG C are evaporated to density is 1.25, obtains concentrated solution, concentrated solution 60 DEG C Vacuum drying 57h, obtains extractum extract, pulverized No. 5 sieves, and obtained medicated powder, add solvable by the mass ratio of 1:1 in medicated powder Property starch, the aspartame accounting for medicated powder gross mass 0.2% with consumption makees correctives, makees wetting agent with the ethanol of 90% and pelletizes, Grain is dried in 60 DEG C～80 DEG C, and secondary is pelletized, and crosses No. 1 and screens out bulky grain, crosses No. 5 and screen out fine powder, obtain granule.This preparation Boiled water is taken after mixing it with water.Once two bags, three times on the one.Every packed 5g.

Embodiment 3

A kind of Chinese medicine preparation treating endometriosis, is made up of following crude drug: Sanguis Draxonis 103g, Radix Et Rhizoma Rhei 412g, Fructus Corni 343g, Radix Angelicae Sinensis 275g, Cortex Moutan 275g, Radix Aucklandiae 175g, Rhizoma Corydalis 257g, Radix Paeoniae Rubra 223g, Poria 343g, cowherb Art 223g, Herba Polygoni cymosi 155g, Ramulus Cinnamomi 223g and Rhizoma Sparganii 223g.Prepare according to following steps: weigh according to quantity Herba Polygoni cymosi, Fructus Corni, Rhizoma Corydalis and rhubarb medicinal material, add 9 times amount, 8 times amount 80% ethanol, reflux, extract, 2 times, each 1h respectively, filter, obtain alcohol extract, Standby；Weigh Sanguis Draxonis, Radix Angelicae Sinensis, Cortex Moutan, the Radix Aucklandiae, Radix Paeoniae Rubra, Poria, Rhizoma Curcumae, Ramulus Cinnamomi and Rhizoma Sparganii according to quantity, add respectively 7 times amount, 6 Times amount water, decocts and extracts 2 times, and each 1h filters, obtains Aqueous extracts, and being evaporated to density through 75 DEG C is 1.05, obtains condensed water and carries Liquid, adds ethanol, stirs, and controlling concentration of alcohol in feed liquid is 60%, stands 12h, discards precipitation, obtain precipitate with ethanol supernatant Liquid, standby；Alcohol extract mixes with precipitate with ethanol supernatant, and 75 DEG C are evaporated to density is 1.25, obtains concentrated solution, and concentrated solution 70 DEG C is true Empty dry 60h, obtains extractum extract, pulverized No. 5 sieves, and obtained medicated powder, and added solubility by the mass ratio of 1:1 in medicated powder Starch, the aspartame accounting for medicated powder gross mass 0.2% with consumption makees correctives, and the ethanol of 90% is made wetting agent and pelletized, and granule exists 60 DEG C～80 DEG C gradually rise warming middle-JIAO and are dried, and secondary is pelletized, and crosses No. 1 and screens out bulky grain, crosses No. 5 and screen out fine powder, obtain granule.This Preparation boiled water is taken after mixing it with water.Once two bags, three times on the one.Every packed 5g.

Embodiment 4

A kind of Chinese medicine preparation treating endometriosis, is made up of following crude drug: Sanguis Draxonis 150g, Radix Et Rhizoma Rhei 350g, Fructus Corni 220g, Radix Angelicae Sinensis 230g, Cortex Moutan 300g, Radix Aucklandiae 250g, Rhizoma Corydalis 240g, Radix Paeoniae Rubra 260g, Poria 310g, cowherb Art 200g, Herba Polygoni cymosi 800g, Ramulus Cinnamomi 260g and Rhizoma Sparganii 210g.Prepare according to following steps: weigh according to quantity Herba Polygoni cymosi, Fructus Corni, Rhizoma Corydalis and rhubarb medicinal material, first add 10 times amount 70% alcohol reflux 1 time, then adds 9 times amount 70% alcohol reflux 2 times, 1.5h every time, filters, obtains alcohol extract, standby；Weigh Sanguis Draxonis, Radix Angelicae Sinensis, Cortex Moutan, the Radix Aucklandiae, Radix Paeoniae Rubra, Poria, Rhizoma Curcumae, osmanthus according to quantity Branch and Rhizoma Sparganii, add 10 times amount water, decocts and extracts 1 time, and each 2h filters, obtains Aqueous extracts, and being evaporated to density through 75 DEG C is 1.05, obtain condensed water extract, add ethanol, stir, controlling concentration of alcohol in feed liquid is 50%, stands 12h, and it is heavy to discard Form sediment, obtain precipitate with ethanol supernatant, standby；Alcohol extract mixes with precipitate with ethanol supernatant, and 75 DEG C are evaporated to density is 1.25, obtains concentration Liquid, concentrated solution 80 DEG C vacuum drying 42h, obtain extractum extract, pulverized No. 5 sieves, and obtained medicated powder, by the mass ratio of 1:1 to Adding soluble starch in medicated powder, the aspartame accounting for medicated powder gross mass 0.2% with consumption makees correctives, and the ethanol of 90% is made to moisten Humectant is pelletized, and granule is dried in 60 DEG C～80 DEG C, and secondary is pelletized, and crosses No. 1 and screens out bulky grain, crosses No. 5 and screen out fine powder, obtain granule Agent.This preparation boiled water is taken after mixing it with water.Once two bags, three times on the one.Every packed 5g.

Embodiment 5

A kind of Chinese medicine preparation treating endometriosis, is made up of following crude drug: Sanguis Draxonis 80g, Radix Et Rhizoma Rhei 150g, Fructus Corni 330g, Radix Angelicae Sinensis 305g, Cortex Moutan 350g, Radix Aucklandiae 180g, Rhizoma Corydalis 120g, Radix Paeoniae Rubra 360g, Poria 390g, Rhizoma Curcumae 210g, Herba Polygoni cymosi 500g, Ramulus Cinnamomi 120g and Rhizoma Sparganii 300g.Prepare according to following steps: weigh Herba Polygoni cymosi, Fructus Corni according to quantity, prolong Rhizoma Corydalis and rhubarb medicinal material, add 8 times amount, 7 times amount 75% ethanol, reflux, extract, 2 times, each 1.5h respectively, filter, obtain alcohol extract, Standby；Weigh Sanguis Draxonis, Radix Angelicae Sinensis, Cortex Moutan, the Radix Aucklandiae, Radix Paeoniae Rubra, Poria, Rhizoma Curcumae, Ramulus Cinnamomi and Rhizoma Sparganii according to quantity, add respectively 9 times amount, 8 Times amount water, decocts and extracts 2 times, and each 2h filters, obtains Aqueous extracts, and being evaporated to density through 75 DEG C is 1.05, obtains condensed water and carries Liquid, adds ethanol, stirs, and controlling concentration of alcohol in feed liquid is 60%, stands 12h, discards precipitation, obtain precipitate with ethanol supernatant Liquid, standby；Alcohol extract mixes with precipitate with ethanol supernatant, and 75 DEG C are evaporated to density is 1.25, obtains concentrated solution, and concentrated solution 60 DEG C is true Empty dry 72h, obtains extractum extract, pulverized No. 5 sieves, and obtained medicated powder, and added solubility by the mass ratio of 1:1 in medicated powder Starch, the aspartame accounting for medicated powder gross mass 0.2% with consumption makees correctives, and the ethanol of 90% is made wetting agent and pelletized, and granule exists 60 DEG C～80 DEG C gradually rise warming middle-JIAO and are dried, and secondary is pelletized, and crosses No. 1 and screens out bulky grain, crosses No. 5 and screen out fine powder, obtain granule.This Preparation boiled water is taken after mixing it with water.Once two bags, three times on the one.Every packed 5g.

Embodiment 6

A kind of Chinese medicine preparation treating endometriosis, is made up of following crude drug: Sanguis Draxonis 135g, Radix Et Rhizoma Rhei 480g, Fructus Corni 270g, Radix Angelicae Sinensis 380g, Cortex Moutan 225g, Radix Aucklandiae 210g, Rhizoma Corydalis 300g, Radix Paeoniae Rubra 300g, Poria 370g, cowherb Art 190g, Herba Polygoni cymosi 200g, Ramulus Cinnamomi 190g and Rhizoma Sparganii 180g.Prepare according to following steps: weigh according to quantity Herba Polygoni cymosi, Fructus Corni, Rhizoma Corydalis and rhubarb medicinal material, first add 9 times amount 65% alcohol reflux 1 time, then adds 8 times amount 65% alcohol reflux 2 times, often Secondary 2h, filters, obtains alcohol extract, standby；Weigh according to quantity Sanguis Draxonis, Radix Angelicae Sinensis, Cortex Moutan, the Radix Aucklandiae, Radix Paeoniae Rubra, Poria, Rhizoma Curcumae, Ramulus Cinnamomi and Rhizoma Sparganii, first adds 7 times amount soak by water 1 time, then adds 6 times amount water boiling and extraction 2 times, each 1h, filters, obtains Aqueous extracts, subtract through 75 DEG C It is 1.05 that pressure is concentrated into density, obtains condensed water extract, adds ethanol, stirs, and controlling concentration of alcohol in feed liquid is 40% ～60%, stand 12h, discard precipitation, obtain precipitate with ethanol supernatant, standby；Alcohol extract mixes with precipitate with ethanol supernatant, 75 DEG C of concentrating under reduced pressure It is 1.25 to density, obtains concentrated solution, concentrated solution 70 DEG C vacuum drying 72h, obtain extractum extract, pulverized No. 5 sieves, and obtained medicine Powder, adds soluble starch by the mass ratio of 1:1 in medicated powder, and the aspartame accounting for medicated powder gross mass 0.2% with consumption is made Correctives, the ethanol of 90% make wetting agent pelletize, granule 60 DEG C～80 DEG C gradually rise warming middle-JIAO be dried, secondary pelletize, cross No. 1 sieve Except bulky grain, cross No. 5 and screen out fine powder, obtain granule.This preparation boiled water is taken after mixing it with water.Once two bags, three times on the one.Every packed 5g.

Claims (8)

1. the Chinese medicine preparation treating endometriosis, it is characterised in that: count by weight, by following crude drug system Become: Sanguis Draxonis 53～198 parts, Radix Et Rhizoma Rhei 99～495 parts, Fructus Corni 198～396 parts, Radix Angelicae Sinensis 198～396 parts, Cortex Moutan 198～ 396 parts, the Radix Aucklandiae 99～330 parts, Rhizoma Corydalis 99～330 parts, Radix Paeoniae Rubra 198～396 parts, Poria 293～495 parts, Rhizoma Curcumae 173～ 297 parts, Herba Polygoni cymosi 105～990 parts, Ramulus Cinnamomi 99～330 parts and Rhizoma Sparganii 165～330 parts.

A kind of Chinese medicine preparation treating endometriosis the most according to claim 1, it is characterised in that: by weight Number meter, is made up of following crude drug: Sanguis Draxonis 103 parts, Radix Et Rhizoma Rhei 412 parts, Fructus Corni 343 parts, Radix Angelicae Sinensis 275 parts, Cortex Moutan 275 Part, the Radix Aucklandiae 175 parts, Rhizoma Corydalis 257 parts, Radix Paeoniae Rubra 223 parts, 343 parts of Poria, Rhizoma Curcumae 223 parts, Herba Polygoni cymosi 155 parts, Ramulus Cinnamomi 223 parts With Rhizoma Sparganii 223 parts.

A kind of Chinese medicine preparation treating endometriosis the most according to claim 1 and 2, it is characterised in that: described Preparation be make excipient with soluble starch, 0.2% aspartame makees correctives, 90% ethanol is made as wetting agent granule Agent.

4. the preparation method of the Chinese medicine preparation for the treatment of endometriosis as claimed in claim 1 or 2, it is characterised in that: Weigh Herba Polygoni cymosi, Fructus Corni, Rhizoma Corydalis and rhubarb medicinal material according to quantity, add ethanol, reflux, extract, filter, obtain alcohol extract, standby；Press Amount weighs Sanguis Draxonis, Radix Angelicae Sinensis, Cortex Moutan, the Radix Aucklandiae, Radix Paeoniae Rubra, Poria, Rhizoma Curcumae, Ramulus Cinnamomi and Rhizoma Sparganii, adds water, and decocts and extracts, and filters, Aqueous extracts, through concentrating under reduced pressure, obtains condensed water extract, adds ethanol, stir, and stands, discards precipitation, obtain precipitate with ethanol supernatant Liquid, standby；Alcohol extract mixes with precipitate with ethanol supernatant, concentrating under reduced pressure, obtains concentrated solution, and concentrated solution is vacuum dried, and obtains extractum extract, Pulverize and sieve, obtain medicated powder, add adjuvant and make various pharmaceutical preparation.

The preparation method of the Chinese medicine preparation for the treatment of endometriosis the most according to claim 4, it is characterised in that: press Amount weighs Herba Polygoni cymosi, Fructus Corni, Rhizoma Corydalis and rhubarb medicinal material, adds 6～10 times amount 60%～80% ethanol, reflux, extract, 1～3 Secondary, each 1～2h, filter, obtain alcohol extract, standby；Weigh Sanguis Draxonis, Radix Angelicae Sinensis, Cortex Moutan, the Radix Aucklandiae, Radix Paeoniae Rubra, Poria, cowherb according to quantity Art, Ramulus Cinnamomi and Rhizoma Sparganii, add 6～10 times amount water, decocts and extracts 1～3 time, and each 1～2h filter, obtain Aqueous extracts, through 75 DEG C of decompressions Being concentrated into density is 1.05, obtains condensed water extract, adds ethanol, stirs, control concentration of alcohol in feed liquid be 40%～ 60%, stand 12h, discard precipitation, obtain precipitate with ethanol supernatant, standby；Alcohol extract mixes with precipitate with ethanol supernatant, and 75 DEG C are evaporated to Density is 1.25, obtains concentrated solution, concentrated solution 60 DEG C～80 DEG C vacuum drying 72～42h, obtains extractum extract, pulverized No. 5 sieves, Obtain medicated powder, add adjuvant and make various pharmaceutical preparation.

The preparation method of the Chinese medicine preparation for the treatment of endometriosis the most according to claim 5, it is characterised in that: press Amount weighs Herba Polygoni cymosi, Fructus Corni, Rhizoma Corydalis and rhubarb medicinal material, adds 9 times amount, 8 times amount 80% ethanol respectively, reflux, extract, 2 times, often Secondary 1h, filters, obtains alcohol extract, standby；Weigh according to quantity Sanguis Draxonis, Radix Angelicae Sinensis, Cortex Moutan, the Radix Aucklandiae, Radix Paeoniae Rubra, Poria, Rhizoma Curcumae, Ramulus Cinnamomi and Rhizoma Sparganii, adds 7 times amount, 6 times amount water respectively, decocts and extracts 2 times, and each 1h filters, obtains Aqueous extracts, be evaporated to close through 75 DEG C Degree is 1.05, obtains condensed water extract, adds ethanol, stirs, and controlling concentration of alcohol in feed liquid is 60%, stands 12h, abandons Go precipitation, obtain precipitate with ethanol supernatant, standby；Alcohol extract mixes with precipitate with ethanol supernatant, and 75 DEG C are evaporated to density is 1.25, obtains dense Contracting liquid, concentrated solution 70 DEG C vacuum drying 60h, obtain extractum extract, pulverized No. 5 sieves, and obtained medicated powder, add adjuvant and make respectively Plant pharmaceutical preparation.

7., according to the preparation method of the Chinese medicine preparation treating endometriosis described in claim 4 or 5, its feature exists In: adding soluble starch in medicated powder by the mass ratio of 1:1, the aspartame accounting for medicated powder gross mass 0.2% with consumption is made Correctives, 90% ethanol makees wetting agent and pelletizes, and granule is dried in 60 DEG C～80 DEG C, and secondary is pelletized, and crosses and screens out bulky grain and except carefully Powder, obtains granule.

The preparation method of the Chinese medicine preparation for the treatment of endometriosis the most according to claim 7, it is characterised in that: press The mass ratio of 1:1 adds soluble starch in medicated powder, and the aspartame accounting for medicated powder gross mass 0.2% with consumption makees taste masking Agent, 90% ethanol make wetting agent pelletize, granule 60 DEG C～80 DEG C gradually rise warming middle-JIAO be dried, secondary pelletize, cross No. 1 screen out big Grain, crosses No. 5 and screens out fine powder, obtain granule.