CN106039210A

CN106039210A - Traditional Chinese medicinal composition for treating hyperplasia of mammary glands as well as preparation method and application thereof

Info

Publication number: CN106039210A
Application number: CN201610497660.4A
Authority: CN
Inventors: 张军龙; 濮存海; 贾晓波; 王伏军; 马少平
Original assignee: NINGXIA GOLD SUN PHARMACEUTICAL CO Ltd
Current assignee: NINGXIA GOLD SUN PHARMACEUTICAL CO Ltd
Priority date: 2016-06-29
Filing date: 2016-06-29
Publication date: 2016-10-26

Abstract

The invention discloses a traditional Chinese medicinal composition for treating hyperplasia of mammary glands as well as a preparation method and application thereof. The traditional Chinese medicinal composition for treating hyperplasia of mammary glands is prepared by adopting a method comprising the following steps: 1) preferentially extracting volatile oil in curcuma aromatica by adopting a CO2 supercritical technology, and carrying out inclusion by adopting beta-cyclodextrin, so that an inclusion compound is obtained; 2) carrying out alcohol extraction on curcuma aromatica herbal residue, hairyvein agrimony and fructus aurantii (stir-fried with bran) according to properties of respective effective ingredients, so that alcohol extraction extract is obtained; 3) carrying out water extraction on alum, saltpeter, trogopterus dung and dry paint, so that water extraction extract is obtained; and (4) uniformly mixing the inclusion compound, water extraction extract, alcohol extraction extract and semen strychni powder. According to the preparation method, effective parts or effective ingredients and auxiliary ingredients are extracted out as many as possible, ineffective ingredients and tissue substances such as heavy metals are avoided, and harm on the human body is reduced. The traditional Chinese medicinal composition disclosed by the invention has the effects of soothing the liver and regulating flow of qi, reducing phlegm and resolving masses, regulating flow of qi and dredging the collaterals as well as regulating thoroughfare and conception channels, and can be used for treating hyperplasia of mammary glands or assisting treatment of hyperplasia of mammary glands.

Description

A kind of Chinese medicine composition treating cyclomastopathy and its preparation method and application

Technical field

The present invention relates to technical field of Chinese medicines, in particular to being a kind of Chinese medicine composition treating cyclomastopathy and preparation thereof Methods and applications.

Background technology

The pathogenesis of cyclomastopathy: motherland's traditional medicine thinks that generation cyclomastopathy is appointed relevant with liver,spleen,kidney, punching, many Having mechanism of qi obstructed, blood stasis, expectorant are solidifying, make the strongly fragrant resistance of meridian qi and blood be agglomerated into caused by core.Ancients think " disease of married woman arises from strongly fragrant more ", Owing to women easily suffers from stagnation of liver-QI for the psychological characteristics of feelings will change.Meanwhile, motherland's medical science thinks that gas and blood are closely bound up, gas Handsome for blood, gas row then blood, the stagnation of QI then blood stasis, hematogenous blockage then mammary gland changes therewith, thus easily forms liver energy stagnation type breast Gland hypertrophy is sick.

The important pathogenesis of cyclomastopathy is stagnation of QI due to depression of the liver liver controlling conveyance and dispersion, and irritability is the happiest and bar reaches, liver being bold and firm viscera, and body the moon is used Sun preferably rises and sends out and evacuate.Irritability had both disliked depression, also avoided high.Owing to feelings will is unsuccessful, melancholy puzzled, long strongly fragrant impairing the liver, or by essence God stimulates, irritable angry, all may result in depression of liver-QI, and the mechanism of qi stasis of blood is stagnant, pents up in breast stomach network, and breast network meridian and vessels obstruction is obstructed, no General rule causes mastalgia bitterly.

The treatment of cyclomastopathy can use blood circulation promoting and blood stasis dispelling and dissipating phlegm and resolving masses method, and activating blood and removing stasis Method is the conventional side for the treatment of nodules of the breast Method.The traditional Chinese medical science has saying of " pathogen usually intruding into collateral in protracted disease ", and nodules of the breast onset is slow, and the course of disease is long, touching does not heals, therefore lump in breast is to tie in breast for accumulation of phlegm in the hypochondrium Caused by network.Qi depression to blood stasis, breast network blocks, is the basic pathogenesis of cyclomastopathy." addiction " " knot " " bitterly " is the sick total clinic of breast Feature, no matter the breast of which kind of pattern of syndrome is sick, on the basis of differentiation of symptoms and signs for classification of syndrome treats, all needs the method for R. concomitans blood circulation promoting and blood stasis dispelling to dredge gas Blood, makes addiction blood agglomeration blockization dissipate, and breast network is unobstructed and swells and ache from disappearing.Modern medicine study result also confirms that invigorating blood circulation addiction method can change Being apt to or correct blood circulation and microcirculation disturbance, drug for invigorating blood circulation and eliminating stasis has reduction blood viscosity, accelerates the effects such as blood flowing, Thus promote the lump of hypertrophy and fiber to absorb.

Existing technique PINGXIAO PIAN is mainly used in the treatment of tumor, but owing to its effective ingredient not being extracted largely, The most notable to the therapeutic effect of cyclomastopathy；On the other hand, Sal Nitri and Alumen are directly pulverized and are used as medicine, heavy metal and having Evil constituent content is higher.

Summary of the invention

Present invention aim to provide the Chinese medicine composition of a kind of effective treatment cyclomastopathy.This Chinese medicine composition rises To effect conditioning endocrine such as depressed liver-energy dispersing and QI regulating, dissipating phlegm and resolving masses, regulating qi and dredging collateral, Chong and Ren Meridians regulating, fundamentally disintegrate cyclomastopathy Primary factors, adds that TAM, to estrogen antagonist, blocks its effect making gland tissue hyperplasia and edema, releases pain and swollen Completely waiting discomfort, the effect reaching treating both the principal and secondary aspects of a disease is the most also avoided that the threat of heavy metal and harmful element.

It is a further object of the present invention to provide the Chinese medicine composition preparation method of this treatment cyclomastopathy.

It is an object of the invention to be accomplished by:

A kind of Chinese medicine composition treating cyclomastopathy, is prepared by the following method and obtains:

Take Radix Curcumae 54 weight portion, Herba Agrimoniae 54 weight portion, Oletum Trogopterori 45 weight portion, Alumen 54 weight portion, Sal Nitri 54 weight Part, Resina Toxicodendri 18 weight portion, stir-baked Fructus Aurantii in bran 90 weight portion, Semen Strychni Pulveratum 36 weight portion；

Above-mentioned raw materials is prepared in such a way:

(1) Radix Curcumae is through CO₂Supercritical extraction obtains Radix Curcumae extract and Radix Curcumae raffinate, by Radix Curcumae extract β-ring Dextrin inclusion, obtains clathrate；

(2) Radix Curcumae raffinate, stir-baked Fructus Aurantii in bran and Herba Agrimoniae mixing alcohol extraction step (1) obtained, filters, obtains alcohol extraction medicine Slag and filtrate, filtrate concentrates, obtains alcohol-extracted extract；

(3) alcohol extraction medicinal residues step (2) obtained carry with Resina Toxicodendri, Oletum Trogopterori, Alumen and Sal Nitri mixing water, filter, obtain Water carries medicinal residues and filtrate, and filtrate concentrates, and obtains the water extracted immersing paste；

(4) alcohol-extracted extract, the water extracted immersing paste, Semen Strychni Pulveratum and clathrate mix and get final product；The fineness of Semen Strychni Pulveratum was 80 mesh Sieve.

CO described in step (1)₂Supercritical extraction condition is: extracting pressure is 25-35MPa, extraction temperature 25-35 DEG C, CO₂Flow 11-15L/h, extraction time 1-2h；Radix Curcumae extract beta-schardinger dextrin-carries out inclusion condition: Radix Curcumae extract and Ratio between beta-schardinger dextrin-is 1ml:3-5g, and the times amount that adds water is 4-8 times, and the inclusion time is 20-60 minute.

CO described in preferred steps (1)₂Supercritical extraction condition is: extracting pressure is 35MPa, extraction temperature 30 DEG C, CO₂ Flow 13L/h, extraction time 1.5h；Separating still I pressure 10～11MPa, temperature 48 DEG C；Separating still II pressure 7～8MPa, temperature 36℃.Radix Curcumae extract beta-schardinger dextrin-carries out inclusion condition: the ratio between Radix Curcumae extract and beta-schardinger dextrin-is 1ml: 5g, the times amount that adds water is 8 times, and the inclusion time is 60 minutes.

Described step (2) may comprise steps of: takes the stir-baked Fructus Aurantii in bran of recipe quantity, Herba Agrimoniae and Radix Curcumae raffinate Thing, adds 6-10 times of weight 70%-90% alcohol heating reflux of three kinds of mixture and extracts 1-3 time, each 1-2 hour, be heated to reflux Liquid stands more than 12 hours, Aspirate supernatant, and 300 mesh filter, and obtain medicinal residues and filtrate；Filtrate is concentrating under reduced pressure under the conditions of 60 DEG C Alcohol-extracted extract to relative density 1.15～1.25.

Described step (2) specifically includes following steps: take the stir-baked Fructus Aurantii in bran of recipe quantity, Herba Agrimoniae and Radix Curcumae raffinate, Add 8 times of weight 80% alcohol heating reflux of three kinds of mixture and extract twice, each 2 hours, be heated to reflux liquid stand 12 hours with On, Aspirate supernatant, filter, the clear paste of relative density 1.15～1.25 under the conditions of filtrate reduced in volume to 60 DEG C.

Described step (3) may comprise steps of: takes the Resina Toxicodendri of recipe quantity, Oletum Trogopterori, Alumen, Sal Nitri and alcohol extraction medicine Slag, adds water heating and refluxing extraction 1-3 time of 6-10 times of weight of five kinds of mixture, each 1-2 hour, backflow stand 12 hours with On, Aspirate supernatant, 300 mesh filter, and filtrate is concentrated under reduced pressure to give the water of relative density 1.15～1.25 under the conditions of 60 DEG C and carries Extractum；

Preferred steps (3) specifically includes following steps: take the Resina Toxicodendri of recipe quantity, Oletum Trogopterori, Alumen, Sal Nitri and alcohol extraction medicine Slag, adds the water heating and refluxing extraction 2 times of 10 times of weight of five kinds of mixture, and each 1.5 hours, backflow stood more than 12 hours, Aspirate supernatant, filters, the clear paste of relative density 1.15～1.25 under the conditions of filtrate reduced in volume to 60 DEG C.

Described step (4) specifically includes following steps: by clathrate, alcohol-extracted extract, the water extracted immersing paste mix homogeneously, adds Semen Strychni Pulveratum, is dried under vacuum to dry cream, is ground into fine powder.

Dosage form made by above-mentioned Chinese medicine composition and pharmaceutically acceptable adjuvant, and preferred dosage form is tablet, capsule, granule Agent, pill.

The preparation method of the Chinese medicine composition of above-mentioned treatment cyclomastopathy, the method comprises the following steps:

Above-mentioned raw materials is prepared in such a way:

(1) Radix Curcumae is through CO₂Supercritical extraction obtains Radix Curcumae extract and Radix Curcumae raffinate, by extract beta-schardinger dextrin- Inclusion, obtains clathrate；

The Chinese medicine composition for the treatment of cyclomastopathy of the present invention is in preparation treatment or prevention or assists treatment mammary gland to increase Raw medicine is applied.

Divide in effect conditionings such as Chinese medicine composition function depressed liver-energy dispersing and QI regulating of the present invention, dissipating phlegm and resolving masses, regulating qi and dredging collateral, Chong and Ren Meridians regulating Secrete.

In this prescription, the pharmacology of each medicine is:

Radix Curcumae is zingiberaceous plant RADIX CURCUMAE (Cur cuma weny uj in Y.H.Chenet C.Ling), Rhizoma Curcumae Longae (Curclma longa L.), Guangxi zedoary (Curcumakw angsiensis S.G.Lee et C.F.Liang) or fluffy cowherb The dried root of art (Curcuma haeocaulis Val.).The above two practise respectively title " RADIX CURCUMAE " with " Radix Curcuma ", remaining Practise by character difference and claim osmanthus Radix Curcumae or green filament Radix Curcumae.Radix Curcumae mainly originates in the ground such as Sichuan, Fujian, Zhejiang, Guangxi.In Radix Curcumae mainly Containing compositions such as volatile oil, curcumin, polysaccharide, a small amount of trace element, wherein volatile oil is Radix Curcumae antineoplastic effective composition, Rhizoma Curcumae Longae Element is the principle active component of Rhizoma Curcumae blood fat reducing, antioxidation, antiinflammatory.Modern pharmacology research shows, it is thin that Radix Curcumae has protection liver Born of the same parents, promotion liver cell regeneration, anticancer, antibacterial, antioxidative effect.Volatile oil and curcumin are the principle active component of Radix Curcumae. Radix Curcumae volatile oil not only has the effect of sterilization, antiviral, antiinflammatory and blood circulation promoting and blood stasis dispelling, removing the necrotic tissue and promoting granulation, and may also suppress tumor The growth of cell, has positive role to prevention cervical cancer.Curcumin has the multiple pharmacology such as antitumor, antiinflammatory, antibacterial, antioxidation Effect, and toxicity is low, has good clinical practice potentiality, is paid close attention to widely by both at home and abroad.

Fructus Aurantii is rutaceae Citrus aurantium Linn. (Citrus aurantium L1) and the dry crude fruit of variety thereof Real.Bitter in the mouth, pungent, sour.Cold nature.Return spleen, stomach warp.There is regulating the flow of QI to ease the stomach, effect of the stagnant relieving distension of row.The stagnation of QI, distension is coerced for breast Pain, accumulation of food in the stomach and intes tine due to indigestion, stops in phlegm retention, visceroptosis.Fructus Aurantii is one of typical QI regulating medicine of Chinese medicine, is widely used in TCM Bed.Contained by Fructus Aurantii, chemical composition is complex, the effective ingredient being currently known mainly have flavonoid, volatile oil, alkaloids, Coumarins and some trace element etc..From the point of view of PINGXIAO PIAN is used for treating cyclomastopathy, we mainly take Fructus Aurantii Hesperidin, naringin and Nobiletin in flavones ingredient.Hesperidin has antiinflammatory action, antitumaous effect.Naringin has Anti-inflammatory and analgesic effect.Nobiletin has the pharmacological actions such as antiinflammatory, antiviral, antioxidation.

Herba Agrimoniae is the ground drying nest of rosaceous plant Radix Agrimoniae (Agrimonia Pilosa Ledeb), mainly becomes Dividing and have flavonoid, agrimonine, agrimonolide, tannin, volatile oil, organic acid and agrimophol etc., property is bitter, puckery, GUIXIN, Liver Channel, has astringing to arrest bleeding, preventing the attack (or recurrence) of malaria, dysentery relieving, Detoxication, can be used for treat hemoptysis, haematemesis, metrostaxis, malaria, dysentery, De-power impairment caused by overstrain, carbuncle sore tumefacting virus, pudendal pruritus leukorrhagia.

Resina Toxicodendri (dried lacquer) is Anacardiaceae (Anacar diaceae) plant Toxicodendron verniciflnum (Stokes) F. A. Barkley (Rhus verniciflua Stokes) Tox icodend ron v The Resina Toxicodendri verniciflui drying of er nicif luum (Sto kes) F1A1Barkley secretion processes.Resina Toxicodendri have another name called paint slag, paint the end, Paint foot, continuous life cylinder, pitch-dark, China goes through an edition pharmacopeia and all includes；Have removing blood stasis with potent drugs blood, disappear the effect such as blood, parasite killing, be mainly used in blood stasis, The treatment of the diseases such as abdominal pain due to worm stagnation, women's amenorrhea.Being used for antineoplastic principle active component in Resina Toxicodendri is urushipolysaccharide, and urushipolysaccharide has There is various biological activity, such as antitumor, anti-H IV, blood coagulation resisting function etc..

Oletum Trogopterori (Faeces trogopterori) is flying squirrel section animal trogopterus xanthipes Milne-Edwards (Trogoterus xanthip Es) dry feces, function is blood circulation promoting and blood stasis dispelling, pain relieving, and applicating history is long, and clinically have in the dysmenorrhea caused by blood stasis, the heart more The diseases such as angor.It is reported, the water decoction of Oletum Trogopterori has inhibitory action to platelet aggregation, and Oletum Trogopterori water extract is external can substantially be pressed down Rabbit platelet aggregation processed, its inhibitory action is relevant to dosage, and Oletum Trogopterori has fibrinolysis activity, Oletum Trogopterori ethyl acetate extract With Oletum Trogopterori water decoction, also there is antiinflammatory action.

Described in " China's book on Chinese herbal medicine ", Sal Nitri has used in " 52 Bingfang "；Acrid in the mouth, hardship are micro-salty；GUIXIN, spleen, Lung meridian.Assaulting fortified position removing mass, under diuresis is rushed down, removing toxic substances and promoting subsidence of swelling, cure mainly heatstroke wound cold, abdominal distention is vomited and diarrhoea, trusted subordinate's pain, jaundice, the puckery pain of all pouring, Sore throat, conjunctival congestion with ophthalmalgia swells, furunculosis.Containing heavy metal arsenic in Sal Nitri, arsenic is insoluble in water, and the present invention is in order to cut down the toxicity of arsenic, to nitre Stone uses water to carry.

Alumen is mainly composed of aqueous sulfuric acid aluminum potassium [KAl (SO₄)₂·12H₂O].Head is loaded in Shennong's Herbal, originates in Zhejiang The ground such as river, Anhui, Gansu, Hubei, Shanxi.For the alum crystallisation of the Sulfates processed refinement of mineral alunite, belong to Trigonal system, have eliminate the phlegm, dampness, hemostasis, antidiarrheal, anticorrosion, effect of sterilization.In Alumen containing a small amount of trace element-selenium and Zinc, selenium can suppress the propagation of tumor cell；Zinc has suppression carcinogen and lures the effect of cancer.Sal Nitri and Alumen are mainly composed of salt Class, and containing heavy metal and arsenic salt, the present invention uses water extraction to eliminate the heavy metal impact on medicine.

Semen Strychni (Nux vomica) is loganiaceae plant Semen Strychni Strychnos nux-vomica L or S. pierriana The dry mature seed of Strychnos pierriana A.W., main product is in the ground such as India, Vietnam.When being recorded in Ming Dynasty Lee the earliest Precious " Compendium of Materia Medica volume 18 " says it: shape is like company's money of horse, therefore named Semen Strychni.Have another name called vomiting nut, Niu Yin, side eight, hardship in fact.Property Bitter in the mouth temperature is very toxic, returns liver, spleen channel, function: removing obstruction in the collateral to relieve pain, mass dissipating and swelling eliminating.For traumatic injury, rheumatoid arthritis stubborn, fracture swells and ache, Paralysis and numbness, skin sore, laryngopharynx swelling and pain.The effective ingredient of Semen Strychni is strychnine, and Yu Zhi is gorgeous waits research to show, along with horse The increase of Semen Strychni alkali concn, the anti-apoptotic genes expression Bcl-2 expression of human breast cancer cell MDA-MB 231 substantially reduces, Promote apoptogene Bax and Caspase-3 expression substantially to increase.In order to avoid in Semen Strychni, strychnine is suffered a loss, weaken drug effect, wave Taking medical material, Semen Strychni is directly pulverized by the present invention, without concocting direct drug injection.

Chinese medicine composition of the present invention has the merits such as blood circulation promoting and blood stasis dispelling, pain relieving eliminating stagnation, heat-clearing and toxic substances removing, strengthening vital QI to eliminate pathogenic factors, qi-restoratives dredging collateral Effect, the tuberosity for each phase hypertrophy all has good dissipation role.Utilize present composition depressed liver-energy dispersing and QI regulating, dissipating phlegm and resolving masses, reason Effect conditioning endocrine such as gas dredging collateral, Chong and Ren Meridians regulating, fundamentally disintegrate the Primary factors of cyclomastopathy, add that TAM antagonism is female Hormone, blocks its effect making gland tissue hyperplasia and edema, releases the discomfort such as pain and distension, to reach treating both the principal and secondary aspects of a disease Effect.Additionally, also cyclomastopathy tuberosity there to be good eliminating stagnation effect.

In this technique, (1) uses CO₂Volatile oil in Radix Curcumae is preferentially proposed by supercritical technology, and is wrapped with beta-schardinger dextrin- Close, obtain clathrate；(2) Radix Curcumae medicinal residues, Herba Agrimoniae, Fructus Aurantii (parched with bran) use alcohol extraction according to its effective ingredient character, obtain alcohol extraction leaching Cream；(3) Alumen, Sal Nitri, Oletum Trogopterori, Resina Toxicodendri use water to carry, and obtain the water extracted immersing paste；(4) clathrate, the water extracted immersing paste, alcohol-extracted extract, horse Semen Strychni powder mixes.The invention have the advantages that the volatile oil in Radix Curcumae is preferentially extracted by (1), and stick with paste with β ring Progress greatly row inclusion, is sufficiently reserved Radix Curcumae volatile oil, makes the active constituent content of monarch drug in PINGXIAO PIAN be greatly improved.(2) Herba Agrimoniae Using alcohol extraction, wherein the organic principle such as flavonoid, Polyphenols and esters is fully extracted.(3) Resina Toxicodendri, Oletum Trogopterori, Alumen And Sal Nitri uses water to carry, make effective site or effective ingredient and auxiliary element is as much as possible extracts, and heavy metal etc. Invalid components and suck tissue do not extract, and reduce the injury to human body.The present invention treats the Chinese medicine of cyclomastopathy Compositions can make various dosage form (hard capsule that includes taking orally, soft capsule, tablet, granule, drop pill).

The know-why of the present invention and technical study:

This technique uses different preparation technologies for different material, enables the effective site of each raw material to obtain fully Application, and decreases side effect, is embodied in the following aspects:

One, Radix Curcumae CO₂The research of supercritical extraction volatile oil technique

1, orthogonal test affects CO₂The principal element of supercritical extraction volatile oil yield have extracting pressure, extraction kettle temperature, CO₂Flow velocity and extraction time, therefore select orthogonal table L₉(3⁴) design orthogonal test, weigh 100g turmeric powder and be broken into coarse powder, with extraction Taking rate (%) is evaluation index, test arrangement and the results are shown in Table 1.(extraction yield %=(gained oil mass/inventory) × 100%)

Table 1 Radix Curcumae CO₂The orthogonal experiment factor level table of supercritical extraction

Table 2 Radix Curcumae CO₂Supercritical extraction Orthogonal experiment results table

(F_0.05(2,2)=19.00) it is A > B > C > D from range analysis result, optimal group between each factor and level It is combined into A₃B₂C₂D₂, with D item as error term, carry out variance analysis further, the results are shown in Table 3.

Table 3 Radix Curcumae CO₂Supercritical extraction analysis of variance table

(F0.05 (2,2)=19.00) from the results of analysis of variance, each factor on extraction yield there are no significant impact.Excellent The optimised process of choosing is combined as A₃B₂C₂D₂。

2. supercritical confirmatory experiment

In order to verify the above results, weigh 100g Radix Curcumae coarse powder, select A₃B₂C₂D₂Condition carries out CO₂Supercritical checking is real Test, the results are shown in Table 4.

Table 4CO₂Supercritical confirmatory experiment result table

Sequence number	The yield of volatile oil
		1	5.18%
2	5.26%
		3	5.39%

Conclusion: 3 times experimental result confirms: A₃B₂C₂D₂Super critical condition is consistent substantially with Orthogonal experiment results, optimal extraction Taking parameter is: optimal extraction parameters is: extracting pressure 35MPa, extraction temperature 30 DEG C, CO₂Flow 13L/h, extraction time is 1.5h.Separating still I pressure 10～11MPa, temperature 48 DEG C；Separating still II pressure 7～8MPa, temperature 36 DEG C.

Two, the determination of Radix Curcumae volatile oil inclusion parameter

1, the determination of inclusion method

Colloid milling, saturated water solution method, ultrasonic method are the most frequently used inclusion method.Under identical material ratio, add Enter beta-schardinger dextrin-20g, with oil: beta-schardinger dextrin-(ml:g)=1:4, add 5 times of the water of beta-schardinger dextrin-weight, inclusion time 40min, add alcohol Amount 50% carries out inclusion, compares colloid milling, saturated water solution method, ultrasonic method with clathrate yield for index.

Finally record colloid milling, saturated water solution method, the inclusion rate of ultrasonic method are respectively 76.18%, 68.11%, 59.31%, determine the best approach that colloid milling is inclusion.

2, the determination of de-bag method parameter

2.1 determinations taking off bag solvent

Take the clathrate prepared through colloid mill method of equivalent, respectively with the methanol of equivalent, dichloromethane, petroleum ether dissolution, super Sound 40min, with oil utilization rate and oil content as index, show that optimal de-bag solvent is methanol.

2.2 determinations taking off bag method

Take the clathrate prepared through colloid mill method of equivalent, dissolve with the methanol of equivalent, be respectively adopted circumfluence method and ultrasonic method Carry out de-bag 40min, with oil utilization rate and oil content as index, show that optimal de-bag method is ultrasonic method.

2.3 determinations taking off the bag time

Take the clathrate prepared through colloid mill method of equivalent, dissolve with the methanol of equivalent, with ultrasonic method de-bag 20min respectively, 40min, 60min, with oil utilization rate and oil content as index, show that the optimal de-bag time is 40min.

3, the determination of inclusion method parameter

3.1 orthogonal experiment

Take the volatile oil of appropriate extraction, design orthogonal experiment water-glass according to amount of water, material ratio and inclusion time and be shown in Table 5。

Table 5 Radix Curcumae volatile oil clathrate orthogonal experiment factor level table

With clathrate yield, oil utilization rate and oil content are that inspection target obtains Orthogonal experiment results table, such as table 6

Clathrate oil content=clathrate oil content/clathrate amount × 100%

Oil utilization rate=clathrate oil content/throwing oil mass × 100%

Table 6 orthogonal experiment calendar and analysis of results table

Table provides 9 experimental programs.If No. 6 experiment is A₂B₃C₁D₂, i.e. material ratio 1:6, amount of water 5 times, inclusion Time 20min, pushes away with this.

With clathrate yield as index, range analysis result A > B > C.Best of breed between each factor and level is A₃B₃C₃, with C item as error term, carry out variance analysis further, the results are shown in Table 7

Table 7 is with clathrate yield for index scoring variance table

Yield is index, each empirical factor on experimental result there are no significant impact, preferred optimised process is A₃B₃C₃。

With oil utilization rate as index, range analysis result A > B > C.Best of breed between each factor and level is A₃B₃C₃, With C item as error term, carry out variance analysis further, the results are shown in Table 8.

Table 8 is with oil utilization rate for index scoring variance table

Index, each level on experimental result there are no significant impact, preferred optimised process is A₃B₃C₃。

With oil content as index, range analysis result A > C > B.Best of breed between each factor and level is A₂B₂C₃, with B item is error term, carries out variance analysis further, the results are shown in Table 9.

Table 9 is with oil content for index scoring variance table

(F_0.05(2,2)=19.00) with oil content as index, oil and β-CD ratio have the impact of work property, the most optimal work to experimental result Skill is A₂B₂C₃。

Can be seen that the oil impact with β-CD ratio is more than other factors from three index range analysiss；Seek with comprehensive grading Look for optimised process, in three indexs of clathrate process research, choose the best conduct of result 100 points respectively, three weight system Number is respectively inclusion yield 0.2, oil utilization rate 0.4, oil content 0.4.By computing formula: comprehensive grading Y=weight × (100-is High level+y_i).Analyzed by directly perceived, with comprehensive grading as index, show that each factor is A > B > C on extracting result impact order, respectively Best of breed between factor and level is A₃B₃C₃, with C item as error term, carry out variance analysis the results of analysis of variance further It is shown in Table 10.

Table 10 comprehensive grading variance table

(F_{0.05 (2,2)}=19.00) with comprehensive grading as index, each factor is on experimental result there are no significant impact, Good technique is A₃B₃C₃。

The confirmatory experiment of 5 inclusion parameters

In order to verify the above results, weigh 100g Radix Curcumae coarse powder, select A₃B₃C₃Condition carries out verifying that inclusion essential oil is real Test, the results are shown in Table 11.

Table 11 inclusion essential oil experimental result table

Experiment	Inclusion rate	Oil utilization rate	Oil content
				1	81.78%	77.35%	15.95%
2	82.19%	78.92%	16.46%
				3	82.67%	80.07%	16.28%

Be consistent with Orthogonal Parameter result through 3 experiment results, i.e. the optimal parameter condition of Radix Curcumae volatile oil inclusion is Oil: beta-schardinger dextrin-is 1:5, adds 8 times amount water, inclusion 60min.

Three, alcohol extraction process research

1, orthogonal test affects the principal element of alcohol extraction process has concentration of alcohol, solvent times amount, is heated to reflux the time and carries Take number of times.Above-mentioned 4 factors respectively take 3 levels and carry out L₉(3⁴) orthogonal test, take the Radix Curcumae CO of recipe quantity₂Supercritical extraction The factor level table of medicinal residues, stir-baked Fructus Aurantii in bran and Herba Agrimoniae according to the form below extracts, and screens optimum extraction process, and experimental factor level is shown in Table 12。

The quadrature factor water-glass of table 12 alcohol extraction condition

The present invention selects dry spun (%), general flavone content (%) to be inspection target, orthogonal experiment is carried out data and divides Analysis.Orthogonal calendar and the results are shown in Table 13.

Table 13 dry spun (%) and orthogonal arrangement that general flavone content (%) is inspection target and result table

(table provides 9 experimental programs.If No. 6 experiment is A₂B₃C₁D₂, i.e. 80% ethanol, 10 times amount are heated to reflux Extracting 2 times, each 1h, the rest may be inferred)

With general flavone content as index, range analysis result it is A > C > D > B, the best of breed between each factor and level For A₃B₂C₃D₂, with B item as error term, carry out variance analysis further, the results are shown in Table 14.

The table 14 analysis of variance table with general flavone content as index

(F_0.05(2,2)=19.00), with general flavone content as index, there are no significant to experimental result for each factor level Impact, extraction process best of breed is A₃B₂C₃D₂。

With dry spun as index, range analysis result is A > D > C > B, and the best of breed between each factor and level is A₂B₃C₂D₃, with B item as error term, carry out variance analysis further, the results are shown in Table 15.

The table 15 analysis of variance table with dry spun as index

(F_0.05(2,2)=19.00), with dry spun as index, each factor on experimental result there are no significant impact, carry Taking technique best of breed is A₂B₃C₂D₃。

For the orthogonal result of more rational evaluation, find optimum extraction process, two evaluation indexes are carried out comprehensive grading, calculate Method is as follows: in two indices, chooses soprano respectively as 100 points, and remaining is pressed formula and calculates: score Y=weight × (100 peak+y_i), to two indices weight coefficient respectively for for 0.6 and 0.4.Analyzed by directly perceived, with comprehensive grading For index, showing that each factor is A > C > D > B on extracting result impact order, the best of breed between each factor and level is A₂B₂C₃D₂, with B item as error term, carry out variance analysis further, the results are shown in Table 16.

The table 16 analysis of variance table with comprehensive grading as index

(F_{0.05 (2,2)}=19.00) with comprehensive grading index as index, each factor, to experimental result not statistically significant, extracts work Skill best of breed is A₂B₂C₃D₂。

2, alcohol extraction confirmatory experiment

In order to verify the above results, take above-mentioned three kinds of medical materials of 0.1 times of recipe quantity, select A₂B₂C₃D₂Condition is verified Experiment, obtains result such as table 17；

Table 17 alcohol extraction confirmatory experiment result table

Experiment number	General flavone content (%)	Dry spun (%)
			1	35.69	29.68
2	34.78	31.76
			3	35.33	30.45

The result of confirmatory experiment is consistent substantially with Orthogonal Parameter, so the optimum process condition of alcohol extraction experiment is concentration of alcohol Being 80%, ethanol consumption is 8 times amount, extracts twice, each 2h.

Four, extraction process by water research

1, orthogonal test affects the principal element of extraction process by water and adds water times amount, extraction time and extraction time.Above-mentioned 3 Individual factor respectively takes 3 levels and carries out L₉(3⁴) orthogonal test, take alcohol extraction medicinal residues, Resina Toxicodendri, Oletum Trogopterori, Alumen and the Sal Nitri of recipe quantity Extract by following factor level table, test arrangement and the results are shown in Table 18.

The quadrature factor water-glass of table 18. abstract methods

The present invention select zinc, ferrum, magnesium, selenium total amount i.e. beneficial element content (/), the i.e. harmful unit of arsenic, chromium, lead, total amount Cellulose content (/) and dry spun (%) be inspection target, orthogonal experiment is carried out data analysis.Orthogonal calendar and result It is shown in Table 19.

Table 19. water carries the orthogonal arrangement of test and result table

(table provides 9 experimental programs.If No. 6 experiment is A₂B₃C₁, water heating and refluxing extraction 2h of i.e. 8 times amount, extract 1 time, The rest may be inferred)

With beneficial element as index, range analysis result B > C > A, the best of breed between each factor and level is A₁B₃C₃, With A item as error term, carry out variance analysis further, the results are shown in Table 20.

The table 20. analysis of variance table with beneficial element total amount as index

(F_0.05(2,2)=19.00) with beneficial element content as index, each factor on experimental result there are no significant impact, Preferably optimised process is A₁B₃C₃。

With harmful element content as index, range analysis result B > A > C.Best of breed between each factor and level is A₃B₂C₁, with C item as error term, carry out variance analysis further, the results are shown in Table 21.

The table 21. analysis of variance table with harmful element content as index

(F_0.05(2,2)=19.00) with harmful element content as index, experimental result is had a significant impact by solvent times amount, Preferably optimised process is A₃B₂C₁。

With dry spun as index, range analysis result A > B > C.Best of breed between each factor and level is A₂B₃C₂, With C item as error term, carry out variance analysis further, the results are shown in Table 22.

The table 22. analysis of variance table with dry spun as index

(F_0.05(2,2)=19.00) with dry spun as index, each level on experimental result there are no significant impact, preferably Optimised process be A₂B₃C₂。

For the orthogonal result of more rational evaluation, find optimum extraction process, three evaluation indexes are carried out comprehensive grading, calculate Method is as follows: in three indexs, chooses soprano respectively as 100 points, and remaining is pressed formula and calculates: score Y=weight × (100 peak+y_i), to three index weights coefficients respectively for for 0.3,0.3 and 0.4.Analyzed by directly perceived, with comprehensively Scoring is index, show that each factor is B > A > C on extracting result impact order, and the best of breed between each factor and level is A₃B₂C₂, with C item as error term, carry out variance analysis the results of analysis of variance further and be shown in Table 23.

Table 23. comprehensive grading is the analysis of variance table of index

(F_0.05(2,2)=19.00) with comprehensive grading as index, experimental result is affected by each factor without significance, Good technique is A₃B₂C₂。

1, water carries confirmatory experiment

In order to verify the above results, take the above-mentioned medical material of 0.1 times of recipe quantity, according to A₃B₂C₂Condition carries out water and proposes experiment and test Card, result such as table 24

Table 24 water carries confirmatory experiment result table

The result of confirmatory experiment is consistent substantially with Orthogonal Parameter, i.e. water carry the extraction conditions of experiment be amount of water be 10 times, Extract twice, each 1.5h.

Below by way of the test of pesticide effectiveness, the present invention is further described (in tests below, the present composition is referred to as flat disappearing Sheet, prepares according to embodiment 1 method):

Invent and obtain most suitable process conditions through repeated screening, summary application, through putting down that these process conditions prepare The sheet that disappears has obvious therapeutical effect on the rat model with cyclomastopathy disease.It is reported as follows:

1, female non-pregnant rat about the 220g of laboratory animal: SD 80

2, reagent: commercially available PINGXIAO PIAN specification 0.24g/ sheet, Jintaiyang Pharmaceutical Co., Ltd., Ningxia

Lot number 2,013 0615

Estradiol benzoate injection specification 2g.L^-1/, Shanghai General Pharmaceutical Co., ltd.

Lot number 150501

Estradiol (E₂), progesterone (P) test kit all has Beijing China English biotechnology research to be produced

Lot number 151012

Slide gauge Shenzhen Xin Baolai detecting instrument company limited

Refrigerated centrifuger Beijing epoch Bei Li centrifuge company limited

R 911 Full automatic exempts from industry head office of calculating instrument Chinese University of Science and Technology

3, method

3.1 take 60 SD rats is randomly divided into 6 groups, model group (normal saline 15ml/), blank group (etc. Amount normal saline 15ml/), positive controls (commercially available PINGXIAO PIAN 0.5g/), the present composition high, medium and low dosage group (2.4、1.2、0.6g/㎏).Blank group rat muscle injecting normal saline (0.05ml/ is only), once a day, each model group Rat muscle injection estradiol benzoate 0.5/, terminate to experiment once a day.Modeling started gastric infusion after 1 week, often Day 1 time, being administered 4 weeks, last is drawn materials after being administered 2h.

The forward and backward slide gauge of mensuration modeling of 3.2 cyclomastopathy accurately measures rat the 2nd to 2, left and right breast diameter And height of nipples, and observe its outward appearance.

Fasting 12h before 3.3 hormone determination experiments, after last is administered 2h, abdominal aortic blood 5mL, 3 000r min^-1High Speed frozen centrifugation 15min, takes serum and adds the cold petroleum ether of 4mL, recentrifuge after mixing.Phase is abandoned in suction, after lower nitrogen dries up It is dried and seals, to be measured.

Use r 911 Full automatic to exempt from calculating instrument and radioimmunoassay kits, by product description, serum is carried out female Glycol (E₂), progesterone (P) detection.

4 results

4.1 on papilla diameter, height of nipples impact

Compared with normal group, model group rats papilla diameter and highly significant increase, and nipple holds up hyperemia.In injection female two Alcohol reaches swelling peak on the 2nd week, and within the 3rd week, swelling maintains an equal level, and begins to decline at the 4th week.PINGXIAO PIAN dosage high, middle group papilla diameter, Highly compare with model group and be substantially reduced.Result shows, PINGXIAO PIAN the cyclomastopathy that estradiol is induced is had significantly suppress make With.

Table 25 PINGXIAO PIAN on papilla diameter affect (N=10)

Compare with blank group^bP<0.001；Compare with model control group^cP<0.01；^dP<0.001；With positive controls Relatively^eP<0.05

Table 26 PINGXIAO PIAN on height of nipples affect (N=10)

Compare with blank group^bP<0.05；Compare with model control group^cP<0.05；^eP<0.01；^dP<0.001；With sun Property matched group compares^fP<0.05

4.2 couples of serum estradiol (E₂), the impact of progesterone (P) content

Testing result shows, positive controls and PINGXIAO PIAN high dose group relatively model group estrogen level decrease, pregnant Ketone level raises, and result see table

Table 27 PINGXIAO PIAN is to serum estradiol (E₂), the impact of progesterone (P) content (N=10)

Compare with blank group^bP<0.001；Compare with model control group^eP<0.05；^cP<0.01；^dP<0.001；

Compare with positive controls^fP<0.05

5. discuss

Being illustrated by above results of animal, PINGXIAO PIAN of the present invention has the work significantly treating cyclomastopathy With, improve the quality of life of patient, and any toxic and side effects and untoward reaction do not occur in experimentation.The present invention It is high that the technique of described preparation PINGXIAO PIAN has medical material utilization rate, and the tablet prepared does not has any side reaction, and stability is high.

6. the side's of tearing open efficacy study

Raw material components of the present invention is split and carries out curing mammary gland hyperplasia experiment by we, effect of the most each prescription, Five prescriptions are respectively as follows:

Prescription 1: volatile oil clathrate compound+Semen Strychni fine powder in technique；

Prescription 2: the water extracted immersing paste+volatile oil clathrate compound+Semen Strychni fine powder；

Prescription 3: alcohol-extracted extract+volatile oil clathrate compound+Semen Strychni fine powder；

Prescription 4: the present composition；

Experimental procedure is with 3.1 curing mammary gland hyperplasia experiment under Efficacy experiments item, after modeling, blank group and model comparison Group gives same volume solvent, and prescription 1-4 gives the given the test agent of 1.2g/kg, the results are shown in Table 28.

Table 28 PINGXIAO PIAN on papilla diameter affect (N=10)

Compare with blank group^bP<0.05；Compare with model control group^cP<0.05；^dP<0.01；Compare with prescription 4^eP< 0.05

Table 29 PINGXIAO PIAN on height of nipples affect (N=10)

Compare with blank group^bP<0.01；Compare with model control group^cP<0.05；^dP<0.01；^eP < 0.001 and prescription 4 compare^fP<0.05

Table 30 PINGXIAO PIAN is to serum estradiol (E₂), the impact of progesterone (P) content (N=10)

Compare with blank group^bP<0.001；Compare with model control group^cP<0.05；^dP<0.01；^eP<0.001；With group Side 4 compares^gP<0.05^fP<0.01；

The therapeutic effect of prescription 4 is significantly better than other prescription as can be seen from the above table, can illustrate that full side is to cyclomastopathy Treat of great advantage.

In sum, compared with prior art, the beneficial effect that the present invention possesses:

The raw material prescription of compositions of the present invention comes the clinical practice under free guidance of traditional Chinese medicine theory, prescription flavour of a drug Refine, with strong points.Described raw material prescription Chinese medicine depressed liver-energy dispersing and QI regulating, dissipating phlegm and resolving masses, regulating qi and dredging collateral, Chong and Ren Meridians regulating, medicine effectively becomes Divide and be prone to absorb, be conducive to playing drug effect；In described raw material prescription, each medical material is integration of edible and medicinal herbs medical material, has no side effect.

The extraction process advantage of compositions of the present invention is: (1) utilizes supercritical extraction technique Radix Curcumae volatile oil Advantage distillation out, and is used beta cyclodextrin inclusion, is sufficiently reserved Radix Curcumae volatile oil, makes effective one-tenth of monarch drug in PINGXIAO PIAN Content is divided to be greatly improved.Additionally can alleviate Radix Curcumae volatile oil to gastrointestinal stimulation.(2) Herba Agrimoniae uses alcohol extraction, its The organic principles such as middle flavonoid, Polyphenols and esters are fully extracted.(3) Resina Toxicodendri, Oletum Trogopterori, Alumen and Sal Nitri use Water carries, and makes effective site or effective ingredient and auxiliary element is as much as possible extracts, and the invalid components such as heavy metal and group Fabric matter does not extracts, and reduces the injury to human body.

Therefore, compositions of the present invention has significantly effect during treatment or prevention or auxiliary treatment cyclomastopathy Really.

Detailed description of the invention

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

Embodiment 1:

Radix Curcumae 54g, Herba Agrimoniae 54g, Oletum Trogopterori 45g, Alumen 54g, Sal Nitri 54g, Resina Toxicodendri 18g, stir-baked Fructus Aurantii in bran 90g, Semen Strychni Sub-powder 36g；

The preparation method of present composition tablet, it comprises the steps:

(1) extraction of Radix Curcumae volatile oil and inclusion: weigh the Radix Curcumae of recipe quantity, utilize CO₂Supercritical extraction carries Taking, extracting pressure is 35MPa, extraction temperature 35 DEG C, CO₂Flow 15L/h, extraction time 2h, be extracted thing Radix Curcumae volatile oil, And raffinate, the extract beta-schardinger dextrin-being obtained by extraction carries out inclusion, the ratio between Radix Curcumae extract and beta-schardinger dextrin- For 1ml:5g, the times amount that adds water is 8 times, and the inclusion time is 60 minutes, obtains clathrate A.

(2) alcohol extraction: take the stir-baked Fructus Aurantii in bran of recipe quantity, Herba Agrimoniae and Radix Curcumae raffinate and add 10 times amount 90% ethanol and heat back Stream extracts 2 times, and each 2 hours, backflow stood more than 12 hours, Aspirate supernatant, and 300 mesh filter, and obtain medicinal residues and filtrate； Filtrate is evaporated to the alcohol-extracted extract of relative density 1.15～1.25 under the conditions of 60 DEG C, standby；

(3) water carries: take the Resina Toxicodendri of recipe quantity, Oletum Trogopterori, Alumen, Sal Nitri and alcohol extraction medicinal residues, and the water adding 10 times amount heats back Stream extracts 3 times, and each 2 hours, backflow stood more than 12 hours, Aspirate supernatant, and 300 mesh filter, and filtrate is 60 DEG C of conditions Under to be concentrated under reduced pressure to give the water extracted immersing paste of relative density 1.15～1.25 standby；

(4) mix, be dried, pulverize: by Radix Curcumae volatile oil clathrate A, alcohol-extracted extract, the water extracted immersing paste mix homogeneously, add Semen Strychni fine powder, the fineness of Semen Strychni Pulveratum was 80 mesh sieves.It is dried under vacuum to dry cream, is ground into fine powder standby.

(5) tabletting: take the fine powder in (4), adds suitable auxiliary materials and mixing, diameter 10mm punch die, tabletting, tablet weight 0.3g/ Sheet；

(6) coating: Opadry film coating and get final product.

Tablets application in treatment cyclomastopathy, containing taking once 3, three times a day.

Embodiment 2:

The preparation method of present composition capsule, it comprises the steps:

(1) extraction of Radix Curcumae volatile oil and inclusion: weigh the Radix Curcumae of recipe quantity, utilize CO₂Supercritical extraction carries Taking, extracting pressure is 35MPa, extraction temperature 30 DEG C, CO₂Flow 13L/h, extraction time 2h, be extracted thing Radix Curcumae volatile oil, And raffinate, the extract beta-schardinger dextrin-being obtained by extraction carries out inclusion, the ratio between Radix Curcumae extract and beta cyclodextrin For 1ml:4g, the times amount that adds water is 6 times, and the inclusion time is 40 minutes, obtains clathrate A.

(2) alcohol extraction: take the stir-baked Fructus Aurantii in bran of recipe quantity, Herba Agrimoniae and Radix Curcumae raffinate and add 8 times amount 80% ethanol and heat back Stream extracts 3 times, and each 1.5 hours, backflow stood more than 12 hours, Aspirate supernatant, and 300 mesh filter, and obtain medicinal residues and filter Liquid；Filtrate is evaporated to the alcohol-extracted extract of relative density 1.15～1.25 under the conditions of 60 DEG C, standby；

(3) water carries: take the Resina Toxicodendri of recipe quantity, Oletum Trogopterori, Alumen, Sal Nitri and alcohol extraction medicinal residues, and the water adding 8 times amount is heated to reflux Extracting 2 times, each 2 hours, backflow stood more than 12 hours, Aspirate supernatant, and 300 mesh filter, and filtrate is under the conditions of 60 DEG C The water extracted immersing paste being concentrated under reduced pressure to give relative density 1.15～1.25 is standby；

(5) capsule is filled: taking the fine powder in (4), add suitable auxiliary materials and mixing, take No. 0 capsule, loading amount is 0.45g/ Grain, carries out fill.

The application in treatment cyclomastopathy of the present composition capsule, oral one time 3, three times a day.

Embodiment 3:

The preparation method of present composition granule, it comprises the steps:

(1) extraction of Radix Curcumae volatile oil and inclusion: weigh the Radix Curcumae of recipe quantity, utilize CO₂Supercritical extraction carries Taking, extracting pressure is 30MPa, extraction temperature 35 DEG C, CO₂Flow 13L/h, extraction time 1.5h, be extracted the volatilization of thing Radix Curcumae Oil, and raffinate, the extract beta-schardinger dextrin-being obtained by extraction carries out inclusion, the ratio between Radix Curcumae extract and beta-schardinger dextrin- Example is 1ml:3g, and the times amount that adds water is 8 times, and the inclusion time is 60 minutes, obtains clathrate A.

(2) alcohol extraction: take the stir-baked Fructus Aurantii in bran of recipe quantity, Herba Agrimoniae and Radix Curcumae raffinate and add 8 times amount 80 alcohol heating reflux Extracting 2 times, each 1.5 hours, backflow stood more than 12 hours, Aspirate supernatant, and 300 mesh filter, and obtain medicinal residues and filtrate； Filtrate is evaporated to the alcohol-extracted extract of relative density 1.15～1.25 under the conditions of 60 DEG C, standby；

(5) pelletize: take the fine powder in (4), add suitable auxiliary materials and mixing, cross 10 mesh sieves, make wet granular.

(6) be dried, granulate: put≤60 DEG C be dried, with 12 mesh sieve granulate.

(7) subpackage: use polyethylene composite film subpackage, loading amount is 10g/ bag and get final product.

The granule of the present invention application in treatment cyclomastopathy, takes after mixing it with water three times a day, each one bag.

Embodiment 4:

The preparation method of present composition capsule, it comprises the steps:

(1) extraction of Radix Curcumae volatile oil and inclusion: weigh the Radix Curcumae of recipe quantity, utilize CO₂Supercritical extraction carries Taking, extracting pressure is 30MPa, extraction temperature 35 DEG C, CO₂Flow 15L/h, extraction time 2h, be extracted thing Radix Curcumae volatile oil, And raffinate, the extract beta-schardinger dextrin-being obtained by extraction carries out inclusion, the ratio between Radix Curcumae extract and beta-schardinger dextrin- For 1ml:5g, the times amount that adds water is 8 times, and the inclusion time is 60 minutes, obtains clathrate A.

(2) alcohol extraction: take the stir-baked Fructus Aurantii in bran of recipe quantity, Herba Agrimoniae and Radix Curcumae raffinate and add 10 times amount 80 alcohol heating reflux Extracting 2 times, each 1.5 hours, backflow stood more than 12 hours, Aspirate supernatant, and 300 mesh filter, and obtain medicinal residues and filtrate； Filtrate is evaporated to the alcohol-extracted extract of relative density 1.15～1.25 under the conditions of 60 DEG C, standby；

(3) water carries: take the Resina Toxicodendri of recipe quantity, Oletum Trogopterori, Alumen, Sal Nitri and alcohol extraction medicinal residues, and the water adding 8 times amount is heated to reflux Extracting 3 times, each 2 hours, backflow stood more than 12 hours, Aspirate supernatant, and 300 mesh filter, and filtrate is under the conditions of 60 DEG C The water extracted immersing paste being concentrated under reduced pressure to give relative density 1.15～1.25 is standby；

(4) mix, be dried, pulverize: by Radix Curcumae volatile oil clathrate A, alcohol-extracted extract, the water extracted immersing paste mix homogeneously, add Semen Strychni fine powder, is dried under vacuum to dry cream, is ground into fine powder standby.

(6) be dried, granulate: put≤60 DEG C be dried, with 16 mesh sieve granulate.

(7) subpackage: with No. 1 capsule, gained capsule is carried out fill, encapsulates gained capsule aluminum-plastic-aluminum, mounted box, to obtain final product.

The capsule of the present invention application in treatment cyclomastopathy, is administered orally three times a day, each two.

Embodiment 5:

The preparation method of present composition soft capsule, it comprises the steps:

(1) extraction of Radix Curcumae volatile oil and inclusion: weigh the Radix Curcumae of recipe quantity, utilize CO₂Supercritical extraction carries Taking, extracting pressure is 30MPa, extraction temperature 35 DEG C, CO₂Flow 15L/h, extraction time 2h, be extracted thing Radix Curcumae volatile oil, And raffinate, the extract beta-schardinger dextrin-being obtained by extraction carries out inclusion, the ratio between Radix Curcumae extract and beta-schardinger dextrin- For 1ml:4g, the times amount that adds water is 4 times, and the inclusion time is 30 minutes, obtains clathrate A.

(2) alcohol extraction: take the stir-baked Fructus Aurantii in bran of recipe quantity, Herba Agrimoniae and Radix Curcumae raffinate and add 8 times amount 90% ethanol and heat back Stream extracts 2 times, and each 2 hours, backflow stood more than 12 hours, Aspirate supernatant, and 300 mesh filter, and obtain medicinal residues and filtrate； Filtrate is evaporated to the alcohol-extracted extract of relative density 1.15～1.25 under the conditions of 60 DEG C, standby；

(5) pelletize: take the fine powder in (4), add suitable auxiliary materials and mixing, make semisolid.

(6) soft capsule processed: semisolid is sealed in suitable soft capsule material, makes soft capsule

The application in treatment cyclomastopathy of the present invention flat elimination capsule, is administered orally three times a day, each two.

Embodiment 6:

The preparation method of present composition drop pill, it comprises the steps:

(1) extraction of Radix Curcumae volatile oil and inclusion: weigh the Radix Curcumae of recipe quantity, utilize CO₂Supercritical extraction carries Taking, extracting pressure is 35MPa, extraction temperature 35 DEG C, CO₂Flow 13L/h, extraction time 2h, be extracted thing Radix Curcumae volatile oil, And raffinate, the extract beta-schardinger dextrin-being obtained by extraction carries out inclusion, the ratio between Radix Curcumae extract and beta-schardinger dextrin- For 1ml:5g, the times amount that adds water is 8 times, and the inclusion time is 60 minutes, obtains clathrate A.

(2) alcohol extraction: take the stir-baked Fructus Aurantii in bran of recipe quantity, Herba Agrimoniae and Radix Curcumae raffinate and add 10 times amount 80% ethanol and heat back Stream extracts 2 times, and each 1.5 hours, backflow stood more than 12 hours, Aspirate supernatant, and 300 mesh filter, and obtain medicinal residues and filter Liquid；Filtrate is evaporated to the alcohol-extracted extract of relative density 1.15～1.25 under the conditions of 60 DEG C, standby；

(3) water carries: take the Resina Toxicodendri of recipe quantity, Oletum Trogopterori, Alumen, Sal Nitri and alcohol extraction medicinal residues, and the water adding 10 times amount heats back Stream extracts 2 times, and each 2 hours, backflow stood more than 12 hours, Aspirate supernatant, and 300 mesh filter, and filtrate is 60 DEG C of conditions Under to be concentrated under reduced pressure to give the water extracted immersing paste of relative density 1.15～1.25 standby；

(5) drop pill processed: take the fine powder in (4), adds suitable matrix body mixing, makes drop pill.

The drop pill of the present invention application in treatment cyclomastopathy, is administered orally three times a day, each 10 balls.

Claims

1. the Chinese medicine composition treating cyclomastopathy, it is characterised in that this Chinese medicine composition is to be prepared by the following method Arrive:

Take Radix Curcumae 54 weight portion, Herba Agrimoniae 54 weight portion, Oletum Trogopterori 45 weight portion, Alumen 54 weight portion, Sal Nitri 54 weight portion, do Paint 18 weight portions, stir-baked Fructus Aurantii in bran 90 weight portion, Semen Strychni Pulveratum 36 weight portion；

Above-mentioned raw materials is prepared in such a way:

(1) Radix Curcumae is through CO₂Supercritical extraction obtains Radix Curcumae extract and Radix Curcumae raffinate, by Radix Curcumae extract beta-schardinger dextrin- Inclusion, obtains clathrate；

(2) Radix Curcumae raffinate, stir-baked Fructus Aurantii in bran and Herba Agrimoniae mixing alcohol extraction step (1) obtained, filter, obtain alcohol extraction medicinal residues and Filtrate, filtrate concentrates, obtains alcohol-extracted extract；

(3) alcohol extraction medicinal residues step (2) obtained carry with Resina Toxicodendri, Oletum Trogopterori, Alumen and Sal Nitri mixing water, filter, obtain water and carry Medicinal residues and filtrate, filtrate concentrates, obtains the water extracted immersing paste；

(4) alcohol-extracted extract, the water extracted immersing paste, Semen Strychni Pulveratum and clathrate mix and get final product；The fineness of Semen Strychni Pulveratum was 80 mesh sieves.

The Chinese medicine composition for the treatment of cyclomastopathy the most according to claim 1, it is characterised in that the CO described in step (1)₂Super Critical extraction conditions is: extracting pressure is 25-35MPa, extraction temperature 25-35 DEG C, CO₂Flow 11-15L/h, extraction time 1- 2h；Radix Curcumae extract beta-schardinger dextrin-carries out inclusion condition: the ratio between Radix Curcumae extract and beta-schardinger dextrin-is 1ml:3- 5g, the times amount that adds water is 4-8 times, and the inclusion time is 20-60 minute.

The Chinese medicine composition for the treatment of cyclomastopathy the most according to claim 2, it is characterised in that the CO described in step (1)₂Super Critical extraction conditions is: extracting pressure is 35MPa, extraction temperature 30 DEG C, CO₂Flow 13L/h, extraction time 1.5h；Radix Curcumae extracts Take thing beta-schardinger dextrin-and carry out inclusion condition and be: the ratio between Radix Curcumae extract and beta-schardinger dextrin-is 1ml:5g, and add water times amount Being 8 times, the inclusion time is 60 minutes.

The Chinese medicine composition for the treatment of cyclomastopathy the most according to claim 1, it is characterised in that the alcohol extraction described in step (2) Condition is: add Radix Curcumae raffinate, stir-baked Fructus Aurantii in bran and Herba Agrimoniae 6-10 times of weight 70%-90% alcohol heating reflux of three kinds of mixture Extracting 1-3 time, each 1-2 hour, backflow stands more than 12 hours, Aspirate supernatant, and 300 mesh filter, and obtain medicinal residues and filter Liquid；Filtrate is evaporated to the alcohol-extracted extract of relative density 1.15～1.25 under the conditions of 60 DEG C.

The Chinese medicine composition for the treatment of cyclomastopathy the most according to claim 1, it is characterised in that the alcohol extraction described in step (2) Condition is: adds Radix Curcumae raffinate, stir-baked Fructus Aurantii in bran and 8 times of weight 80% alcohol heating reflux of three kinds of mixture of Herba Agrimoniae and extracts two Secondary, each 2 hours, backflow stood more than 12 hours, Aspirate supernatant, filtered, phase under the conditions of filtrate reduced in volume to 60 DEG C Clear paste to density 1.15～1.25.

The Chinese medicine composition for the treatment of cyclomastopathy the most according to claim 1, it is characterised in that

Described step (3) specifically includes following steps: take the Resina Toxicodendri of recipe quantity, Oletum Trogopterori, Alumen, Sal Nitri and alcohol extraction medicinal residues, Adding water heating and refluxing extraction 1-3 time of 6-10 times of weight of five kinds of mixture, each 1-2 hour, backflow stood more than 12 hours, Aspirate supernatant, 300 mesh filter, and filtrate is concentrated under reduced pressure to give the water of relative density 1.15～1.25 under the conditions of 60 DEG C and proposes leaching Cream；

Preferred steps (3) specifically includes following steps: takes the Resina Toxicodendri of recipe quantity, Oletum Trogopterori, Alumen, Sal Nitri and alcohol extraction medicinal residues, adds The water heating and refluxing extraction of 10 times of weight of five kinds of mixture 2 times, each 1.5 hours, backflow stood more than 12 hours, in absorption Clear liquid, filters, the clear paste of relative density 1.15～1.25 under the conditions of filtrate reduced in volume to 60 DEG C.

The Chinese medicine composition for the treatment of cyclomastopathy the most according to claim 1, it is characterised in that described step (4) is concrete Comprise the following steps: by clathrate, alcohol-extracted extract, the water extracted immersing paste mix homogeneously, add Semen Strychni Pulveratum, be dried under vacuum to dry cream, It is ground into fine powder.

The Chinese medicine composition for the treatment of cyclomastopathy the most according to claim 1, it is characterised in that described Chinese medicine composition Making dosage form with pharmaceutically acceptable adjuvant, preferred dosage form is tablet, capsule, granule, pill.

9. the preparation method of the Chinese medicine composition of the treatment cyclomastopathy described in a claim 1, it is characterised in that the method Comprise the following steps:

Above-mentioned raw materials is prepared in such a way:

(1) Radix Curcumae is through CO₂Supercritical extraction obtains Radix Curcumae extract and Radix Curcumae raffinate, by extract beta-cyclodextrin inclusion compound, Obtain clathrate；

10. the Chinese medicine composition of the treatment cyclomastopathy described in claim 1 in preparation treatment or prevention or assists treatment mammary gland Application in the medicine of hypertrophy.