Application of the present invention is to divide an application, and original application is Chinese patent CN201010131832.9, and the applying date is on March 25th, 2010, and denomination of invention is: a kind of Chinese medicine composition of treating chronic pelvic inflammatory disease and preparation method thereof.
Summary of the invention
The purpose of this invention is to provide a kind of medicine of treating chronic pelvic inflammatory disease, another object of the present invention provides the method for preparing of this medicine.
Medicine of the present invention is according to theory of Chinese medical science, develops to the pathomechanism of chronic pelvic inflammatory disease." chronic pelvic inflammatory disease " is commonly encountered diseases, the frequently-occurring disease on a kind of gynecological clinic, and prevalence is about 30%, and the multiple age is 30^-40 year crowd.Primary disease sporadically appears in Chinese medicine “ mass in the abdomen ", disease such as " leukorrhagia, disease ", " dysmenorrhea ", " infertility ".Be secondary to acute pelvic inflammatory disease mostly, not thorough because of treatment, the state of an illness shows as chronic delay, outbreak repeatedly more, and produces a series of complication (like menoxenia, dysmenorrhea, infertile, pelvic cavity venous congestion disease etc.) and cause; Or patient's body constitution is relatively poor, pathogen virulence a little less than, chronic from the beginning of being.Clinical common type has: chronic salpingitis and hydrosalpinx, adnexitis and tubo-ovarian cyst, inflammation of pelvic connective tissue.The primary disease state of an illness is obstinate, is prone to acute attack repeatedly, is difficult for thoroughly curing, and causes very big misery to patient.The relatively poor area of particularly vast rural health condition, sickness rate is very high, has a strong impact on the physical and mental health of female patient.
Be used to treat chronic pelvic inflammatory disease at present clinically, the western modern medicine treatment:, cooperate metronidazole etc. with antimicrobial drug quinolones, cephalosporins; Or naturopathy: be beneficial to the absorption of inflammation like ultrashort wave, infrared ray, medicine ion importing etc. to promote the pelvic cavity blood circulation, but therapeutic effect is all not good enough; Severe patient is granted operation.Chinese medicine: to cold-damp silt combined symptoms type: method of treatment is a dispelling cold by warming the meridian, and removing dampness is eliminated the phlegm, and Ramuli Cinnamimi and Poriae Decoction commonly used, few abdomen are by the silt ball; Or Chinese medicine decoction coloclysis, Orally taken and externally etc., though effective in cure being difficult to promote; The combination of Chinese and Western medicine adds " bitter cold Chinese medicine " treatment with antibiotic and also just attempts; On the Chinese patent medicine market, Amino-Cerv is more, and the Chinese patent medicine that can be exclusively used in the treatment chronic pelvic inflammatory disease is few in number again, far can not satisfy the demand, and therefore, the safe and effective medicine of many exploitation treatment chronic pelvic inflammatory diseases is needs of extensive patients.This medicine prescription derives from mountain, famous nest county, Anhui and Shan Yangshi TCM Gynecology old and well-known family's side handed down from one's ancestors, cures undergoing chronic pelvic inflammation and reaches thousands of examples, and is evident in efficacy.This side is made up of 12 flavor Chinese medicines.Be the mechanism of curing the disease with clearing away heat-damp and promoting diuresis, morbid leukorrhea and the undergoing chronic pelvic inflammation that is applicable to damp invasion of lower energizer has damp-heat syndrome person, not only curative effect is high, and does not have obvious adverse reaction.In a single day this side succeeds in developing through the granule that the research of science is processed, and market prospect is wide.
Flos Lonicerae merit tool heat-clearing and toxic substances removing wherein, the effect of dispelling wind and heat pathogens, nature and flavor are sweet, cold.Return lung, the heart, stomach warp.The tall and erect title with the card of controlling pyretic toxicity.These article of in recent years research proof have obvious anti-inflammatory and anti and refrigeration function.The several diseases pathogenic microorganism there is inhibitory action.The Fructus Forsythiae nature and flavor are bitter, are slightly cold.Return lung, the heart, gallbladder meridian.Merit tool heat-clearing and toxic substances removing, eliminating carbuncle eliminating stagnation, the effect of dispelling wind and heat pathogens.Be used for sore swollen toxin reaches affection due to external wind and heat more.In recent years research confirms that these article have broad-spectrum antiseptic and antiinflammatory action.Two flavors share and focus on heat-clearing and toxic substances removing.The Rhizoma Dioscoreae Collettii nature and flavor are bitter, are slightly cold.Return liver, stomach warp.Merit tool dampness removing goes turbid, the effect of expelling wind and removing dampness.Be used for married woman leucorrhea card more.The Poria nature and flavor are sweet, light, flat.GUIXIN, spleen, kidney channel.Merit tool promoting diuresis to eliminate damp pathogen.The effect of spleen-benefiting mind-tranquilizing.Be used for the wet insufficiency of the spleen card of water.The seed of Jobs tears nature and flavor are sweet, light, be slightly cold.Return the taste lung meridian.The clinical wet card of water that is used for.Polyporus property slightly sweet flavor, flat.Return stomach, wing moon bright warp.The effect of merit tool promoting diuresis to eliminate damp pathogen.The Semen Plantaginis nature and flavor are sweet, cold.Return kidney, liver, lung meridian.The effect of merit tool inducing diuresis for treating stranguria syndrome, eliminating dampness by diuresis antidiarrheal.Be used for the wet card of water more.The Rhizoma Alismatis nature and flavor are sweet, light trembles with fear, returns kidney, wing skin warp.Merit tool promoting diuresis to eliminate damp pathogen, the effect that expels the heat-evil.Be used to drench the card of drop, leukorrhagia more.Caulis Akebiae nature and flavor bitter cold.GUIXIN, small intestinal, urinary bladder channel.The effect of merit tool diuresis promoting, the stimulating milk secretion of stimulating the menstrual flow.Also diseases that are used to drench drop, leukorrhagia more.Psychotria rubra (Lour.) Poir. Chang is the good person that ancient literature is claimed Rhizoma Acori Graminei.Nature and flavor are hot, bitter, warm.GUIXIN, stomach warp.The effect of merit tool removing dampness to restore normal function of the stomach.The hot fragrant removing dampness of these article is turbid, and bitter temperature is with the stomach of being amusing.Pericarpium Citri Reticulatae, Rhizoma Pinelliae Preparata two flavors are regulated the flow of vital energy and are reduced phlegm wet.
Chinese medicine composition of the present invention is processed by following raw materials according:
The formula optimization weight proportion scope of preparation Chinese medicine composition of the present invention is:
The optimum weight proportioning of preparation Chinese medicine composition of the present invention is:
The method for preparing that above-mentioned each component is processed Chinese medicine composition of the present invention is:
Semen Coicis adds 3-10 at every turn and doubly measures with 40%~90% ethanol extraction 1-3 time, and backflow 1-3 hour, filter, merging filtrate, decompression recycling ethanol, low-temperature vacuum drying is pulverized, and is subsequent use.Pericarpium Citri Reticulatae adds 40%~90% alcohol reflux 3 times, and alcohol adding amount is respectively 12 times, 10 times and 8 times, and each 1 hour, merge backflow, filter, decompression recycling ethanol is concentrated into relative density and is 1.10~1.30 clear paste.Mixing that Flos Lonicerae, Fructus Forsythiae are criticized, Rhizoma Anemones Altaicae three is distinguished the flavor of adds 2-8 times of water gaging soaked 1~2 hour, extracted volatile oil 2-7 hour with steam distillation, filtered, and distilled other device of rear solution and collected; Medicinal residues merge with seven flavors such as remaining Semen Plantaginis, and decocte with water 1-3 time adds 12 times of water gagings at every turn, decocts 1 hour; Collecting decoction filters, and filtrating merges with above-mentioned aqueous solution; Be concentrated into the clear paste of relative density 1.10~1.30, merge above-mentioned clear paste, Semen Coicis extract adds an amount of dextrin and protein sugar; Mixing, spraying one step pelletize, subsequent use.The volatile oil of collecting adopts β-CD saturated water solution method enclose.(β-CD and volatile oil proportioning are 4g: 0.75ml), it is an amount of to add water, and heating makes dissolving, reduces to 45 ℃ to get β-CD.(oil: with dehydrated alcohol dilute, slowly inject 45 ℃ β-CD solution, constant temperature stir 2 hour, put cold, put refrigerator (10 ℃ below) vacuum drying, pulverize, sieve, be added in above-mentioned granule, mixing promptly get in 1: 3 by ratio ethanol) for volatile oil.
Traditional Chinese medicine composition for treating chronic pelvic inflammatory disease of the present invention has better curative effect.For showing the therapeutical effect of Chinese medicine composition of the present invention to chronic pelvic inflammatory disease, we have done a large amount of experimentatioies, below experimental example be used to further specify the present invention.
The Pharmacodynamic test of active extract data of preparation of the present invention
1 receives the reagent thing:
Medicine of the present invention: supplier: Jiangsu JumpCan Medicines Co., Ltd., lot number: 020910.
FULE KELI: Hangzhou Tianmushan Pharmaceutical Co., Ltd., 20022701,2 times/d of lot number, 2 bags/inferior, other medicines of 6g/ bag are commercially available qualified medicine
4. experimental animal: Kunming mouse and Wistar rat provide by Anhui Prov. Medical Science Inst.'s animal center,
2 experimental techniques and result:
2.1 therapeutic test to the chronic pelvic inflammatory disease rat model
2.1.1 the Pyrogentisinic Acid causes the therapeutic test of rat chronic pelvic inflammatory disease model
[1]
2.1.1.1 test method
1. the preparation of phenol rubber cement: get phenol 5ml, tragakanta 19, glycerol 4ml, adding distil water are made into the rubber cement that contains 25% phenol to 20ml.
2. chronic pelvic inflammatory disease replication of Model: animal is used ether inhalation anesthesia, abdominal part routine disinfection, the about 0.8~1cm of median incision of lower abdomen; Expose the uterus, with No. 4 syringe needles in the uterus the careful inserting needle of crotch, slowly inject phenol rubber cement 0.04ml to the ovary direction; Abdomen is closed in layering then; Sterilization art district, other gets 10 and opens abdomen and do not inject the phenol rubber cement, as Sham-operated control group.
3. medication: after the modeling 7d with 60 of animal patterns by being divided into 5 groups at random, 10 every group, positive controls (8.00g crude drug/kg wherein; Be equivalent to 20 times of clinical people's consumption 24g), medicine of the present invention in a small amount (7.75g crude drug/kg), middle amount (15.50g crude drug/kg), a large amount of (group (calculating 5,10 and 20 times that are equivalent to clinical people's consumption 93g) of 31.00g crude drug/kg) by kg body weight, other adds totally 6 groups of Sham-operated control group (waiting the capacity distilled water), administration according to dosage (2.0ml/100g body weight) respectively; Continuous 20d, 24h behind the last medicine presses the 40mg/kg intraperitoneal anesthesia with pentobarbital sodium; Perusal is also write down the inflammation of uterus variation; Win the uterus, take by weighing both sides weight respectively, and calculate its weight difference; Get then and cause scorching Aconitum carmichaeli Debx. palace and put in 10% formalin solution fixing; Conventional section, HE dyeing, light microscopic is observed the uterus morphological changes of various tissue components down.
Uterus weight difference=left side uterus weight one right side uterus weight
2.1.1.2 result of the test, result are seen table 1,2
Table 1 medicine Pyrogentisinic Acid of the present invention rubber cement causes the influence (x ± s) of chronic pelvic inflammatory disease rat model uterus weight
With sham operated rats than #P<0.05, ##P<0.01 and model group ratio
*P<0.05
*P<0.01
Table 2 medicine Pyrogentisinic Acid of the present invention rubber cement duplicates the uterus pathology integrated value of the therapeutical effect of rat chronic pelvic inflammatory disease model
With sham operated rats than well P<0.05, ##P<0.01 and model group ratio
*P<0.05
*P<0.01
Perusal: it is visible to open the rat abdominal cavity naked eyes, the obvious swelling in Aconitum carmichaeli Debx. palace of injection phenol rubber cement, hyperemia, and what have has a purulence thing.Do not inject phenol rubber cement Aconitum carmichaeli Debx. palace and sham operated rats uterus ratio, do not have notable difference.
By table 1,2 visible: medicine Pyrogentisinic Acid rubber cement of the present invention causes pelvic inflammatory disease rat model uterus weight to be had obviously and alleviates; Pathological replacement by uterine cancer cell is visible: it is inaccessible that the phenol rubber cement causes the adhesion of rat uterus chamber, and pathological changes such as epithelial cell degeneration necrosis, chronic inflammatory cell infiltration, inner membrance congestion and edema explain that duplicating the casual property pelvic inflammatory disease model of rat with the phenol rubber cement sets up; After with medicine of the present invention, all pathological symptoms improve significantly, and explain that medicine Pyrogentisinic Acid rubber cement of the present invention causes the pelvic inflammatory disease rat model obvious treatment effect is arranged.
2.1.2 escherichia coli are caused the therapeutical effect of rat chronic pelvic inflammatory disease model
[2]
2.1.2.1 test method:
1. chronic pelvic inflammatory disease replication of Model: get 60 rats; Use ether inhalation anesthesia; The abdominal part routine disinfection, the about 0.8~1cm of median incision of lower abdomen exposes the uterus; With No. 4 syringe needles in the uterus the careful inserting needle of crotch, slowly inject the escherichia coli suspension (3 * 10 of 0.2ml from the uterus, left side to the ovary direction through the trial test result
8CFU/ml), abdomen is closed in layering, and sterilization art district keeps 10 and opens abdomen and do not inject the escherichia coli suspension as Sham-operated control group, before injecting bacterium liquid, with syringe mechanical damage endometrial tissue, sews up the incision, and recovers drinking-water, normally cleans raising.
2. medication: 7d begins the modeling animal is divided into 5 groups at random after the modeling, 10 every group, adds Sham-operated control group, totally 6 groups; Press dosed administration in the table 2 (2.0ml/100g body weight), continuous 20d, behind the last medicine behind the 24h, with animal with pentobarbital sodium 40mg/kg intraperitoneal anesthesia; Cut open the belly, perusal is also write down the inflammation of uterus variation, wins the uterus; Take by weighing both sides weight respectively, and calculate its weight difference, get then and cause scorching Aconitum carmichaeli Debx. palace and put in 10% formalin solution fixing; Conventional section, HE dyeing, light microscopic is observed the uterus morphological changes of various tissue components down.2.1.2.2 result of the test result sees table 3 as a result, 4,
Table 3 medicine of the present invention causes the influence (x ± s) of chronic pelvic inflammatory disease rat model uterus weight to escherichia coli
With sham operated rats than #P<0.05, ##P<0.01 and model group ratio
*P<0.05
*P<0.01
Table 4 pair escherichia coli are duplicated the uterus pathology integrated value (X ± s) of the therapeutical effect of rat chronic pelvic inflammatory disease model
With sham operated rats than #P<0.05, ##P<0.01 and model group ratio
*P<0.05
*P<0.01
Perusal: it is visible to open the rat abdominal cavity naked eyes, the obvious swelling in Aconitum carmichaeli Debx. palace of injection escherichia coli, hyperemia.Do not inject escherichia coli Aconitum carmichaeli Debx. palace and sham operated rats uterus ratio, do not have notable difference.
By table 3,4 is visible: medicine of the present invention causes pelvic inflammatory disease rat model uterus weight to escherichia coli to be had obviously and alleviates; Pathological replacement by uterine cancer cell is visible: it is inaccessible that escherichia coli cause the rat uterus intrauterine adhesion, and pathological changes such as epithelial cell degeneration necrosis, chronic inflammatory cell infiltration, inner membrance congestion and edema explain that duplicating the casual property pelvic inflammatory disease model of rat with escherichia coli sets up; After with medicine of the present invention, all pathological symptoms improve significantly, and explain that medicine of the present invention causes the pelvic inflammatory disease rat model to escherichia coli the obvious treatment effect is arranged.
2.2 antibacterial tests
2.2.1 in-vitro antibacterial test
2.2.1.1 materials and methods
1. strain: 8 strains of Gartner Salmonella, staphylococcus aureus 11 strains (containing type strain ATCC25923), staphylococcus epidermidis 9 strains; Beta hemolytic streptococcus 8 strains, pneumobacillus 7 strains, escherichia coli 11 strains (containing reference culture ATCC25922); Alpha streptococcus 8 strains, Bacillus proteus 10 strains, bacillus pyocyaneus 9 strains; Candida albicans 7 strains; More than 8 kind of 68 strain bacterial strain, wherein reference culture is preserved the center from Beijing biological product checks institute strain, all the other bacterial strains are examined the BIAO and BEN separation by Anhui Chinese Medicine College microorganism teaching and research room and are obtained from clinical outside.Strain was write " national Clinical Laboratory rule of operation " in 1997 according to Ministry of Public Health Department of Medical Administration.
2. culture medium: select the MH culture medium for use; And add 5% calf serum; Fungus, Candida albicans are selected husky Bao Shi culture medium for use.
3. MIC experiment
Supply the preparation of examination bacterium liquid: individual strains tested is inoculated in respectively in the above-mentioned corresponding culture medium; Cultivate 24h for 37 ℃; Wherein inoculate in the second chain bacterium culture medium and add 5% calf serum, the Gartner Salmonella adds 5% human blood, cultivates 6h for 37 ℃; Make standard bacterium colony subcultivation in fluid medium behind the 6h, the adjustment bacterial concentration is 10
8CFU/ml, subsequent use.
The preparation of pastille culture medium: in supplying the examination culture medium, add prepared beforehand good medicine medicinal liquid of the present invention and positive drug respectively; Make the drug level of culture medium be respectively 200mg, 100mg, 50mg, 25mg, 12.5mg, 6.25mg, 3.125mg, 1.56mg and 0.78mg/ml, other establish one not the flat board of drug make negative control.
Supply the examination bacterial classification inoculation: get confession examination bacterium liquid one ring (bacteria containing amount is about 104CFU/ml) respectively with inoculating loop and be inoculated on the culture medium of different pharmaceutical concentration; 37 ℃ of temperature are incubated, and Candida albicans is cultivated 48h, behind other antibacterial culturing 24h; Observed result; On the flat board of front and back 2 variable concentrations gradients medicine, make the concentration of the unexpected minimizing 80%~90% of bacterial number be MIC, the result sees table 5.
Table 5 medicine of the present invention is measured the result to 68 strain antibacterial MIC
Visible by table 5, medicine of the present invention all has certain bacteriostasis outward to above-mentioned various bacterial bodies.What wherein effect was the strongest is to staphylococcus aureus, its MIC
50Be 0.78mg/ml.
2.2.1.2 antibacterial tests in the body
2.2.2.1 protective effect to the candida albicans infection mice
Get 50 of body weight 18-22g mices; Be divided into distilled water group, FULE KELI group, little, the heavy dose of group of neutralization of medicine of the present invention at random by body weight; Each group is pressed oral dose administration in the table 6 (0.25ml/10g body weight) respectively; Continuous 7d, (bacterial concentration is 4.0 * 10 in respectively organizing ip in mice Candida albicans suspension 0.4ml according to the trial test result behind the 40min on the 3rd day after the administration
8CFU/ml) 0.1ml 5% yeast soln, the death condition of observing mice in the 7d then is total to 9d, and the result sees table 6,7.
Table 6 medicine of the present invention is to candida albicans infection dead mouse distribution situation
Table 7 medicine of the present invention is to the protective effect of candida albicans infection mice
2.8.1.2 to the intravital protective effect of coli-infection mice
Get 50 of body weight 18~22g mices; Be divided into the happy positive group of distilled water group, woman at random and medicine of the present invention is little, in and heavy dose of group; According to the trial test result, each group is pressed table 8 oral dose administration (0.25ml/10g body weight) respectively, continuously 7d; Behind administration 3d 40min, each organizes ip in mice Escherichia coli bacteria liquid 0.5ml (3 * 10
8CFU/ml), observe the death condition of mice in the 7d then, be total to 9d, the result sees table 8,9.
Table 8 medicine of the present invention is to coli-infection dead mouse distribution situation
Table 9 medicine of the present invention is to the protective effect of coli-infection mice
2.3.2 writhing method
Get 50 of body weight 18~22g mices, the male and female dual-purpose is divided into 5 groups at random, presses oral dose administration in the table 12 (0.25ml/10g body weight) respectively, successive administration 5d.40min lumbar injection 0.7% acetum 0.1ml/10g body weight behind the last medicine, behind the record injection acetic acid, each organizes each mice 10min, turns round the body number of times in the 20min respectively, and the result sees table 12.
Table 12 medicine of the present invention causes the inhibitory action (n=10x ± s) of pain to writhing method
With distilled water group ratio
*P<0.05
*P<0.01
Visible by table 12, the pain due to medicine Dichlorodiphenyl Acetate of the present invention stimulates has obvious inhibitory action, and with distilled water group ratio, its medium and small, heavy dose of group has significant difference.
2.4 antiinflammatory test
2.4.1 xylol causes the inhibitory action of mice ear
Get 50 of body weight 18~22g male mices, be divided into 5 groups at random.Press dosed administration in the table 13, (0.25ml/10g body weight), continuous use 5d, 40min behind the last medicine, every Mus left side ear is coated with xylene 0.1ml, and auris dextra is coated with equivalent NS.Put to death mice behind the 1h, cut auricle and respectively get an auricle with the 0.8cm card punch in mice two ear same area, in scales/electronic balance weighing, as the swelling degree, and calculate swelling resistance rate with two ear weight differences, the result sees table 13.
Swelling degree (g)=left auricle weight-auris dextra sheet is heavy
Swelling rate (%)=(swelling degree/left auricle is heavy) * 100%
Swelling resistance rate (%)=(model group-administration group)/model group * 100%
Table 13 medicine xylol of the present invention causes the inhibitory action (n=10x ± s) of mice ear
With distilled water group ratio
*P<0.05
*P<0.01
Visible by table 13, the mice ear due to the medicine xylol of the present invention has the obvious suppression effect, with distilled water group ratio significant difference is arranged.
2.4.2 Ovum Gallus domesticus album is caused the inhibitory action of rat paw edema
Get 50 of body weight 180~220g male rats, be divided into 5 groups at random, press oral dose administration in the table 14 (2.0ml/100g body weight), continuous use 7d.Survey right back sufficient volume with volumetric method, 40min after the last administration then, the subcutaneous injection of the right back sufficient intestinal of every Mus 0.1ml 100% Ovum Gallus domesticus album; And respectively at cause scorching back 0.5,1,1.5,2,3,4h surveys sufficient volume; Deduct with this volume and to cause scorching front foot volume as paw swelling, the result sees table 14,15.
Table 14 medicine of the present invention causes the inhibitory action (n=10x ± s) of rat paw edema to Ovum Gallus domesticus album
With distilled water group ratio
*P<0.05
*P<0.01
Table 15 medicine of the present invention causes the suppression ratio effect (n=10x ± s) of rat paw edema to Ovum Gallus domesticus album
By table 14,15 is visible, and medicine of the present invention causes rat paw edema to Ovum Gallus domesticus album has the obvious suppression effect; It is medium and small, in, heavy dose of group of effect be obvious; Middle amount group 0.5h just has the obvious suppression effect, and the inhibitory action of a large amount of groups remains to 4h always, with the distilled water group significant difference is arranged.
2.4.3 cotton pellet method is caused the inhibitory action of rat granulation hyperplasia
Get 50 of body weight 200~220g male rats, be divided into 5 groups at random, under the etherization aseptic condition, through autoclaving, each cotton balls adds ampicillin 1mg/0.1ml with the cotton balls of having weighed, and after 50 ℃ of oven dry, it is subcutaneous to implant rat right side groin.After animal is clear-headed, by the continuous 7d of above-mentioned oral dose administration (2.0ml/100g body weight).40min puts to death rat after the last administration, peels off and take out granulation tissue, claims its weight, deducts the raw cotton ball weight and gets the granulation weight in wet base, and dry 24h in 90 ℃ of baking ovens weighs again then, and deducts former cotton balls recuperation granulation dry weight, and the result sees table 16.
Table 16 medicine of the present invention causes inhibitory action (the n=10 x ± s) of granulation hyperplasia to cotton pellet method
With the model group ratio
*P<0.05
*P<0.01
Visible by table 16, medicine of the present invention can obviously suppress cotton balls and cause granulation hyperplasia, and granulation weight in wet base and dry weight are all obviously reduced, and with the model group ratio, highly significant difference is arranged.
2.5 medicine of the present invention is to the influence of the hemorheology index of rat model
Get 250~350g rat, the male and female dual-purpose, be divided at random normal control group, model group, positive controls, medicine of the present invention little, in, a large amount of group; Cause the modeling of rat chronic pelvic inflammatory disease method by phenol, oral dose administration in the table 17 (2.0ml/100g body weight), 20d continuously; 24h after the last administration presses the 40mg/kg intraperitoneal anesthesia with pentobarbital sodium, the ventral aorta blood drawing; Do the hemorheological property inspection, survey clotting time with slide method simultaneously.The result sees table 17.
Table 17 medicine of the present invention to the influence of chronic pelvic inflammatory disease rat WBV ratio (x ± s, n=10)
With the distilled water group than ##p<0.01 and model group ratio
*P<0.01
Visible by table 17, the viscosity of the hemorheology index of rat model obviously increases; And after using medicine of the present invention, hemorheological property is obviously improved, and degree of killing reduces, and explains that medicine of the present invention obviously improves the hemorheological property of chronic pelvic inflammatory disease rat.
2.6 medicine of the present invention is to the influence of the mda content of chronic pelvic inflammatory disease rat model
Get 250~350g rat, the male and female dual-purpose, be divided at random Sham-operated control group, model group, positive controls, woman's relaxation grain little, in, a large amount of group; Cause the casual property pelvic inflammatory disease method modeling of rat by escherichia coli, use 20d continuously by dosage in the table 18,24h behind the last medicine; Abdominal aortic blood; (Biochemics Inc.'s lot number is built up in Nanjing: explain that 20021230) detect its trap at 754 spectrophotometer 532nm places, the result sees table 18 to measure test kit by malonaldehyde.
Table 18 medicine of the present invention to the influence of the mda content of chronic pelvic inflammatory disease rat model (x ± s, n=10)
With the distilled water group than ##p<0.01 and model group ratio
*P<0.01
By the visible model group mda content of table 18 apparently higher than, with the distilled water group significant difference is arranged, and with
Mda content obviously descends behind the invention medicine.
2.7 medicine of the present invention is to the influence of uterus smooth muscle contraction
[3]
2.7.1 to the influence of shrinking at the body uterine smooth muscle
Get not 50 of pregnant rats of female health, body weight 180~220g.Be divided at random normal control group, positive controls, medicine of the present invention little, in, a large amount of group, behind the 40mg/kg pentobarbital sodium iv anesthetized animal, face upward the position and be fixed in operating-table, be about 4^-5cm through median incision of lower abdomen and go into abdomen, find out an Aconitum carmichaeli Debx. palace.Choose from cornua uteri and to be about the 5cm section, in bring a cotton thread out into the open in succession on tonotransducer, and fix with special glass; That continues makes a kerf under xiphoid-process; Find out duodenum, put one within it and irritate the stomach syringe needle in order to administration, animal is with operating lamp irradiation insulation; Tonotransducer is connected in MedLab bio signal acquisition processing system (Meiyi Science & Technology Co., Ltd., Nanjing's production); Give the uterus preload, trace the normal uterus shrinkage curve after stablizing, then through duodenal administration (2ml/100g); Observe and write down after the administration 0.5,1,1.5,2,3 respectively, 4h uterine contraction situation, before and after the measurements and calculations administration in the variation of body uterine contraction amplitude and contraction frequency.The result sees table 18,19,20.
Following embodiment is further openly the present invention, need to prove that these embodiment are merely optimal way of the present invention, does not limit the present invention and requires the scope protected.
Embodiment 1
Semen Coicis adds 10 times of amounts with 40% ethanol extraction 1 time at every turn, refluxes 2 hours, filter, and merging filtrate, decompression recycling ethanol, low-temperature vacuum drying is pulverized, and is subsequent use.Pericarpium Citri Reticulatae adds 40% alcohol reflux 3 times, and alcohol adding amount is respectively 12 times, 10 times and 8 times, and each 1 hour, merge backflow, filter, decompression recycling ethanol is concentrated into relative density and is 1.15 clear paste.Mixing that Flos Lonicerae, Fructus Forsythiae are criticized, Rhizoma Anemones Altaicae three is distinguished the flavor of adds 2 times of water gagings soaked 1 hour, extracted volatile oil 2 hours with steam distillation, filtered, and distilled other device of rear solution and collected; Medicinal residues merge with seven flavors such as remaining Semen Plantaginis, and decocte with water 1 time adds 12 times of water gagings at every turn, decocts 1 hour; Collecting decoction filters, and filtrating merges with above-mentioned aqueous solution; Be concentrated into the clear paste of relative density 1.10, merge above-mentioned clear paste, Semen Coicis extract adds an amount of dextrin and protein sugar; Mixing, spraying one step pelletize, subsequent use.The volatile oil of collecting adopts β-CD saturated water solution method enclose.(β-CD and volatile oil proportioning are 4g: 0.75ml), it is an amount of to add water, and heating makes dissolving, reduces to 45 ℃ to get β-CD.(oil: with dehydrated alcohol dilute, slowly inject 45 ℃ β-CD solution, constant temperature stir 2 hour, put cold, put refrigerator (10 ℃ below) vacuum drying, pulverize, sieve, be added in above-mentioned granule, mixing promptly get in 1: 3 by ratio ethanol) for volatile oil.
Embodiment 2
Semen Coicis adds 10 times of amounts with 60% ethanol extraction 2 times at every turn, refluxes 3 hours, filter, and merging filtrate, decompression recycling ethanol, low-temperature vacuum drying is pulverized, and is subsequent use.Pericarpium Citri Reticulatae adds 90% alcohol reflux 3 times, and alcohol adding amount is respectively 12 times, 10 times and 8 times, and each 1 hour, merge backflow, filter, decompression recycling ethanol is concentrated into relative density and is 1.10 clear paste.Mixing that Flos Lonicerae, Fructus Forsythiae are criticized, Rhizoma Anemones Altaicae three is distinguished the flavor of adds 8 times of water gagings soaked 2 hours, extracted volatile oil 7 hours with steam distillation, filtered, and distilled other device of rear solution and collected; Medicinal residues merge with seven flavors such as remaining Semen Plantaginis, and decocte with water 3 times adds 12 times of water gagings at every turn, decocts 1 hour; Collecting decoction filters, and filtrating merges with above-mentioned aqueous solution; Be concentrated into the clear paste of relative density 1.30, merge above-mentioned clear paste, Semen Coicis extract adds an amount of dextrin and protein sugar; Mixing, spraying one step pelletize, subsequent use.The volatile oil of collecting adopts β-CD saturated water solution method enclose.(β-CD and volatile oil proportioning are 4g: 0.75ml), it is an amount of to add water, and heating makes dissolving, reduces to 45 ℃ to get β-CD.(oil: with dehydrated alcohol dilute, slowly inject 45 ℃ β-CD solution, constant temperature stir 2 hour, put cold, put refrigerator (10 ℃ below) vacuum drying, pulverize, sieve, be added in above-mentioned granule, pulverize, pill promptly get in 1: 3 by ratio ethanol) for volatile oil.
Embodiment 3
Semen Coicis adds 6 times of amounts with 70% ethanol extraction 3 times at every turn, refluxes 2 hours, filter, and merging filtrate, decompression recycling ethanol, low-temperature vacuum drying is pulverized, and is subsequent use.Pericarpium Citri Reticulatae adds 90% alcohol reflux 3 times, and alcohol adding amount is respectively 12 times, 10 times and 8 times, and each 1 hour, merge backflow, filter, decompression recycling ethanol is concentrated into relative density and is 1.30 clear paste.Mixing that Flos Lonicerae, Fructus Forsythiae are criticized, Rhizoma Anemones Altaicae three is distinguished the flavor of adds 4 times of water gagings soaked 2 hours, extracted volatile oil 4 hours with steam distillation, filtered, and distilled other device of rear solution and collected; Medicinal residues merge with seven flavors such as remaining Semen Plantaginis, and decocte with water 1 time adds 12 times of water gagings at every turn, decocts 1 hour; Collecting decoction filters, and filtrating merges with above-mentioned aqueous solution; Be concentrated into the clear paste of relative density 1.20, merge above-mentioned clear paste, Semen Coicis extract adds an amount of dextrin and protein sugar; Mixing, spraying one step pelletize, subsequent use.The volatile oil of collecting adopts β-CD saturated water solution method enclose.(β-CD and volatile oil proportioning are 4g: 0.75ml), it is an amount of to add water, and heating makes dissolving, reduces to 45 ℃ to get β-CD.(oil: with dehydrated alcohol dilute, slowly inject 45 ℃ β-CD solution, constant temperature stir 2 hour, put cold in 1: 3 by ratio ethanol) for volatile oil; Put refrigerator (below 10 ℃) vacuum drying, pulverize, sieve, be added in the above-mentioned granule; Mixing, capsule charge promptly gets.
Embodiment 4
Semen Coicis adds 8 times of amounts with 60% ethanol extraction 2 times at every turn, refluxes 1 hour, filter, and merging filtrate, decompression recycling ethanol, low-temperature vacuum drying is pulverized, and is subsequent use.Pericarpium Citri Reticulatae adds 90% alcohol reflux 3 times, and alcohol adding amount is respectively 12 times, 10 times and 8 times, and each 1 hour, merge backflow, filter, decompression recycling ethanol is concentrated into relative density and is 1.30 clear paste.Mixing that Flos Lonicerae, Fructus Forsythiae are criticized, Rhizoma Anemones Altaicae three is distinguished the flavor of adds 4 times of water gagings soaked 2 hours, extracted volatile oil 5 hours with steam distillation, filtered, and distilled other device of rear solution and collected; Medicinal residues merge with seven flavors such as remaining Semen Plantaginis, and decocte with water 1 time adds 12 times of water gagings at every turn, decocts 1 hour; Collecting decoction filters, and filtrating merges with above-mentioned aqueous solution; Be concentrated into the clear paste of relative density 1.20, merge above-mentioned clear paste, Semen Coicis extract adds an amount of dextrin and protein sugar; Mixing, spraying one step pelletize, subsequent use.The volatile oil of collecting adopts β-CD saturated water solution method enclose.(β-CD and volatile oil proportioning are 4g: 0.75ml), it is an amount of to add water, and heating makes dissolving, reduces to 45 ℃ to get β-CD.Volatile oil in 1: 3 (oil: ratio ethanol) is diluted with dehydrated alcohol, slowly injects β-CD solution of 45 ℃, and constant temperature stirred 2 hours, puts coldly, puts refrigerator (below 10 ℃) vacuum drying, pulverizes, and sieves, be added in the above-mentioned granule, mixing, tabletting promptly gets.
Embodiment 5
Semen Coicis adds 6 times of amounts with 60% ethanol extraction 1 time at every turn, refluxes 2 hours, filter, and merging filtrate, decompression recycling ethanol, low-temperature vacuum drying is pulverized, and is subsequent use.Pericarpium Citri Reticulatae adds 50% alcohol reflux 3 times, and alcohol adding amount is respectively 12 times, 10 times and 8 times, and each 1 hour, merge backflow, filter, decompression recycling ethanol is concentrated into relative density and is 1.15 clear paste.Mixing that Flos Lonicerae, Fructus Forsythiae are criticized, Rhizoma Anemones Altaicae three is distinguished the flavor of adds 6 times of water gagings soaked 2 hours, extracted volatile oil 6 hours with steam distillation, filtered, and distilled other device of rear solution and collected; Medicinal residues merge with seven flavors such as remaining Semen Plantaginis, and decocte with water 3 times adds 12 times of water gagings at every turn, decocts 1 hour; Collecting decoction filters, and filtrating merges with above-mentioned aqueous solution; Be concentrated into the clear paste of relative density 1.15, merge above-mentioned clear paste, Semen Coicis extract adds an amount of dextrin and protein sugar; Mixing, spraying one step pelletize, subsequent use.The volatile oil of collecting adopts β-CD saturated water solution method enclose.(β-CD and volatile oil proportioning are 4g: 0.75ml), it is an amount of to add water, and heating makes dissolving, reduces to 45 ℃ to get β-CD.(oil: with dehydrated alcohol dilute, slowly inject 45 ℃ β-CD solution, constant temperature stir 2 hour, put cold, put refrigerator (10 ℃ below) vacuum drying in 1: 3 by ratio ethanol) for volatile oil; Pulverize, sieve, be added in the above-mentioned granule mixing; Add the water for injection dissolving, embedding, sterilization promptly gets.
Embodiment 6
Semen Coicis adds 5 times of amounts with 75% ethanol extraction 3 times at every turn, refluxes 1 hour, filter, and merging filtrate, decompression recycling ethanol, low-temperature vacuum drying is pulverized, and is subsequent use.Pericarpium Citri Reticulatae adds 50% alcohol reflux 3 times, and alcohol adding amount is respectively 12 times, 10 times and 8 times, and each 1 hour, merge backflow, filter, decompression recycling ethanol is concentrated into relative density and is 1.20 clear paste.Mixing that Flos Lonicerae, Fructus Forsythiae are criticized, Rhizoma Anemones Altaicae three is distinguished the flavor of adds 2-8 times of water gaging soaked 1~2 hour, extracted volatile oil 2-7 hour with steam distillation, filtered, and distilled other device of rear solution and collected; Medicinal residues merge with seven flavors such as remaining Semen Plantaginis, and decocte with water 2 times adds 12 times of water gagings at every turn, decocts 1 hour; Collecting decoction filters, and filtrating merges with above-mentioned aqueous solution; Be concentrated into the clear paste of relative density 1.20, merge above-mentioned clear paste, Semen Coicis extract adds an amount of dextrin and protein sugar; Mixing, spraying one step pelletize, subsequent use.The volatile oil of collecting adopts β-CD saturated water solution method enclose.(β-CD and volatile oil proportioning are 4g: 0.75ml), it is an amount of to add water, and heating makes dissolving, reduces to 45 ℃ to get β-CD.(oil: with dehydrated alcohol dilute, slowly inject 45 ℃ β-CD solution, constant temperature stir 2 hour, put cold in 1: 3 by ratio ethanol) for volatile oil; Put refrigerator (below 10 ℃) vacuum drying, pulverize, sieve, be added in the above-mentioned granule; Pulverize, mixing promptly gets powder.
Promptly get.
Embodiment 7
Semen Coicis adds 6 times of amounts with 80% ethanol extraction 3 times at every turn, refluxes 2 hours, filter, and merging filtrate, decompression recycling ethanol, low-temperature vacuum drying is pulverized, and is subsequent use.Pericarpium Citri Reticulatae adds 60 alcohol reflux 3 times, and alcohol adding amount is respectively 12 times, 10 times and 8 times, and each 1 hour, merge backflow, filter, decompression recycling ethanol is concentrated into relative density and is 1.10~1.20 clear paste.Mixing that Flos Lonicerae, Fructus Forsythiae are criticized, Rhizoma Anemones Altaicae three is distinguished the flavor of adds 7 times of water gagings soaked 1.5 hours, extracted volatile oil 3 hours with steam distillation, filtered, and distilled other device of rear solution and collected; Medicinal residues merge with seven flavors such as remaining Semen Plantaginis, and decocte with water 2 times adds 12 times of water gagings at every turn, decocts 1 hour; Collecting decoction filters, and filtrating merges with above-mentioned aqueous solution; Be concentrated into the clear paste of relative density 1.10~1.20, merge above-mentioned clear paste, Semen Coicis extract adds an amount of dextrin and protein sugar; Mixing, spraying one step pelletize, subsequent use.The volatile oil of collecting adopts β-CD saturated water solution method enclose.(β-CD and volatile oil proportioning are 4g: 0.75ml), it is an amount of to add water, and heating makes dissolving, reduces to 45 ℃ to get β-CD.(oil: with dehydrated alcohol dilute, slowly inject 45 ℃ β-CD solution, constant temperature stir 2 hour, put cold, put refrigerator (10 ℃ below) vacuum drying, pulverize, sieve, be added in above-mentioned granule, mixing promptly get in 1: 3 by ratio ethanol) for volatile oil.
Embodiment 8
Semen Coicis adds 3 times of amounts with 40% ethanol extraction 1 time at every turn, refluxes 1 hour, filter, and merging filtrate, decompression recycling ethanol, low-temperature vacuum drying is pulverized, and is subsequent use.Pericarpium Citri Reticulatae adds 40% alcohol reflux 3 times, and alcohol adding amount is respectively 12 times, 10 times and 8 times, and each 1 hour, merge backflow, filter, decompression recycling ethanol is concentrated into relative density and is 1.10 clear paste.Mixing that Flos Lonicerae, Fructus Forsythiae are criticized, Rhizoma Anemones Altaicae three is distinguished the flavor of adds 2 times of water gagings soaked 1 hour, extracted volatile oil 2 hours with steam distillation, filtered, and distilled other device of rear solution and collected; Medicinal residues merge with seven flavors such as remaining Semen Plantaginis, and decocte with water 1 time adds 12 times of water gagings at every turn, decocts 1 hour; Collecting decoction filters, and filtrating merges with above-mentioned aqueous solution; Be concentrated into the clear paste of relative density 1.10, merge above-mentioned clear paste, Semen Coicis extract adds an amount of dextrin and protein sugar; Mixing, spraying one step pelletize, subsequent use.The volatile oil of collecting adopts β-CD saturated water solution method enclose.(β-CD and volatile oil proportioning are 4g: 0.75ml), it is an amount of to add water, and heating makes dissolving, reduces to 45 ℃ to get β-CD.(oil: with dehydrated alcohol dilute, slowly inject 45 ℃ β-CD solution, constant temperature stir 2 hour, put cold, put refrigerator (10 ℃ below) vacuum drying, pulverize, sieve, be added in above-mentioned granule, mixing promptly get in 1: 3 by ratio ethanol) for volatile oil.
Embodiment 9
Semen Coicis adds 4 times of amounts with 45 ethanol extraction 2 times at every turn, refluxes 2 hours, filter, and merging filtrate, decompression recycling ethanol, low-temperature vacuum drying is pulverized, and is subsequent use.Pericarpium Citri Reticulatae adds 45 alcohol reflux 3 times, and alcohol adding amount is respectively 12 times, 10 times and 8 times, and each 1 hour, merge backflow, filter, decompression recycling ethanol is concentrated into relative density and is 1.20 clear paste.Mixing that Flos Lonicerae, Fructus Forsythiae are criticized, Rhizoma Anemones Altaicae three is distinguished the flavor of adds 3 times of water gagings soaked 1.5 hours, extracted volatile oil 3 hours with steam distillation, filtered, and distilled other device of rear solution and collected; Medicinal residues merge with seven flavors such as remaining Semen Plantaginis, and decocte with water 2 times adds 12 times of water gagings at every turn, decocts 1 hour; Collecting decoction filters, and filtrating merges with above-mentioned aqueous solution; Be concentrated into the clear paste of relative density 1.10~1.30, merge above-mentioned clear paste, Semen Coicis extract adds an amount of dextrin and protein sugar; Mixing, spraying one step pelletize, subsequent use.The volatile oil of collecting adopts β-CD saturated water solution method enclose.(β-CD and volatile oil proportioning are 4g: 0.75ml), it is an amount of to add water, and heating makes dissolving, reduces to 45 ℃ to get β-CD.(oil: with dehydrated alcohol dilute, slowly inject 45 ℃ β-CD solution, constant temperature stir 2 hour, put cold, put refrigerator (10 ℃ below) vacuum drying, pulverize, sieve, be added in above-mentioned granule, mixing promptly get in 1: 3 by ratio ethanol) for volatile oil.
Embodiment 10
Semen Coicis adds 5 times of amounts with 50% ethanol extraction 3 times at every turn, refluxes 3 hours, filter, and merging filtrate, decompression recycling ethanol, low-temperature vacuum drying is pulverized, and is subsequent use.Pericarpium Citri Reticulatae adds 50% alcohol reflux 3 times, and alcohol adding amount is respectively 12 times, 10 times and 8 times, and each 1 hour, merge backflow, filter, decompression recycling ethanol is concentrated into relative density and is 1.30 clear paste.Mixing that Flos Lonicerae, Fructus Forsythiae are criticized, Rhizoma Anemones Altaicae three is distinguished the flavor of adds 4 times of water gagings soaked 2 hours, extracted volatile oil 4 hours with steam distillation, filtered, and distilled other device of rear solution and collected; Medicinal residues merge with seven flavors such as remaining Semen Plantaginis, and decocte with water 3 times adds 12 times of water gagings at every turn, decocts 1 hour; Collecting decoction filters, and filtrating merges with above-mentioned aqueous solution; Be concentrated into the clear paste of relative density 1.30, merge above-mentioned clear paste, Semen Coicis extract adds an amount of dextrin and protein sugar; Mixing, spraying one step pelletize, subsequent use.The volatile oil of collecting adopts β-CD saturated water solution method enclose.(β-CD and volatile oil proportioning are 4g: 0.75ml), it is an amount of to add water, and heating makes dissolving, reduces to 45 ℃ to get β-CD.(oil: with dehydrated alcohol dilute, slowly inject 45 ℃ β-CD solution, constant temperature stir 2 hour, put cold, put refrigerator (10 ℃ below) vacuum drying, pulverize, sieve, be added in above-mentioned granule, mixing promptly get in 1: 3 by ratio ethanol) for volatile oil.
Embodiment 11
Semen Coicis adds 6 times of amounts with 55% ethanol extraction 1 time at every turn, refluxes 1 hour, filter, and merging filtrate, decompression recycling ethanol, low-temperature vacuum drying is pulverized, and is subsequent use.Pericarpium Citri Reticulatae adds 55% alcohol reflux 3 times, and alcohol adding amount is respectively 12 times, 10 times and 8 times, and each 1 hour, merge backflow, filter, decompression recycling ethanol is concentrated into relative density and is 1.10 clear paste.Mixing that Flos Lonicerae, Fructus Forsythiae are criticized, Rhizoma Anemones Altaicae three is distinguished the flavor of adds 5 times of water gagings soaked 1 hour, extracted volatile oil 5 hours with steam distillation, filtered, and distilled other device of rear solution and collected; Medicinal residues merge with seven flavors such as remaining Semen Plantaginis, and decocte with water 1 time adds 12 times of water gagings at every turn, decocts 1 hour; Collecting decoction filters, and filtrating merges with above-mentioned aqueous solution; Be concentrated into the clear paste of relative density 1.10, merge above-mentioned clear paste, Semen Coicis extract adds an amount of dextrin and protein sugar; Mixing, spraying one step pelletize, subsequent use.The volatile oil of collecting adopts β-CD saturated water solution method enclose.(β-CD and volatile oil proportioning are 4g: 0.75ml), it is an amount of to add water, and heating makes dissolving, reduces to 45 ℃ to get β-CD.(oil: with dehydrated alcohol dilute, slowly inject 45 ℃ β-CD solution, constant temperature stir 2 hour, put cold, put refrigerator (10 ℃ below) vacuum drying, pulverize, sieve, be added in above-mentioned granule, mixing promptly get in 1: 3 by ratio ethanol) for volatile oil.
Embodiment 12
Semen Coicis adds 7 times of amounts with 60% ethanol extraction 2 times at every turn, refluxes 2 hours, filter, and merging filtrate, decompression recycling ethanol, low-temperature vacuum drying is pulverized, and is subsequent use.Pericarpium Citri Reticulatae adds 60% alcohol reflux 3 times, and alcohol adding amount is respectively 12 times, 10 times and 8 times, and each 1 hour, merge backflow, filter, decompression recycling ethanol is concentrated into relative density and is 1.20 clear paste.Flos Lonicerae, Fructus Forsythiae are criticized, Rhizoma Anemones Altaicae three flavor mixes and adds 6 times of water gagings and soaked 2 hours, extract volatile oil 6 hours with steam distillation, filter, and distillation rear solution device is in addition collected, and seven flavors such as medicinal residues and residue Semen Plantaginis merge; Decocte with water 3 times adds 12 times of water gagings at every turn, decocts collecting decoction 1 hour; Filter, filtrating merges with above-mentioned aqueous solution, is concentrated into the clear paste of relative density 1.20, merges above-mentioned clear paste; Semen Coicis extract adds an amount of dextrin and protein sugar, mixing, and spraying one step pelletize, subsequent use.The volatile oil of collecting adopts β-CD saturated water solution method enclose.(β-CD and volatile oil proportioning are 4g: 0.75ml), it is an amount of to add water, and heating makes dissolving, reduces to 45 ℃ to get β-CD.(oil: with dehydrated alcohol dilute, slowly inject 45 ℃ β-CD solution, constant temperature stir 2 hour, put cold, put refrigerator (10 ℃ below) vacuum drying, pulverize, sieve, be added in above-mentioned granule, mixing promptly get in 1: 3 by ratio ethanol) for volatile oil.
Embodiment 13
Semen Coicis adds 8 times of amounts with 70% ethanol extraction 1 time at every turn, refluxes 1 hour, filter, and merging filtrate, decompression recycling ethanol, low-temperature vacuum drying is pulverized, and is subsequent use.Pericarpium Citri Reticulatae adds 60% alcohol reflux 3 times, and alcohol adding amount is respectively 12 times, 10 times and 8 times, and each 1 hour, merge backflow, filter, decompression recycling ethanol is concentrated into relative density and is 1.30 clear paste.Mixing that Flos Lonicerae, Fructus Forsythiae are criticized, Rhizoma Anemones Altaicae three is distinguished the flavor of adds 8 times of water gagings soaked 1 hour, extracted volatile oil 7 hours with steam distillation, filtered, and distilled other device of rear solution and collected; Medicinal residues merge with seven flavors such as remaining Semen Plantaginis, and decocte with water 1 time adds 12 times of water gagings at every turn, decocts 1 hour; Collecting decoction filters, and filtrating merges with above-mentioned aqueous solution; Be concentrated into the clear paste of relative density 1.20, merge above-mentioned clear paste, Semen Coicis extract adds an amount of dextrin and protein sugar; Mixing, spraying one step pelletize, subsequent use.The volatile oil of collecting adopts β-CD saturated water solution method enclose.(β-CD and volatile oil proportioning are 4g: 0.75ml), it is an amount of to add water, and heating makes dissolving, reduces to 45 ℃ to get β-CD.(oil: with dehydrated alcohol dilute, slowly inject 45 ℃ β-CD solution, constant temperature stir 2 hour, put cold, put refrigerator (10 ℃ below) vacuum drying, pulverize, sieve, be added in above-mentioned granule, mixing promptly get in 1: 3 by ratio ethanol) for volatile oil.
Embodiment 14
Semen Coicis adds 6 times of amounts with 65% ethanol extraction 2 times at every turn, refluxes 2 hours, filter, and merging filtrate, decompression recycling ethanol, low-temperature vacuum drying is pulverized, and is subsequent use.Pericarpium Citri Reticulatae adds 65% alcohol reflux 3 times, and alcohol adding amount is respectively 12 times, 10 times and 8 times, and each 1 hour, merge backflow, filter, decompression recycling ethanol is concentrated into relative density and is 1.30 clear paste.Mixing that Flos Lonicerae, Fructus Forsythiae are criticized, Rhizoma Anemones Altaicae three is distinguished the flavor of adds 7 times of water gagings soaked 2 hours, extracted volatile oil 5 hours with steam distillation, filtered, and distilled other device of rear solution and collected; Medicinal residues merge with seven flavors such as remaining Semen Plantaginis, and decocte with water 2 times adds 12 times of water gagings at every turn, decocts 1 hour; Collecting decoction filters, and filtrating merges with above-mentioned aqueous solution; Be concentrated into the clear paste of relative density 1.20, merge above-mentioned clear paste, Semen Coicis extract adds an amount of dextrin and protein sugar; Mixing, spraying one step pelletize, subsequent use.The volatile oil of collecting adopts β-CD saturated water solution method enclose.(β-CD and volatile oil proportioning are 4g: 0.75ml), it is an amount of to add water, and heating makes dissolving, reduces to 45 ℃ to get β-CD.(oil: with dehydrated alcohol dilute, slowly inject 45 ℃ β-CD solution, constant temperature stir 2 hour, put cold, put refrigerator (10 ℃ below) vacuum drying, pulverize, sieve, be added in above-mentioned granule, mixing promptly get in 1: 3 by ratio ethanol) for volatile oil.
Embodiment 15
Semen Coicis adds 8 times of amounts with 70% ethanol extraction 3 times at every turn, refluxes 3 hours, filter, and merging filtrate, decompression recycling ethanol, low-temperature vacuum drying is pulverized, and is subsequent use.Pericarpium Citri Reticulatae adds 70% alcohol reflux 3 times, and alcohol adding amount is respectively 12 times, 10 times and 8 times, and each 1 hour, merge backflow, filter, decompression recycling ethanol is concentrated into relative density and is 1.20 clear paste.Mixing that Flos Lonicerae, Fructus Forsythiae are criticized, Rhizoma Anemones Altaicae three is distinguished the flavor of adds 2-8 times of water gaging soaked 2 hours, extracted volatile oil 2-7 hour with steam distillation, filtered, and distilled other device of rear solution and collected; Medicinal residues merge with seven flavors such as remaining Semen Plantaginis, and decocte with water 2 times adds 12 times of water gagings at every turn, decocts 1 hour; Collecting decoction filters, and filtrating merges with above-mentioned aqueous solution; Be concentrated into the clear paste of relative density 1.30, merge above-mentioned clear paste, Semen Coicis extract adds an amount of dextrin and protein sugar; Mixing, spraying one step pelletize, subsequent use.The volatile oil of collecting adopts β-CD saturated water solution method enclose.(β-CD and volatile oil proportioning are 4g: 0.75ml), it is an amount of to add water, and heating makes dissolving, reduces to 45 ℃ to get β-CD.(oil: with dehydrated alcohol dilute, slowly inject 45 ℃ β-CD solution, constant temperature stir 2 hour, put cold, put refrigerator (10 ℃ below) vacuum drying, pulverize, sieve, be added in above-mentioned granule, mixing promptly get in 1: 3 by ratio ethanol) for volatile oil.
Embodiment 16
Semen Coicis adds 7 times of amounts with 75% ethanol extraction 2 times at every turn, refluxes 2 hours, filter, and merging filtrate, decompression recycling ethanol, low-temperature vacuum drying is pulverized, and is subsequent use.Pericarpium Citri Reticulatae adds 75% alcohol reflux 3 times, and alcohol adding amount is respectively 12 times, 10 times and 8 times, and each 1 hour, merge backflow, filter, decompression recycling ethanol is concentrated into relative density and is 1.10 clear paste.Mixing that Flos Lonicerae, Fructus Forsythiae are criticized, Rhizoma Anemones Altaicae three is distinguished the flavor of adds 5 times of water gagings soaked 2 hours, extracted volatile oil 6 hours with steam distillation, filtered, and distilled other device of rear solution and collected; Medicinal residues merge with seven flavors such as remaining Semen Plantaginis, and decocte with water 2 times adds 12 times of water gagings at every turn, decocts 1 hour; Collecting decoction filters, and filtrating merges with above-mentioned aqueous solution; Be concentrated into the clear paste of relative density 1.30, merge above-mentioned clear paste, Semen Coicis extract adds an amount of dextrin and protein sugar; Mixing, spraying one step pelletize, subsequent use.The volatile oil of collecting adopts β-CD saturated water solution method enclose.(β-CD and volatile oil proportioning are 4g: 0.75ml), it is an amount of to add water, and heating makes dissolving, reduces to 45 ℃ to get β-CD.(oil: with dehydrated alcohol dilute, slowly inject 45 ℃ β-CD solution, constant temperature stir 2 hour, put cold, put refrigerator (10 ℃ below) vacuum drying, pulverize, sieve, be added in above-mentioned granule, mixing promptly get in 1: 3 by ratio ethanol) for volatile oil.
Embodiment 17
Semen Coicis adds 4 times of amounts with 80% ethanol extraction 1 time at every turn, refluxes 2 hours, filter, and merging filtrate, decompression recycling ethanol, low-temperature vacuum drying is pulverized, and is subsequent use.Pericarpium Citri Reticulatae adds 80% alcohol reflux 3 times, and alcohol adding amount is respectively 12 times, 10 times and 8 times, and each 1 hour, merge backflow, filter, decompression recycling ethanol is concentrated into relative density and is 1.10~1.20 clear paste.Mixing that Flos Lonicerae, Fructus Forsythiae are criticized, Rhizoma Anemones Altaicae three is distinguished the flavor of adds 5 times of water gagings soaked 1 hour, extracted volatile oil 2 hours with steam distillation, filtered, and distilled other device of rear solution and collected; Medicinal residues merge with seven flavors such as remaining Semen Plantaginis, and decocte with water 1-3 time adds 12 times of water gagings at every turn, decocts 1 hour; Collecting decoction filters, and filtrating merges with above-mentioned aqueous solution; Be concentrated into the clear paste of relative density 1.10~1.20, merge above-mentioned clear paste, Semen Coicis extract adds an amount of dextrin and protein sugar; Mixing, spraying one step pelletize, subsequent use.The volatile oil of collecting adopts β-CD saturated water solution method enclose.(β-CD and volatile oil proportioning are 4g: 0.75ml), it is an amount of to add water, and heating makes dissolving, reduces to 45 ℃ to get β-CD.(oil: with dehydrated alcohol dilute, slowly inject 45 ℃ β-CD solution, constant temperature stir 2 hour, put cold, put refrigerator (10 ℃ below) vacuum drying, pulverize, sieve, be added in above-mentioned granule, mixing promptly get in 1: 3 by ratio ethanol) for volatile oil.
Embodiment 18
Semen Coicis adds 7 times of amounts with 85% ethanol extraction 2 times at every turn, refluxes 3 hours, filter, and merging filtrate, decompression recycling ethanol, low-temperature vacuum drying is pulverized, and is subsequent use.Pericarpium Citri Reticulatae adds 85% alcohol reflux 3 times, and alcohol adding amount is respectively 12 times, 10 times and 8 times, and each 1 hour, merge backflow, filter, decompression recycling ethanol is concentrated into relative density and is 1.20~1.30 clear paste.Mixing that Flos Lonicerae, Fructus Forsythiae are criticized, Rhizoma Anemones Altaicae three is distinguished the flavor of adds 6 times of water gagings soaked 2 hours, extracted volatile oil 2-7 hour with steam distillation, filtered, and distilled other device of rear solution and collected; Medicinal residues merge with seven flavors such as remaining Semen Plantaginis, and decocte with water 3 times adds 12 times of water gagings at every turn, decocts 1 hour; Collecting decoction filters, and filtrating merges with above-mentioned aqueous solution; Be concentrated into the clear paste of relative density 1.20~1.30, merge above-mentioned clear paste, Semen Coicis extract adds an amount of dextrin and protein sugar; Mixing, spraying one step pelletize, subsequent use.The volatile oil of collecting adopts β-CD saturated water solution method enclose.(β-CD and volatile oil proportioning are 4g: 0.75ml), it is an amount of to add water, and heating makes dissolving, reduces to 45 ℃ to get β-CD.(oil: with dehydrated alcohol dilute, slowly inject 45 ℃ β-CD solution, constant temperature stir 2 hour, put cold, put refrigerator (10 ℃ below) vacuum drying, pulverize, sieve, be added in above-mentioned granule, mixing promptly get in 1: 3 by ratio ethanol) for volatile oil.
Embodiment 19
Semen Coicis adds 8 times of amounts with 90% ethanol extraction 2 times at every turn, refluxes 3 hours, filter, and merging filtrate, decompression recycling ethanol, low-temperature vacuum drying is pulverized, and is subsequent use.Pericarpium Citri Reticulatae adds 90% alcohol reflux 3 times, and alcohol adding amount is respectively 12 times, 10 times and 8 times, and each 1 hour, merge backflow, filter, decompression recycling ethanol is concentrated into relative density and is 1.10~1.20 clear paste.Mixing that Flos Lonicerae, Fructus Forsythiae are criticized, Rhizoma Anemones Altaicae three is distinguished the flavor of adds 7 times of water gagings soaked 2 hours, extracted volatile oil 6 hours with steam distillation, filtered, and distilled other device of rear solution and collected; Medicinal residues merge with seven flavors such as remaining Semen Plantaginis, and decocte with water 2 times adds 12 times of water gagings at every turn, decocts 1 hour; Collecting decoction filters, and filtrating merges with above-mentioned aqueous solution; Be concentrated into the clear paste of relative density 1.10~1.20, merge above-mentioned clear paste, Semen Coicis extract adds an amount of dextrin and protein sugar; Mixing, spraying one step pelletize, subsequent use.The volatile oil of collecting adopts β-CD saturated water solution method enclose.(β-CD and volatile oil proportioning are 4g: 0.75ml), it is an amount of to add water, and heating makes dissolving, reduces to 45 ℃ to get β-CD.(oil: with dehydrated alcohol dilute, slowly inject 45 ℃ β-CD solution, constant temperature stir 2 hour, put cold, put refrigerator (10 ℃ below) vacuum drying, pulverize, sieve, be added in above-mentioned granule, mixing promptly get in 1: 3 by ratio ethanol) for volatile oil.
Embodiment 20
Semen Coicis adds 5 times of amounts with 50% ethanol extraction 1 time at every turn, refluxes 2 hours, filter, and merging filtrate, decompression recycling ethanol, low-temperature vacuum drying is pulverized, and is subsequent use.Pericarpium Citri Reticulatae adds 60% alcohol reflux 3 times, and alcohol adding amount is respectively 12 times, 10 times and 8 times, and each 1 hour, merge backflow, filter, decompression recycling ethanol is concentrated into relative density and is 1.10~1.20 clear paste.Mixing that Flos Lonicerae, Fructus Forsythiae are criticized, Rhizoma Anemones Altaicae three is distinguished the flavor of adds 6 times of water gagings soaked 2 hours, extracted volatile oil 2-7 hour with steam distillation, filtered, and distilled other device of rear solution and collected; Medicinal residues merge with seven flavors such as remaining Semen Plantaginis, and decocte with water 2 times adds 12 times of water gagings at every turn, decocts 1 hour; Collecting decoction filters, and filtrating merges with above-mentioned aqueous solution; Be concentrated into the clear paste of relative density 1.10~1.20, merge above-mentioned clear paste, Semen Coicis extract adds an amount of dextrin and protein sugar; Mixing, spraying one step pelletize, subsequent use.The volatile oil of collecting adopts β-CD saturated water solution method enclose.(β-CD and volatile oil proportioning are 4g: 0.75ml), it is an amount of to add water, and heating makes dissolving, reduces to 45 ℃ to get β-CD.(oil: with dehydrated alcohol dilute, slowly inject 45 ℃ β-CD solution, constant temperature stir 2 hour, put cold, put refrigerator (10 ℃ below) vacuum drying, pulverize, sieve, be added in above-mentioned granule, mixing promptly get in 1: 3 by ratio ethanol) for volatile oil.
Embodiment 21
Semen Coicis adds 5 times of amounts with 75% ethanol extraction 3 times at every turn, refluxes 2 hours, filter, and merging filtrate, decompression recycling ethanol, low-temperature vacuum drying is pulverized, and is subsequent use.Pericarpium Citri Reticulatae adds 50% alcohol reflux 3 times, and alcohol adding amount is respectively 12 times, 10 times and 8 times, and each 1 hour, merge backflow, filter, decompression recycling ethanol is concentrated into relative density and is 1.10~1.20 clear paste.Mixing that Flos Lonicerae, Fructus Forsythiae are criticized, Rhizoma Anemones Altaicae three is distinguished the flavor of adds 5 times of water gagings soaked 1~2 hour, extracted volatile oil 2-7 hour with steam distillation, filtered, and distilled other device of rear solution and collected; Medicinal residues merge with seven flavors such as remaining Semen Plantaginis, and decocte with water 3 times adds 12 times of water gagings at every turn, decocts 1 hour; Collecting decoction filters, and filtrating merges with above-mentioned aqueous solution; Be concentrated into the clear paste of relative density 1.10~1.20, merge above-mentioned clear paste, Semen Coicis extract adds an amount of dextrin and protein sugar; Mixing, spraying one step pelletize, subsequent use.The volatile oil of collecting adopts β-CD saturated water solution method enclose.(β-CD and volatile oil proportioning are 4g: 0.75ml), it is an amount of to add water, and heating makes dissolving, reduces to 45 ℃ to get β-CD.(oil: with dehydrated alcohol dilute, slowly inject 45 ℃ β-CD solution, constant temperature stir 2 hour, put cold, put refrigerator (10 ℃ below) vacuum drying, pulverize, sieve, be added in above-mentioned granule, mixing promptly get in 1: 3 by ratio ethanol) for volatile oil.
Embodiment 22
Semen Coicis adds 6 times of amounts with 75% ethanol extraction 2 times at every turn, refluxes 2 hours, filter, and merging filtrate, decompression recycling ethanol, low-temperature vacuum drying is pulverized, and is subsequent use.Pericarpium Citri Reticulatae adds 50% alcohol reflux 3 times, and alcohol adding amount is respectively 12 times, 10 times and 8 times, and each 1 hour, merge backflow, filter, decompression recycling ethanol is concentrated into relative density and is 1.20~1.30 clear paste.Mixing that Flos Lonicerae, Fructus Forsythiae are criticized, Rhizoma Anemones Altaicae three is distinguished the flavor of adds 5 times of water gagings soaked 1~2 hour, extracted volatile oil 3 hours with steam distillation, filtered, and distilled other device of rear solution and collected; Medicinal residues merge with seven flavors such as remaining Semen Plantaginis, and decocte with water 3 times adds 12 times of water gagings at every turn, decocts 1 hour; Collecting decoction filters, and filtrating merges with above-mentioned aqueous solution; Be concentrated into the clear paste of relative density 1.20~1.30, merge above-mentioned clear paste, Semen Coicis extract adds an amount of dextrin and protein sugar; Mixing, spraying one step pelletize, subsequent use.The volatile oil of collecting adopts β-CD saturated water solution method enclose.(β-CD and volatile oil proportioning are 4g: 0.75ml), it is an amount of to add water, and heating makes dissolving, reduces to 45 ℃ to get β-CD.(oil: with dehydrated alcohol dilute, slowly inject 45 ℃ β-CD solution, constant temperature stir 2 hour, put cold, put refrigerator (10 ℃ below) vacuum drying, pulverize, sieve, be added in above-mentioned granule, mixing promptly get in 1: 3 by ratio ethanol) for volatile oil.
Embodiment 23
Semen Coicis adds 7 times of amounts with 70% ethanol extraction 3 times at every turn, refluxes 2 hours, filter, and merging filtrate, decompression recycling ethanol, low-temperature vacuum drying is pulverized, and is subsequent use.Pericarpium Citri Reticulatae adds 60% alcohol reflux 3 times, and alcohol adding amount is respectively 12 times, 10 times and 8 times, and each 1 hour, merge backflow, filter, decompression recycling ethanol is concentrated into relative density and is 1.10~1.20 clear paste.Mixing that Flos Lonicerae, Fructus Forsythiae are criticized, Rhizoma Anemones Altaicae three is distinguished the flavor of adds 6 times of water gagings soaked 1 hour, extracted volatile oil 4 hours with steam distillation, filtered, and distilled other device of rear solution and collected; Medicinal residues merge with seven flavors such as remaining Semen Plantaginis, and decocte with water 2 times adds 12 times of water gagings at every turn, decocts 1 hour; Collecting decoction filters, and filtrating merges with above-mentioned aqueous solution; Be concentrated into the clear paste of relative density 1.10~1.20, merge above-mentioned clear paste, Semen Coicis extract adds an amount of dextrin and protein sugar; Mixing, spraying one step pelletize, subsequent use.The volatile oil of collecting adopts β-CD saturated water solution method enclose.(β-CD and volatile oil proportioning are 4g: 0.75ml), it is an amount of to add water, and heating makes dissolving, reduces to 45 ℃ to get β-CD.(oil: with dehydrated alcohol dilute, slowly inject 45 ℃ β-CD solution, constant temperature stir 2 hour, put cold, put refrigerator (10 ℃ below) vacuum drying, pulverize, sieve, be added in above-mentioned granule, mixing promptly get in 1: 3 by ratio ethanol) for volatile oil.
Embodiment 24
Semen Coicis adds 5 times of amounts with 75% ethanol extraction 3 times at every turn, refluxes 3 hours, filter, and merging filtrate, decompression recycling ethanol, low-temperature vacuum drying is pulverized, and is subsequent use.Pericarpium Citri Reticulatae adds 50% alcohol reflux 3 times, and alcohol adding amount is respectively 12 times, 10 times and 8 times, and each 1 hour, merge backflow, filter, decompression recycling ethanol is concentrated into relative density and is 1.10~1.20 clear paste.Mixing that Flos Lonicerae, Fructus Forsythiae are criticized, Rhizoma Anemones Altaicae three is distinguished the flavor of adds 5 times of water gagings soaked 1~2 hour, extracted volatile oil 5 hours with steam distillation, filtered, and distilled other device of rear solution and collected; Medicinal residues merge with seven flavors such as remaining Semen Plantaginis, and decocte with water 3 times adds 12 times of water gagings at every turn, decocts 1 hour; Collecting decoction filters, and filtrating merges with above-mentioned aqueous solution; Be concentrated into the clear paste of relative density 1.10~1.20, merge above-mentioned clear paste, Semen Coicis extract adds an amount of dextrin and protein sugar; Mixing, spraying one step pelletize, subsequent use.The volatile oil of collecting adopts β-CD saturated water solution method enclose.(β-CD and volatile oil proportioning are 4g: 0.75ml), it is an amount of to add water, and heating makes dissolving, reduces to 45 ℃ to get β-CD.(oil: with dehydrated alcohol dilute, slowly inject 45 ℃ β-CD solution, constant temperature stir 2 hour, put cold, put refrigerator (10 ℃ below) vacuum drying, pulverize, sieve, be added in above-mentioned granule, mixing promptly get in 1: 3 by ratio ethanol) for volatile oil.
Embodiment 25
Semen Coicis adds 8 times of amounts with 60% ethanol extraction 2 times at every turn, refluxes 2 hours, filter, and merging filtrate, decompression recycling ethanol, low-temperature vacuum drying is pulverized, and is subsequent use.Pericarpium Citri Reticulatae adds 70% alcohol reflux 3 times, and alcohol adding amount is respectively 12 times, 10 times and 8 times, and each 1 hour, merge backflow, filter, decompression recycling ethanol is concentrated into relative density and is 1.20~1.30 clear paste.Mixing that Flos Lonicerae, Fructus Forsythiae are criticized, Rhizoma Anemones Altaicae three is distinguished the flavor of adds 6 times of water gagings soaked 1~2 hour, extracted volatile oil 4 hours with steam distillation, filtered, and distilled other device of rear solution and collected; Medicinal residues merge with seven flavors such as remaining Semen Plantaginis, and decocte with water 3 times adds 12 times of water gagings at every turn, decocts 1 hour; Collecting decoction filters, and filtrating merges with above-mentioned aqueous solution; Be concentrated into the clear paste of relative density 1.10~1.20, merge above-mentioned clear paste, Semen Coicis extract adds an amount of dextrin and protein sugar; Mixing, spraying one step pelletize, subsequent use.The volatile oil of collecting adopts β-CD saturated water solution method enclose.(β-CD and volatile oil proportioning are 4g: 0.75ml), it is an amount of to add water, and heating makes dissolving, reduces to 45 ℃ to get β-CD.(oil: with dehydrated alcohol dilute, slowly inject 45 ℃ β-CD solution, constant temperature stir 2 hour, put cold, put refrigerator (10 ℃ below) vacuum drying, pulverize, sieve, be added in above-mentioned granule, mixing promptly get in 1: 3 by ratio ethanol) for volatile oil.
Embodiment 25
Semen Coicis adds 9 times of amounts with 60% ethanol extraction 3 times at every turn, refluxes 1.5 hours, filter, and merging filtrate, decompression recycling ethanol, low-temperature vacuum drying is pulverized, and is subsequent use.Pericarpium Citri Reticulatae adds 60% alcohol reflux 3 times, and alcohol adding amount is respectively 12 times, 10 times and 8 times, and each 1 hour, merge backflow, filter, decompression recycling ethanol is concentrated into relative density and is 1.10~1.20 clear paste.Mixing that Flos Lonicerae, Fructus Forsythiae are criticized, Rhizoma Anemones Altaicae three is distinguished the flavor of adds 7 times of water gagings soaked 1~2 hour, extracted volatile oil 5 hours with steam distillation, filtered, and distilled other device of rear solution and collected; Medicinal residues merge with seven flavors such as remaining Semen Plantaginis, and decocte with water 3 times adds 12 times of water gagings at every turn, decocts 1 hour; Collecting decoction filters, and filtrating merges with above-mentioned aqueous solution; Be concentrated into the clear paste of relative density 1.10~1.20, merge above-mentioned clear paste, Semen Coicis extract adds an amount of dextrin and protein sugar; Mixing, spraying one step pelletize, subsequent use.The volatile oil of collecting adopts β-CD saturated water solution method enclose.(β-CD and volatile oil proportioning are 4g: 0.75ml), it is an amount of to add water, and heating makes dissolving, reduces to 45 ℃ to get β-CD.(oil: with dehydrated alcohol dilute, slowly inject 45 ℃ β-CD solution, constant temperature stir 2 hour, put cold, put refrigerator (10 ℃ below) vacuum drying, pulverize, sieve, be added in above-mentioned granule, mixing promptly get in 1: 3 by ratio ethanol) for volatile oil.