Scorching capsule of wild flower woman and preparation method thereof
Technical field
The invention belongs to Chinese medicine patent medicine and pharmaceutical field, particularly a kind of gynecological Chinese patent medicine and preparation method thereof.
Background technology
The Chinese patent medicine close with the present invention is the medicine that is applicable to gynaecopathias such as chronic adnexitis, pelvic inflammatory disease, vaginitis, cystitis, chronic appendicitis, urinary tract infection, and name is called FUYANKANG PIAN.This herbal pharmaceutical composition has Radix Paeoniae Rubra 60g, Rhizoma Smilacis Glabrae 100g, rhizoma sparganic (processed with vinegar) 60g, Fructus Toosendan (stir-fry) 60g, Rhizoma Curcumae (processed with vinegar) 60g, Rhizoma Corydalis (processed with vinegar) 60g, Semen Euryales (stir-fry) 100g, Radix Angelicae Sinensis 100g, Radix Sophorae Flavescentis 60g, Rhizoma Cyperi (processed with vinegar) 40g, Cortex Phellodendri 60g, Radix Salviae Miltiorrhizae 100g, Rhizoma Dioscoreae 120g.The FUYANKANG PIAN that makes with above-mentioned 13 flavor Chinese crude drug processing has blood circulation promoting and blood stasis dispelling, hard masses softening and resolving, heat-clearing and toxic substances removing, the function of anti-inflammatory analgesic.
The preparation method of FUYANKANG PIAN is that Rhizoma Curcumae, Rhizoma Dioscoreae powder are broken into coarse powder, sieve.All the other rhizoma sparganic etc. ten decoct with water three times simply, and 2 hours for the first time, second and third time each 1 hour, collecting decoction, filter, filtrate is condensed into thick paste, and with above-mentioned powder mixing, drying is ground into fine powder, make granule, put 60~90 ℃ of dryings, be pressed into 1000, sugar coating, promptly.
Summary of the invention
The technical problem to be solved in the present invention is, develops a kind of new drug that is used for the treatment of commonly encountered disease, and the effective ingredient of high efficiency extraction Chinese crude drug, selects suitable dosage form, the purpose of the gynecological's new drug that reach a kind of curative effect height of exploitation, has no side effect.
The scorching capsule of wild flower woman of the present invention is a crude drug with following Chinese crude drug, effective ingredient by crude drug or its extraction is formed, and crude drug is 1~3 part in 10 parts of Flos Loniceraes, 5~7 parts of Fructus Forsythiaes, 11~13 parts of the Radixs Astragali, 4~5 parts of Cortex Moutans, 5~7 parts of Radix Isatidis, 5~7 parts of Flos Chrysanthemi Indicis, 3~4 parts of Rhizoma Curcumae and a Radix Glycyrrhizae by the quality proportioning.
In the above-mentioned eight flavor Chinese crude drugs, Flos Lonicerae is the dry flower of caprifoliaceae plant Radix Ophiopogonis Lonicera japonica Thunb, Flos Lonicerae Lonicera hypoglauca Miq, Flos Lonicerae Lonicera confusa DC. or hair post Radix Ophiopogonis Lonicera dasystyla Rehd. or the flower that band is just opened.Fructus Forsythiae is the dry fruit of Oleaceae plant Fructus Forsythiae Forsythia suspensa (Thunb.) Vahl.Cortex Moutan is the dry root bark of ranunculaceae peony Paeonia suffruticosa Andr..The Radix Astragali is the dry root for leguminous plant Radix Astagali Astragalus membranaceus (Fisch) Bge.var.mongholicus (Bge) Hsiao or film folder Radix Astragali Astragalus membranaceus (Fisch.) Bge.Rhizoma Curcumae is the dry rhizome of zingiberaceous plant Rhizoma Curcumae Curcuma phaeocaulisVal. Guangxi zedoary Curcuma kwangsiensis S.G.Lee etC.F.Liang or RADIX CURCUMAE Curcuma wenyujin Y.H.chen et C.Ling.Radix Glycyrrhizae is glycyrrhizic legume Glycyrrhiza uraensis Fisch,, the dry root and rhizome of Glycyrrhiza inflata Bat. Glycyrrhizainflata Bat. or Glycyrrhiza glabra L. Glycyrrhiza glabra L..Radix Isatidis is the dry root of cruciferae isatis lsatis indigotica Fort.Flos Chrysanthemi Indici; This product is the dry capitulum of feverfew Herba Dendranthematis indici Chrysanthemun indicum L..
In the crude drug, Flos Lonicerae is sweet in flavor and cold in property, heat-clearing and toxic substances removing, and wind-heat dissipating occupies first of the heat-clearing and toxic substances removing, is the monarch drug in the prescription.Its effective ingredient is a chlorogenic acid, has resisting pathogenic microbes, antitoxin, antipyretic and anti-inflammatory and promotes the effect of peripheral blood leucocyte and abdominal inflammation sexual cell phagocytic function.The Fructus Forsythiae hardship is slightly cold, heat-clearing and toxic substances removing, dispersing swelling and dissipating binds has remarkable inhibitory action to multiple pathogen, and have antiinflammatory, analgesic, protect the liver, effect such as antiallergic, with the Flos Lonicerae mutual reinforcement between be usefulness, strengthen the power of antibacterial anti-inflammatory, be principal agent altogether.Flos Chrysanthemi Indici, Radix Isatidis are accessory drugs.Cortex Moutan, Rhizoma Curcumae, Radix Isatidis, the Radix Astragali are adjuvant drug altogether.Radix Glycyrrhizae is a messenger drug.All medicine compatibilities are played the merit of heat-clearing and toxic substances removing, blood circulation promoting and blood stasis dispelling, removing food stagnancy eliminating stagnation altogether.
Thus, the scorching capsule of wild flower woman of the present invention has the function of heat-clearing and toxic substances removing, blood circulation promoting and blood stasis dispelling, anti-inflammatory analgetic.Cure mainly that pruritus, pelvic lump, profuse leukorrhea yellow skin have diseases such as abnormal flavour in lower abdomen pain that female pelvic inflammation, adnexitis, endometritis, cervicitis etc. cause, the moon.
Effective ingredient in the scorching capsule of wild flower woman serves as to investigate index with chlorogenic acid contained in the Flos Lonicerae, if chlorogenic acid content reaches the 3.84mg/ grain, then dosage is for take 3~4, every day 3 times at every turn.
The scorching capsular preparation method of wild flower woman of the present invention is, with 10 parts of Flos Loniceraes, 5~7 parts of Fructus Forsythiaes, 11~13 parts of the Radixs Astragali, 4~5 parts of Cortex Moutans, 5~7 parts of Radix Isatidis, 5~7 parts of Flos Chrysanthemi Indicis, 3~4 parts of Rhizoma Curcumae, Radix Glycyrrhizae is raw material for 1~3 part, through alcohol extraction, extract volatile oil, decocting boils and precipitate with ethanol (ethanol precipitation), the standby material process of producing pulverized, and makes product through batch mixing, packing again.
Said alcohol extraction is that 65~80% alcohol heating reflux that Flos Lonicerae adds 8~10 times of amounts are extracted 2~3 times, each 1~2 hour, filter, decompression filtrate recycling ethanol continues to be concentrated into the thick paste shape, drying under reduced pressure, Getrocknete Blumen cream is standby;
Said extraction volatile oil is that Rhizoma Curcumae coarse powder, Fructus Forsythiae and Flos Chrysanthemi Indici are put in the volatile oil extractor, and the water that adds 8~12 times of amounts was carried volatile oil 8~16 hours, and the volatile oil of carrying obtains volatile oil clathrate compound with beta-cyclodextrin inclusion compound, and is standby; Water extract after filtration device is in addition stored standby; Medicinal residues are standby;
Said decocting boils and precipitate with ethanol, is the medicinal residues that the Radix Astragali, Radix Isatidis, Radix Glycyrrhizae and extraction volatile oil are obtained, and the decocting that adds 6~10 times boils 2~3 times, each 1.5~3 hours, filter while hot, collecting decoction and carry volatile oil after the water extract, add ethanol after concentrating and make and contain the alcohol amount and reach 60~70%, placed 20~28 hours, filter, filtrate recycling ethanol is concentrated into the thick paste shape, drying under reduced pressure, it is standby to get the dried cream of precipitate with ethanol;
Said pulverizing is that Cortex Moutan is pulverized, and is standby;
Said batch mixing is, the dried cream that Getrocknete Blumen cream and precipitate with ethanol are obtained together is ground into fine powder, adds Cortex Moutan fine powder and volatile oil clathrate compound again, mixing, and sieving obtains product;
Said packing is that product is encapsulated.
Above-mentioned extraction volatile oil can adopt polishing, uses beta-cyclodextrin inclusion compound, volatile oil: beta-schardinger dextrin-is 1: 4~1: 6, and the enclose temperature is 40~50 ℃, and the enclose time is 0.75~1 hour.
Above-mentioned decocting boil and the precipitate with ethanol process in, the decocting liquid that is combined and carry volatile oil after the water extract concentrate, can be concentrated into that relative density is 1.05~1.20 under 60 ℃ of conditions of temperature.
Method of the present invention is that each processing step has all adopted preferred version through the research screening.Such as, relatively Flos Lonicerae alcohol extraction and water carry active ingredient chlorogenic acid content have remarkable different, alcohol extraction average out to 29.4mg/g, water is carried average out to 19.7mg/g, so the method for Flos Lonicerae employing alcohol extraction effective ingredient.For another example, Rhizoma Curcumae, Fructus Forsythiae, Flos Chrysanthemi Indici all mainly contain volatile ingredient, are one of effective ingredient in the prescription, so need to pulverize reflux, extract, volatile oil; For fear of loss of active ingredients, medicinal liquid and the medicinal residues carried behind the oil should be used as medicine with common decoction of other medical material.For another example, mainly contain the Saponin constituents in the Radix Astragali, soluble in water, so adopt decocting, composition is complicated in the Radix Isatidis, and it is all soluble in water mainly to contain compositions such as indigo, indirubin, several amino acids class, so the employing decocting boils; Anti-inflammatory component is a glycyrrhizin in the Radix Glycyrrhizae, and it is very easily water-soluble, so adopt decocting to boil.For the dose that reduces capsule with draw moistly, on the basis that decocting boils, carry out ethanol precipitation, to remove some polysaccharides and stickum, reduce the paste volume and the viscosity of extractum, so the employing decocting boils ethanol precipitation.For another example, the main component of Cortex Moutan is a paeonol, and it is volatile at low temperatures, and its pulverizing is used as medicine, and has both overcome the loss of active ingredients problem, has saved adjuvant again, has avoided moisture absorption phenomenon.For another example, the selection of dosage form considers that the decoction consumption is big, decoct the shortcoming of inconvenience, covers the bad smell of medicine again, just selects capsule.The scorching capsular preparation method of wild flower woman of the present invention is scientific and reasonable, process stabilizing, and the yield rate height can reach curative effect preferably with less dosage, can ensure drug quality and make things convenient for patient's medication.
The product that adopts crude drug prescription of the present invention and pharmaceutical methods to obtain is an initiative Chinese medicine patent medicine product.The pharmacological results shows: the scorching capsule of wild flower woman can suppress the rat uterus inflammation due to the rat paw edema and plastic hoop due to dimethylbenzene induced mice ear swelling, the carrageenin; Reduce the acetic acid induced mice and turn round the body number of times, prolong the mice hot plate pain threshold time; Exothermic reaction to the microbial rat of yeast has the obvious suppression effect; Improve rat acute blood stasis model hemorheology index due to the epinephrine; Promote the clean up speed of mononuclear phagocyte, improve phagocytic function carbon granules in the blood; Rat there is relexation at the body uterus movement.Bacteriostatic test is the result show: the scorching capsule of wild flower woman has the obvious in-vitro bacteriostasis to ten kinds of antibacterials such as staphylococcus aureus, escherichia coli, micrococcus scarlatinaes, and staphylococcus aureus, micrococcus scarlatinae mice infected are had protective effect.Show that the scorching capsule of wild flower woman has the pharmacological action of aspects such as antiinflammatory, analgesia, analgesic, antibacterial, raise immunity and blood circulation promoting and blood stasis dispelling.
Adopt the maximum dosage-feeding mouse stomach to detect the scorching capsule acute toxicity of wild flower woman, the result: the mice behavioral activity is normal, and body weight gain is normal; Detect routine blood test, blood biochemistry index, no abnormal change illustrates that the scorching capsule toxicity of wild flower woman is very little.Detect the scorching capsule long term toxicity of wild flower woman to rat oral gavage, the result: rat body weight does not have obvious decline.Each internal organs structure of histopathologic examination is normal, and no degeneration necrosis changes, and each period, each internal organs histopathologic examination and matched group did not more all have significant difference.All other hematologys, blood biochemical learn index and matched group does not relatively have significant difference.In 2 weeks of drug withdrawal, every inspection there is no unusually.Illustrate that the scorching capsule long term administration toxicity of wild flower woman is very little.
The specific embodiment
1 one kinds of preferred proportioning raw materials of embodiment and pharmaceutical technology
Raw material and proportioning thereof:
Flos Lonicerae 350g Fructus Forsythiae 210g
Radix Astragali 420g Cortex Moutan 168g
Radix Isatidis 210g Flos Chrysanthemi Indici 210g
Rhizoma Curcumae 126g Radix Glycyrrhizae 70g
Method for making: above eight flavor medicines, Cortex Moutan is ground into fine powder, and is standby; Flos Lonicerae adds ten times of amount 70% ethanol, heating and refluxing extraction 3 times, and each 1 hour, filter, decompression filtrate recycling ethanol continues to be concentrated into the thick paste shape, drying under reduced pressure to there not being the alcohol flavor; Rhizoma Curcumae, Flos Chrysanthemi Indici, Fructus Forsythiae three flavor medical materials, wherein Rhizoma Curcumae is ground into coarse powder, put in the volatile oil extractor, add ten times of water gagings and carry volatile oil, the time is 14 hours, institute's volatile oil of carrying adopts polishing, use beta-cyclodextrin inclusion compound, oil: beta-schardinger dextrin-is 1: 4, and the enclose temperature is 40 ℃, the enclose time is 1 hour, and is standby; Water extract device is in addition stored, and the medicinal residues and the Radix Astragali, Radix Isatidis, Radix Glycyrrhizae add the octuple water gaging, decoct twice, each 2 hours, filter while hot, collecting decoction and carry volatile oil after the water extract, being concentrated into relative density is 1.10 (60 ℃), adds ethanol and makes and contain alcohol amount and reach 60%, places 24 hours, filter, filtrate recycling ethanol is concentrated into the thick paste shape, drying under reduced pressure to there not being the alcohol flavor; Together be ground into fine powder with Getrocknete Blumen cream and add Cortex Moutan fine powder, volatile oil clathrate compound, mixing is crossed 60 mesh sieves, encapsulatedly makes 1000.
After testing, chlorogenic acid content 4.93mg/ grain.
The consumption of pressing the present embodiment crude drug calculates, and each crude drug changes in 35g, the therapeutic effect of product is not had too big influence, as long as Flos Lonicerae and Fructus Forsythiae do not reduce simultaneously.
The selection of the preferred plan of embodiment 2 alcohol extraction Flos Loniceraes
In order to investigate the condition of alcohol extraction process comprehensively, concentration of alcohol (60%, 70%, 80%), ethanol consumption (8,10,12 times of amounts of Flos Lonicerae), extraction time (1,1.5,2 hour), extraction time (1,2,3 time), as the investigation factor, three levels that each factor is chosen in the bracket are arranged orthogonal test, are performance assessment criteria with chlorogenic acid contents in the Flos Lonicerae.Several groups of data see Table 1 preferably.
Table 1
Sequence number | Concentration of alcohol | The ethanol consumption | Extraction time | Extraction time | Chlorogenic acid content |
??1 | ???70% | 8 times | 1.5 hour | ????3 | ?23.412mg/g |
??2 | ???70% | 12 times | 1.0 hour | ????2 | ?24.823mg/g |
??3 | ???80% | 8 times | 2.0 hour | ????2 | ?23.167mg/g |
??4 | ???80% | 10 times | 1.0 hour | ????3 | ?25.078mg/g |
Analysis of experiments as can be known, concentration of alcohol, extraction time are bigger to the effective ingredient influence of extracting Flos Lonicerae, concentration of alcohol is 60%, extraction time is 1, effect is relatively poor; So Flos Lonicerae alcohol extraction suitable process conditions is: 65~80% alcohol heating reflux that add 8~10 times of amounts extract each 1~2 hour 2~3 times.
Determining of 3 volatile oil extraction times of embodiment
Since all contain the volatile oil composition in Rhizoma Curcumae, Fructus Forsythiae, the Flos Chrysanthemi Indici, thus volatile oil will be extracted earlier, in order to avoid loss of effective components.
Test method: get Fructus Forsythiae 300g, Flos Chrysanthemi Indici 300g, Rhizoma Curcumae 180g, amount of water is 10 times of medical material amounts, heating and refluxing extraction volatile oil, the relation of investigation volatile oil extraction time and oil pump capacity.The results are shown in Table 2.
Table 2.
Extraction time (h) 468 10 12 14 16
Oil pump capacity (ml) 7.5 8.6 9.3 9.7 9.9 10 10
As can be seen from Table 2, oil pump capacity just no longer increased later on from 14 hours, so the extraction time of volatile oil is chosen to be 8~16 hours, preferred 12~14 hours.
Embodiment 4 inclusion essential oil Selection of technological conditions
For investigate the condition of inclusion essential oil technology comprehensively, oily: beta-schardinger dextrin-(1: 4,1: 6,1: 8), enclose time (0.5 hour, 0.75 hour, 1.0 hours), enclose temperature (40 ℃, 50 ℃, 60 ℃) are as the influence factor, each factor selects three levels in the bracket to arrange orthogonal test, is performance assessment criteria with the volatile oil utilization rate.Reasonable several groups of data see Table 3.
Table 3
Sequence number | Oil: beta-schardinger dextrin- | The enclose time | The enclose temperature | The volatile oil utilization rate |
??1 | ?????1∶4 | 0.50 hour | ???40℃ | ????78.3% |
??2 | ?????1∶4 | 0.75 hour | ???50℃ | ????71.7% |
??3 | ?????1∶4 | 1.00 hour | ???60℃ | ????68.3% |
??4 | ?????1∶6 | 1.00 hour | ???40℃ | ????73.3% |
??5 | ?????1∶8 | 0.75 hour | ???40℃ | ????70.0% |
Analysis of experiments shows that oil has appreciable impact with beta-schardinger dextrin-ratio and enclose temperature to the volatile oil utilization rate.In the test, what effect was relatively poor is oil: the combination of beta-schardinger dextrin-=1: 8,0.50 hour enclose time, 60 ℃ of enclose temperature, the volatile oil utilization rate is 60.0%.As can be seen from Table 3, should select oil in each factor preferably in effect: beta-schardinger dextrin-is 1: 4~1: 6, and the enclose temperature is 40~50 ℃, 0.75~1.0 hour enclose time.Optimum selection is oil: beta-schardinger dextrin-is 1: 4, and the enclose temperature is 40 ℃, 1 hour enclose time.
The selection of embodiment 5 extraction process by water
Test is carried out raw material dose 267g.Wherein Radix Astragali 90g, Fructus Forsythiae 45g, Flos Chrysanthemi Indici 45g, Radix Isatidis 45g, Radix Glycyrrhizae 15g, Rhizoma Curcumae 27g.Amount of water (raw material dose 8 times, 10 times, 12 times), extraction time (1 hour, 1.5 hours, 2 hours), extraction time (1 time, 2 times, 3 times) as the influence factor, each factor selects three levels in the bracket to arrange orthogonal tests, is performance assessment criteria with the content of astragaloside in the Radix Astragali.Reasonable several groups of data see Table 4.
Table 4
Sequence number | Amount of water | Extraction time | Extraction time | Astragaloside content |
??1 | 8 times | 1.5 hour | 2 times | ??156.5μg/g |
??2 | 8 times | 2 hours | 3 times | ??147.8μg/g |
??3 | 10 times | 1 hour | 2 times | ??139.9μg/g |
??4 | 12 times | 2 hours | 2 times | ??139.1μg/g |
In the test, effect is relatively poor is that amount of water is that 12 times of the raw material dose, extraction time are that 1.5 hours, extraction time are one group of process conditions of 1 time, and the content of astragaloside is 72.2 μ g/g.Analysis of experiments shows that amount of water and extraction time have a significant effect to the content of astragaloside.From table 4 also as can be seen the optimum condition of extraction process by water be that amount of water is that 8~10 times of the raw material dose, extraction time are that 1~2 hour, extraction time are 2~3 times; Best extraction process by water condition is that amount of water is that 8 times of the raw material dose, extraction time are that 2 hours, extraction time are 2 times.
The selection of embodiment 6 alcohol precipitation processes
For the dose that reduces capsule with draw moistly, on the basis that decocting boils, carry out ethanol precipitation, to remove some polysaccharides and stickum, reduce the paste volume and the viscosity of extractum, so on the basis that decocting boils, carried out ethanol precipitation.Now carrying out the precipitate with ethanol of variable concentrations, is that performance assessment criteria is tested preferably with the content of astragaloside in the Radix Astragali.Test data sees Table 5, and data are the content (μ g/g) of astragaloside in the table
Table 5
Sequence number | 60% the alcohol amount of containing | 70% the alcohol amount of containing | 80% the alcohol amount of containing |
???1 | ???????91.13 | ??????81.89 | ??????69.55 |
???2 | ???????89.03 | ??????86.64 | ??????71.18 |
The result shows that alcohol precipitation concentration is at 60~70% o'clock, and astragaloside content is higher, and optimum condition is to adopt 60% precipitate with ethanol behind the decocting.
The investigation of embodiment 7 preparations shaping technologies
The scorching capsule of wild flower woman of the present invention is a hard capsule, does not need complicated moulding process, on the working foundation of finishing extraction, concentrating, pulverize, adopts the direct fill of medicated powder.Experimental results show that: all pulverize, do not need to add any adjuvant, place six months medicines and do not have moisture absorption phenomenon, good fluidity can obtain good finished product.So do not need to add any adjuvant.
The investigation of embodiment 8 technology stabilities
Press embodiment 1 prepared three batch samples, reserved sample observing is investigated several respects such as its outward appearance, character, discriminating, inspection, assay, microbial limits on schedule at ambient temperature.The result shows that three batch sample quality are all more stable.The stable preparation process of this preparation is described.