CN101940745B - Jinji blood stasis eliminating particles and preparation method thereof - Google Patents
Jinji blood stasis eliminating particles and preparation method thereof Download PDFInfo
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- CN101940745B CN101940745B CN2010102811525A CN201010281152A CN101940745B CN 101940745 B CN101940745 B CN 101940745B CN 2010102811525 A CN2010102811525 A CN 2010102811525A CN 201010281152 A CN201010281152 A CN 201010281152A CN 101940745 B CN101940745 B CN 101940745B
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Abstract
The invention discloses traditional Chinese medicine Jinji blood stasis eliminating particles for treating a chronic pelvic inflammatory disease and a preparation method thereof. The preparation method comprises the following steps of: taking 200g of honeysuckle, 200g of baical skullcap root, 150g of dandelion, 100g of Chinese violet, 150g of Chinese honeylocust spine, 150g of common peony root, 200g of suberect spatholobus stem, 100g of common burreed rhizome, 100g of szechuan lovage rhizome, 100g of nutgrass galingale rhizome (vinegar), 100g of corydalis tuber (vinegar) and 100g of cowherb seed (frying); extracting by adopting a carbon dioxide supercritical fluid extracting method; crushing an extract into ultrafine powder with the particle diameter of smaller than 50 microns (completely passing through a sieve in 300 meshes) by utilizing a jet mill; and preparing the particle from the ultrafine powder together with excipient dextrin and flavoring agent xylitol. The invention has the advantages of complete extraction of active components, high product purity, less taking dosage, stable quality, and the like, and meanwhile, the product does not contain sugar, can be taken by a diabetes mellitus patient and expands the range of applicative people of medicaments.
Description
One technical field
The present invention relates to the field of Chinese medicines, specifically, relate to a kind of Jinji blood stasis removing pellet of treating chronic pelvic inflammatory disease and preparation method thereof.
Two background technologies
Jinji blood stasis removing pellet is used for card and belongs to damp-heat accumulation; The treatment of qi stagnation and blood stasis type women's chronic pelvic inflammatory disease; But have deficiencies such as active ingredient extracts not exclusively, product purity is low, taking dose is big, as correctives, granule is prone to moisture absorption caking to product with sucrose simultaneously; Quality is unstable, has also limited diabetes and prohibits sugared personnel and take.
Three summary of the invention
For overcoming above-mentioned deficiency, the purpose of this invention is to provide that a kind of active ingredient extracts fully, product purity is high, taking dose is little, steady quality is suitable for diabetes and prohibit Jinji blood stasis removing pellet that sugared personnel take and preparation method thereof.
Jinji blood stasis removing pellet is through following method preparation:
Extracting honeysuckle 200g, Radix Scutellariae 200g, Herba Taraxaci 150g, Herba Violae 100g, Spina Gleditsiae 150g, Radix Paeoniae Rubra 150g, Caulis Spatholobi 200g, triangular 100g, Rhizoma Chuanxiong 100g, Rhizoma Cyperi (vinegar) 100g, Rhizoma Corydalis (vinegar) 100g, Semen Vaccariae (stir-fry) 100g; Be ground into coarse powder; The employing carbon dioxide supercritical extraction method is extracted, extracting pressure 20-50Mpa, extraction temperature 30-60 ℃; Separator pressure 5-10Mpa; Separator temperature 40-60 ℃, disengaging time 2-6 hour, carbon dioxide flow was 20-30L/H; Get extracting solution, drying adopts jet mill extract powder to be broken into the superfine powder of particle diameter＜50 micron; The excipient that adopts is a dextrin, and correctives is xylitol, preferably dextrin: xylitol 1: 3.
The Chinese crude drug that above-mentioned embodiment is mentioned is originated as follows:
Flos Lonicerae: be caprifoliaceae plant dry flower or the first flower of opening of band of Radix Ophiopogonis.Heat-clearing and toxic substances removing is arranged, the effect of wind-heat dissipating.
Radix Scutellariae: be the dry root of labiate Radix Scutellariae.Heat clearing and damp drying is arranged, the effect of eliminating fire and detoxication.
Herba Taraxaci: for feverfew Herba Taraxaci, alkali ground Herba Taraxaci or belong to the dry herbs of several plants together.Heat-clearing and toxic substances removing is arranged, dispersing swelling and dissipating binds, the effect of inducing diuresis for treating stranguria syndrome is used for jaundice due to damp-heat, the puckery pain of pyretic stranguria.
Viola: plants violet to violet dry grass.The effect that heat-clearing and toxic substances removing is arranged.
Spina Gleditsiae: be the dry Spina jujubae of leguminous plant Fructus Gleditsia.The detumescence poison holding is arranged, the effect of evacuation of pus.
Radix Paeoniae Rubra: be the dry root of ranunculaceae plant Radix Paeoniae or river Radix Paeoniae Rubra.Clearing away heat and cooling blood is arranged, the effect of eliminating stasis to stop pain,
Be used for maculae caused by violent heat pathogen, hematemesis and epistaxis, conjunctival congestion and swelling pain, hypochondriac pain due to stagnation of liverQI, amenorrhea dysmenorrhea, lump in the abdomen stomachache.
Caulis Spatholobi: be the dry rattan of leguminous plant spatholobus suberectus.Be used for menoxenia; Dysmenorrhea; Amenorrhea.
Triangular: as to be the dry tuber of Sparganiaceae plant rhizoma scirpi.The removing blood stasis circulation of qi promoting is arranged, removing food stagnancy analgesic effect.
Rhizoma Chuanxiong: be the dry rhizome of samphire Rhizoma Chuanxiong.Blood-activating and qi-promoting is arranged, the effect of wind-expelling pain-stopping.Be used for menoxenia, amenorrhea dysmenorrhea ， mass in the abdomen stomachache.
Rhizoma Cyperi (vinegar): be the process of preparing Chinese medicine processed goods of Rhizoma Cyperi.Promoting QI circulation for relieving depression are arranged, the effect of menstruction regulating and pain relieving.
Rhizoma Corydalis (vinegar): be the process of preparing Chinese medicine processed goods of Rhizoma Corydalis.Invigorate blood circulation promoting the circulation of QI, analgesic effect.
Semen Vaccariae (stir-fry): be the process of preparing Chinese medicine processed goods of Semen Vaccariae.The effect that promoting blood circulation to restore menstrual flow is arranged.
The used crude drug of Jinji blood stasis removing pellet all can be bought from common pharmacy and obtain, and its specification meets national medical standard.
Four specific embodiment
The following example only is used to explain the present invention, rather than limits the present invention by any way.
Specific embodiment 1 of the present invention
1. extracting honeysuckle 200g, Radix Scutellariae 200g, Herba Taraxaci 150g, Herba Violae 100g, Spina Gleditsiae 150g, Radix Paeoniae Rubra 150g, Caulis Spatholobi 200g, triangular 100g, Rhizoma Chuanxiong 100g, Rhizoma Cyperi (vinegar) 100g, Rhizoma Corydalis (vinegar) 100g, Semen Vaccariae (stir-fry) 100g are ground into 60 order coarse powder, adopt carbon dioxide supercritical extraction method to extract; Extracting pressure 20Mpa; 30 ℃ of extraction temperature, separator pressure 5Mpa, 40 ℃ of separator temperatures; Disengaging time 2 hours, carbon dioxide flow are 20L/H.
Extracting solution is dry 2., adopt jet mill extract powder to be broken into the superfine powder of particle diameter 47-15 micron (fully through 300 mesh sieves).
3. by dextrin: xylitol adds in superfine powder at 1: 3 processes granule.
Specific embodiment 2 of the present invention
1. extracting honeysuckle 200g, Radix Scutellariae 200g, Herba Taraxaci 150g, Herba Violae 100g, Spina Gleditsiae 150g, Radix Paeoniae Rubra 150g, Caulis Spatholobi 200g, triangular 100g, Rhizoma Chuanxiong 100g, Rhizoma Cyperi (vinegar) 100g, Rhizoma Corydalis (vinegar) 100g, Semen Vaccariae (stir-fry) 100g are ground into 60 order coarse powder, adopt carbon dioxide supercritical extraction method to extract; Extracting pressure 50Mpa; 60 ℃ of extraction temperature, separator pressure 10Mpa, 60 ℃ of separator temperatures; Disengaging time 6 hours, carbon dioxide flow are 30L/H.
Extracting solution is dry 2., adopt jet mill extract powder to be broken into the superfine powder of particle diameter 47-15 micron (fully through 300 mesh sieves).
3. by dextrin: xylitol adds in superfine powder at 1: 3 processes granule.
The most preferred specific embodiment 3 of the present invention
1. extracting honeysuckle 200g, Radix Scutellariae 200g, Herba Taraxaci 150g, Herba Violae 100g, Spina Gleditsiae 150g, Radix Paeoniae Rubra 150g, Caulis Spatholobi 200g, triangular 100g, Rhizoma Chuanxiong 100g, Rhizoma Cyperi (vinegar) 100g, Rhizoma Corydalis (vinegar) 100g, Semen Vaccariae (stir-fry) 100g are ground into 60 order coarse powder, adopt carbon dioxide supercritical extraction method to extract; Extracting pressure 40Mpa; 40 ℃ of extraction temperature, separator pressure 6Mpa, 50 ℃ of separator temperatures; Disengaging time 4 hours, carbon dioxide flow are 25L/H.
Extracting solution is dry 2., adopt jet mill extract powder to be broken into the superfine powder of particle diameter 47-15 micron (fully through 300 mesh sieves).
3. by dextrin: xylitol adds in superfine powder at 1: 3 processes granule.
(1) method of inspection of Jinji blood stasis removing pellet embodiment:
These article 2.5g is got in [discriminating] (1), adds water 50ml, puts hot bath and makes dissolving, and with n-butanol extraction 2 times, each 20ml merges n-butyl alcohol liquid, and water bath method, residue add 2ml methanol makes dissolving, as need testing solution.Other gets baicalin reference substance, chlorogenic acid reference substance, adds methanol respectively and processes the solution that every 1ml contains 0.1mg, as reference substance solution.According to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw each 2 μ l of above-mentioned three kinds of solution, put respectively on same polyamide film, be developing solvent with acetic acid, launch, take out, dry, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
(2) get the peoniflorin reference substance, add ethanol and process the solution that every 1ml contains 1mg, as reference substance solution.According to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw down need testing solution 10 μ l respectively of reference substance solution and discriminating (1), put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose; With chloroform-ethyl acetate-methanol-formic acid (40: 15: 10: 0.2) be developing solvent; Launch, take out, dry; Spray is with 5% vanillin sulfuric acid solution, and it is clear that hot blast blows to the speckle colour developing.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show identical bluish violet speckle.
(3) get these article 2.5g, porphyrize adds methanol 50ml supersound process 30 minutes, filters the filtrating evaporate to dryness; Residue adds water makes dissolving, adds ammonia solution and transfers to alkalescence, ether extraction 3 times, each 15ml; Merge extractive liquid,, evaporate to dryness, residue add methanol 1ml makes dissolving, as need testing solution.Other gets the tetrahydropalmatine reference substance, adds ethanol and processes the solution that every 1ml contains 1mg, as reference substance solution.According to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B) test, draw above-mentioned need testing solution 10 μ l, reference substance solution 1 μ l respectively, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose; With cyclohexane extraction-chloroform-methanol (10: 6: 1) is developing solvent; Launch, take out, dry; After putting in the iodine vapor the smoked several seconds, put under the ultra-violet lamp (365nm) and inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
(4) get these article 5g, add water 50ml, regulate pH value to 2 ~ 3 with dilute hydrochloric acid, hot bath makes dissolving, puts cold; With ether extraction 3 times, each 20ml merges ether solution, extracts 3 times with 2% sodium carbonate liquor, at every turn 15ml; Obtain alkali liquor, add hydrochloric acid and regulate pH value to 2 ~ 3, add diethyl ether again and extract 3 times, each 15ml; Merge ether solution, volatilize, residue adds methanol 1ml makes dissolving, as need testing solution.Other gets the ferulic acid reference substance and adds methanol and process the solution that every 1ml contains 1mg, as reference substance solution.Test according to thin layer chromatography (an appendix VI of Chinese Pharmacopoeia version in 2005 B); Draw each 5 μ l of above-mentioned two kinds of solution, put respectively in same be on the silica gel g thin-layer plate of adhesive with the sodium carboxymethyl cellulose, be developing solvent with benzene-glacial acetic acid-methanol (30: 1: 3); Launch; Take out, dry, under ultra-violet lamp (365nm), inspect.In the test sample chromatograph, with the corresponding position of reference substance chromatograph on, show the fluorescence speckle of same color.
[inspection] should meet each item regulation (an appendix I of Chinese Pharmacopoeia version in 2005 C) under the granule item.
[assay] measured according to HPLC (an appendix VI of Chinese Pharmacopoeia version in 2005 D).Chromatographic condition and system suitability test are filler with the octadecylsilane chemically bonded silica; With acetonitrile-0.4% phosphoric acid solution (13: 87) is mobile phase; The detection wavelength is 327nm.Number of theoretical plate calculates by the chlorogenic acid peak should be not less than 1000.
It is an amount of that the preparation precision of reference substance solution takes by weighing the chlorogenic acid reference substance, puts in the brown measuring bottle, adds 50% methanol and process the solution that every 1ml contains 40 μ g, promptly gets (preserving below 10 ℃).
These article are got in the preparation of need testing solution, porphyrize, and precision takes by weighing 2.5g, puts in the tool plug conical flask; Add 50% methanol 30ml, supersound extraction 25 minutes filters, and residue is with 50% methanol wash 3 times; Each 5ml filters, and merging filtrate quantitatively shifts in the 100ml measuring bottle; Add 50% methanol and be diluted to scale, shake up, promptly get.Accurate need testing solution and each the 10 μ l of reference substance solution of drawing of algoscopy inject chromatograph of liquid respectively, measure, and calculate, and promptly get.
These article contain chlorogenic acid (C for every bag
16H
18O
9) must not be less than 7.0mg.
The clinical observation on the therapeutic effect test of (two) two groups of Jinji blood stasis removing pellet treatment chronic pelvic inflammatory diseases
1. physical data
Statistics outpatient service and inpatient accept undergoing chronic pelvic inflammation 230 examples altogether for medical treatment, and the patient all has symptoms such as in various degree leucorrhea abnormal, adhesion.30～68 years old age wherein, 41 years old mean age.Adopting former Jinji blood stasis removing pellet is matched group.
2. efficacy assessment standard
Cure: clinical symptom disappearance, leucorrhea is normal, and adhesion disappears.Produce effects: clinical symptoms disappears basically, and leucorrhea is normal basically, and adhesion has significant improvement.Effectively: clinical symptoms takes a turn for the better, and leucorrhea and adhesion symptom have improvement to a certain degree.Invalid: clinical symptoms does not have improvement, and leucorrhea and adhesion symptom do not have improvement.
3. clinical observation result
The clinical observation on the therapeutic effect comparative test result of treatment undergoing chronic pelvic inflammation
Above-mentioned clinical observation on the therapeutic effect result shows, the Jinji blood stasis removing pellet of the present invention's preparation can more effectively improve patient's symptoms such as leucorrhea abnormal, adhesion under the same conditions with respect to former Jinji blood stasis removing pellet when treatment chronic pelvic inflammatory disease symptom.Simultaneously these article do not contain sugar, steady quality, and diabetes patient and prohibit sugared personnel and all can take has enlarged the suitable crowd of medicine.
The viewing test of (three) two groups of Jinji blood stasis removing pellet chlorogenic acid contents, dose
Adopting former Jinji blood stasis removing pellet is matched group.
Above-mentioned observation shows that the Jinji blood stasis removing pellet of the present invention's preparation has active component with respect to former Jinji blood stasis removing pellet and extracts complete, remarkable advantages such as taking dose is little, purity height when treatment chronic pelvic inflammatory disease symptom.
(4) two groups of Jinji blood stasis removing pellet stability and suitable crowd's comparing result
The above results shows that the Jinji blood stasis removing pellet of the present invention's preparation has advantages such as suitable crowd is wide, good stability with respect to former Jinji blood stasis removing pellet.
Claims (4)
1. Chinese medicine of treating women's chronic pelvic inflammation; It is characterized in that extracting honeysuckle 200g, Radix Scutellariae 200g, Herba Taraxaci 150g, Herba Violae 100g, Spina Gleditsiae 150g, Radix Paeoniae Rubra 150g, Caulis Spatholobi 200g, triangular 100g, Rhizoma Chuanxiong 100g, Rhizoma Cyperi (processed with vinegar) 100g, vinegar Rhizoma Corydalis 100g, Semen Vaccariae (parched) 100g; The employing carbon dioxide supercritical extraction method is extracted, extracting pressure 20-50Mpa wherein, extraction temperature 30-60 ℃; Separator pressure 5-10Mpa; Separator temperature 40-60 ℃, disengaging time 2-6 hour, carbon dioxide flow was 20-30L/H; Jet mill is broken into superfine powder with extract powder; Process Jinji blood stasis removing pellet with pharmaceutically acceptable excipient and correctives.
2. according to the said preparation method of Chinese medicine of claim 1; It is characterized in that adopting carbon dioxide supercritical extraction method to extract extracting pressure 20-50Mpa, extraction temperature 30-60 ℃; Separator pressure 5-10Mpa; Separator temperature 40-60 ℃, disengaging time 2-6 hour, carbon dioxide flow was 20-30L/H.
3. according to the said preparation method of Chinese medicine of claim 1, it is characterized in that adopting jet mill extract powder to be broken into the superfine powder of particle diameter＜50 micron.
4. according to the said preparation method of Chinese medicine of claim 1, it is characterized in that adopting dextrin is excipient, and xylitol is a correctives.
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| CN103432275B (en) * | 2013-08-30 | 2015-07-22 | 贵阳新天药业股份有限公司 | Sustained-release nano-capsules for improving endometrial receptivity and application thereof |
| CN107441150A (en) * | 2017-06-28 | 2017-12-08 | 江苏省徐州医药高等职业学校 | The technique of general flavone in a kind of spina gleditsiae using supercritical carbon dioxide extraction |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1891285A (en) * | 2005-07-08 | 2007-01-10 | 仁和（集团）发展有限公司 | Chinese medicine composition, and its preparing method and quality control method |
| CN101085299A (en) * | 2006-06-07 | 2007-12-12 | 朱齐超 | Traditional Chinese medicinal composition for treating female pelvic inflammation and its application |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1891285A (en) * | 2005-07-08 | 2007-01-10 | 仁和（集团）发展有限公司 | Chinese medicine composition, and its preparing method and quality control method |
| CN101085299A (en) * | 2006-06-07 | 2007-12-12 | 朱齐超 | Traditional Chinese medicinal composition for treating female pelvic inflammation and its application |
Non-Patent Citations (1)
| Title |
|---|
| 杨义芳.中药提取分离的组合与集成优化技术.《中药材》.2008,第31卷(第12期),1915-1921. * |
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