CN103446378A - Preparation method of traditional Chinese medicine effective part for treating endoxemia - Google Patents
Preparation method of traditional Chinese medicine effective part for treating endoxemia Download PDFInfo
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- CN103446378A CN103446378A CN2013104265238A CN201310426523A CN103446378A CN 103446378 A CN103446378 A CN 103446378A CN 2013104265238 A CN2013104265238 A CN 2013104265238A CN 201310426523 A CN201310426523 A CN 201310426523A CN 103446378 A CN103446378 A CN 103446378A
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Abstract
The invention relates to a preparation method of a traditional Chinese medicine effective part for treating endoxemia, belonging to the technical field of Chinese medicine production. The preparation method comprises the following steps of: crushing dry scirpus yagara ohw tubers, adding 85% ethanol-water solution three times amount of the material, soaking for 24 hours, then carrying out reflux extraction for 2 times, wherein each reflux extraction lasts for 2 hours, filtering, combining extracting solutions and concentrating; adding water, the volume of which is 1.5 times of the volume of the concentrated extracting solution, to the concentrated extracting solution, respectively extracting by using extracting solvents, the polarities of which are from small to large, thus obtaining extract liquor, then concentrating, passing through a normal phase column for chromatography, and eluting by using an elution solvent; drying the collected eluant so as to obtain the scirpus yagara ohw effective part. According to the preparation method, the collected extracting solvent in the extract liquor is ethyl acetate, and the eluant solvent at least comprises an elution solvent formed by petroleum ether and ethyl acetate in a volume ratio of 100: 1, 100: 10 or 100: 12. Pharmacology experiments prove that the scirpus yagara ohw effective part prepared by the method has very good anti-endoxemia effect.
Description
Technical field
The present invention relates to from Chinese medicine to extract preparation and the application of effective site, what relate to specifically to obtain from the cyperus iria L. rhizoma scirpi plant a kind ofly can treat effective site of endotoxemia and preparation method thereof.
Background technology
Endotoxin is present in gram negative bacteria (gram-negative bacteria, G
-antibacterial) in the cell wall of thalline, by antibacterial, disengaged during cell wall disintegrate after death, viable bacteria can also send out the bleb form endotoxin is disengaged, and its chemical composition is lipopolysaccharide (lipopolysaccharide, LPS), the lipoid A of lipopolysaccharide is LPS " virulence " center ".A small amount of endotoxin is to impelling the liver reticuloendothelial system to have the certain significance in state of activation, but when a large amount of endotoxins enters blood circulation, can discharge in a large number cytokine profiles by the excitating organism immunocyte, destroy the body inflammatory molecular balance, produce endotoxemia, thereby cause pathological reaction widely, as systemic inflammatory response syndrome (SIRS), multiple organ dysfunction syndrome (MODS), multiple organ dysfunction syndrome (MOF) etc.In recent years, much research shows that septic shock and the multi-functional infull syndrome of Secondary cases are the major causes of death of sepsis patient.In the past when control and treatment endotoxemia, often from the flora of the endotoxic gram negative bacteria of inhibition generation, breed and reduce the starting point that is absorbed as of intestinal endotoxin, as the stability by supplementing normal intestinal flora, maintenance intestinal mucosa reduces generation and the absorption of intestinal endotoxin.Above Therapeutic Method is often used antibiotic, but a large amount of antibiotic application there will be the drug resistance bacterium, and a large amount of endotoxins of simultaneously killed gram negative bacteria meeting sudden outburst cause the hyperfunction or endotoxin shock of endotoxemia.Therefore in large quantity research subsequently, some other drugs have been developed, as the quasi-grease A structure analog of direct anti-endotoxin; Have sterilization, in and antiendotoxin albumen and the polypeptide class of endotoxin, the effect of Immunosuppression cytoactive.Yet clinical research shows up to now, also do not have a kind of medicine of these types can significantly reduce endotoxemia patient's mortality rate.Cause the reaction of systemic inflammatorome for endotoxemia, the scholar had proposed the direction that many target drugs may be control and treatment endotoxemia in recent years.Chinese medicine has multiple target effect, to take control and the treatment of the endotoxemia that theory of Chinese medical science statement pathogenesis is " accumulate in pyretic toxicity, blood-stasis internal-depression ", has important value.
Cyperus iria L. rhizoma scirpi (Scirpus yagara Ohwi) is Cyperaceae Herba Scirpi triqueteris platymiscium, and its dry tuber was just used as Sparganium stoloniferum in the Tang Dynasty, was the kind that Rhizoma Sparganii is used the earliest.All there is distribution in the areas such as its northeast in China, Zhejiang, Jiangsu, Anhui.Cyperus iria L. rhizoma scirpi, property is flat, bitter in the mouth, enters liver, spleen channel, has removing blood stasis circulation of qi promoting, removing food stagnancy pain-relieving functions, multiplex in menoxenia, gathers the diseases such as caking, is clinical blood-activating and stasis-removing commonly used.From the cyperus iria L. rhizoma scirpi tuber, separated at present obtained flavonoid, Phenylpropanoid Glycosides class, diphenylethylene, 4 '-compound (Kang kun, et al.Nat Prod Res Dev, 2008,20:639-640,649 such as phenyl isocoumarin class, phenolic acids; Zhang Tiejun, etc. modern medicines and clinical, 2009,24 (1): 36-38; Cui Xiaodong, etc. Acta Pharmaceutica Sinica, 2012,47 (24): 1987-1989; Qiaoli Liang, et al.Fitoterapia, 2013,84 (1): 170-173).In recent years Chinese scholars find part diphenylethylene, 4 '-pharmacological action (Li Ou that phenyl isocoumarin class and phenolic acid compound have the aspects such as antiinflammatory, anti-HIV, et al.Biol.Pharm.Bull, 2003,26 (11): 1511-1516; Gu-xunYang, et al.Planta Med, 2005,71:569-571).So far, there is not yet the report that relevant cyperus iria L. rhizoma scirpi effective site has the treatment endotoxemia.
Summary of the invention
The preparation method that the purpose of this invention is to provide a kind of effective ingredient in Chinese for the treatment of endotoxemia.Preparation method technological operation of the present invention is simple, and stable performance, cyperus iria L. rhizoma scirpi plant effective site that pharmacologically active is good can be provided.
A kind of preparation method for the treatment of the effective ingredient in Chinese of endotoxemia comprises the following steps:
(1) extract: get the dry tuber of cyperus iria L. rhizoma scirpi, pulverize, spend the night with the extraction solvent soaking, then, with extracting the solvent heating and refluxing extraction, merge extractive liquid,, be evaporated to without the alcohol flavor.
(2) column chromatography: the concentrated solution of step (1) is added to 1.5 times of water and be diluted to suspension, more ascending extractant is extracted by polarity respectively, is extracted liquid, extract is after concentrated, and upper normal phase column chromatography carries out eluting with eluting solvent; Collect eluent, drying, obtain cyperus iria L. rhizoma scirpi effective site.
The described extraction solvent of above-mentioned steps (1) is ethanol water, and this extracts solvent and uses safety cheap; Its concentration is 70%～95%, and the ethanol water in this concentration range is better to the permeability of plant tissue, is applicable to very much the extraction of the tubers medical materials such as cyperus iria L. rhizoma scirpi, thereby can obtain fully the active component of cyperus iria L. rhizoma scirpi effective site.
Above-mentioned steps (1) adds the extraction solvent of 3～4 times of weight that are equivalent to medical material at every turn, and 90 ℃～100 ℃ heating and refluxing extraction, each extraction time is 2～3h, extracts 2～3 times.
The described extractant of above-mentioned steps (2) at least comprises ethyl acetate.
The described normal phase column chromatography of above-mentioned steps (2) is silica gel column chromatography, and silica gel order number is the 100-200 order, the eluting solvent that the petroleum ether that it is 100:1,100:10,100:12 that eluting solvent at least comprises by volume ratio and ethyl acetate form.
Eluting solvent has stricter requirement, and to volume ratio also restriction to some extent, this eluting solvent eluting power is medium, thereby can concentrate, obtains stable performance, cyperus iria L. rhizoma scirpi effective site that pharmacologically active is good.When the eluting solvent polarity of selecting is too large, can access too much the material irrelevant with the institute pharmacologically active of wanting, thus the reduction effective site material concentration of integral body, on the contrary eluting solvent polarity is too little, just can not fully obtain desired effective site.
The extraction solvent that at every turn adds 3～4 times of weight that are equivalent to medical material, 90 ℃～100 ℃ heating extraction, each time of extracting is 2～3 hours, extracts 2～3 times.Under such extraction conditions, not only saved the use amount of medical material and extraction solvent, and can fully effective site in medical material have been extracted, improve extraction ratio.
The eluting solvent that the petroleum ether that it is 100:0,100:1,100:2,100:4,100:6,100:8,100:10,100:12 that eluting solvent used comprises by volume ratio and ethyl acetate form, and by the ascending gradient elution that carries out successively of polarity.Inspect the eluent after the eluting solvent eluting that the eluting solvent that the cyperus iria L. rhizoma scirpi effective site petroleum ether that to be arranged in by volume ratio be 100:1 and ethyl acetate form and the petroleum ether that is 100:10,100:12 by volume ratio and ethyl acetate form, three part eluents more than merging by thin layer chromatography (TLC).
Cyperus iria L. rhizoma scirpi effective site prepared by described preparation method, contain 4 '-phenyl isocoumarin class, diphenylethylene, the compound of phenolic acids.
Cyperus iria L. rhizoma scirpi effective site in the present invention can be made into any acceptable preparation on pharmaceutics, such as making oral Preparation: tablet, pill, capsule, granule, drop pill, oral liquid etc.; Be prepared into the rectally preparation: suppository etc.; Be prepared into the percutaneous drug delivery preparation: unguentum, Emulsion, patch etc.; Be prepared into injecting and administering preparations: intramuscular dose, intravenous injection etc.
Cyperus iria L. rhizoma scirpi effective site in the present invention acceptable carrier on pharmaceutics includes but not limited to: excipient, as starch and derivant, dextrin etc.; Disintegrating agent, as sodium carboxymethyl cellulose etc.; Lubricant, as magnesium stearate etc.; The sugar coating material, as sucrose, Pulvis Talci, gelatin, pigment etc.; Other are as buffer, saline etc.
Cyperus iria L. rhizoma scirpi effective site prepared by described preparation method shows that in the experimentation of endotoxemia mice cyperus iria L. rhizoma scirpi effective site of the present invention has the treating endotoxemia effect.In the experimentation of endotoxemia mice, 40 mices are divided into 4 groups at random, every group 10, be respectively matched group, model group, administration low dose group, administration high dose group, take each group mice survival rate is index, after modeling, observes and respectively organizes mice 7 days, the survival rate of last control group mice is 100%, model group is 0%, and the administration low dose group is 60%, and the administration high dose group is 70%.
Compared with prior art, the present invention has the following advantages: cyperus iria L. rhizoma scirpi effective site provided by the invention, physiologically active is strong, have quality controllable, dosage is little, the advantage such as easy to use, is different from thick, large, the black backwardness of Chinese medicine.
The present invention's cyperus iria L. rhizoma scirpi used has distribution on China northeast, the Inner Mongol, Zhejiang, Jiangsu and other places, and its ABUNDANT NATUREAL RESOURSES is cheap and easy to get; The Herba Scirpi triqueteris platymiscium is herbaceous plant, and regeneration capacity is strong, even carry out large-scale production, also can not cause resource exhaustion, also less to environmental effect; The preparation method of cyperus iria L. rhizoma scirpi effective site provided by the invention is simple to operate, and production cost is low, is applicable to suitability for industrialized production.
The accompanying drawing explanation
See Figure of description: cyperus iria L. rhizoma scirpi effective site high-efficient liquid phase chromatogram
The specific embodiment
Below by specific embodiment, content of the present invention is described in further detail, but these embodiment should never be understood to limitation of the present invention.Without departing from the idea case in the present invention described above, any change that the invention process is done, within all being included in the present invention for those skilled in the art.
The preparation of embodiment 1 treating endotoxemia effective site
(1) extract: get cyperus iria L. rhizoma scirpi dry tuber 20kg, pulverize, after soaking 1 day with the ethanol water of 3 times of amounts 85%, 90 ℃ of heating and refluxing extraction, extraction time is 2h at every turn, altogether extracts 2 times, merges extracting solution 2 times.
(2) column chromatography: the extracting solution that step (1) is obtained is evaporated to without the alcohol flavor, concentrated solution adds 1.5 times of water and is diluted to suspension, use respectively again petroleum ether, ethyl acetate, n-butanol extraction, the concentrated extractum 90.5g that to obtain of ethyl acetate extract extract merging.Ethyl acetate extract extractum is carried out to purification on normal-phase silica gel (100-200 order) column chromatography, then use respectively a plurality of different eluting solvents to carry out eluting, each eluting solvent all is comprised of petroleum ether and ethyl acetate, and the volume ratio of each eluting solvent PetroChina Company Limited. ether and ethyl acetate is respectively 100:0,100:1,100:2,100:4,100:6,100:8,100:10,100:12, and carry out successively from small to large gradient elution by polarity.Thin layer chromatography (TLC) is inspected the eluent that cyperus iria L. rhizoma scirpi effective site yellow green speckle and skin dark stain concentrate on respectively the eluting solvent that the volume ratio of the eluent of the eluting solvent that petroleum ether and ethyl acetate volume ratio are 100:1 and petroleum ether and ethyl acetate is 100:10,100:12, collect three part eluents, at 60 ℃ of concentrating under reduced pressure 30min, obtain cyperus iria L. rhizoma scirpi effective site 14.0g with Rotary Evaporators.
The weight reduction precision takes the cyperus iria L. rhizoma scirpi effective site 11.04mg of embodiment 1 preparation, adds the chromatograph methanol constant volume to the volumetric flask of 10ml, and the extractum solution after the standardize solution that takes a morsel is analyzed with Waters2996HPLC, and liquid phase chromatogram condition: flow velocity is 0.5ml/min; Uv absorption wavelength: 300nm; Eluent system is methanol-water; The mass fraction of methanol is 10%～100%; Elution time: 0～65min.Its high-efficient liquid phase chromatogram is shown in Figure of description.
Treating endotoxemia experiment in the body of embodiment 2 cyperus iria L. rhizoma scirpi effective sites
Experiment material
(1) preparation of experimental drug liquid: the weight reduction precision takes appropriate two parts of cyperus iria L. rhizoma scirpi effective site respectively, adds respectively appropriate 0.5%CMC-Na solution, is made into the medicinal liquid of low, high two concentration.
(2) experiment endotoxin: e. coli lipopolysaccharide (LPS, 055:B5, U.S. Sigma company).
(3) laboratory animal: the BALB/c female mice, purchased from Nanjing Qinglongshan Experimental Animal Center, the quality certification is: SOXK (Soviet Union) 009-0001, weight range: 18～22g.
Experimental technique
This experiment administering mode is gastric infusion, and modeling method is that lumbar injection endotoxin (15mg/kg) causes the endotoxemia model, and concrete experimental technique is as follows.Precision takes endotoxin, is made into the solution of 1.5mg/ml with PBS buffer solution.40 mices are divided into to 4 groups at random, every group 10, first group (matched group), 3d is to mouse stomach 0.5%CMC-Na solution 0.2ml/10g continuously, 2time/d, the 3rd day 1h after gavage for the first time, lumbar injection 0.1ml/10g PBS buffer solution, give mouse stomach 0.5%CMC-Na solution 0.2ml/10g again after 6h; Second group (model group), 3d is to mouse peritoneal injection 0.1ml/10g PBS buffer solution continuously, and 1time/d, after 3d lumbar injection PBS buffer solution 1h, to this group mouse peritoneal injection LPS solution (15mg/kg, 0.1ml/10g); The 3rd group (administration low dose group), 3d is to mouse stomach low dosage medicinal liquid, 2time/d continuously, the 3rd day 1h after gavage for the first time, lumbar injection 0.1ml/10g chamber injection LPS solution (15mg/kg, 0.1ml/10g), give mouse stomach low dosage medicinal liquid 1 time again after 6h; The 4th group (administration high dose group), 3d is to mouse stomach high dose medicinal liquid, 2time/d continuously, the 3rd day 1h after gavage for the first time, lumbar injection 0.1ml/10g chamber injection LPS solution (15mg/kg, 0.1ml/10g), give mouse stomach high dose medicinal liquid 1 time again after 6h.
Observation index and data processing method
After injection LPS solution, the survival rate of each group mice of take is index, observes and record 7d, calculates dead number and the survival rate of every group of mice, and experimental result sees attached list one.
The Antiendotoxin Effect result (survival rate) in the body of subordinate list one cyperus iria L. rhizoma scirpi effective site
Claims (7)
1. a preparation method for the treatment of the effective ingredient in Chinese of endotoxemia comprises the following steps:
(1) extract: get the dry tuber of cyperus iria L. rhizoma scirpi, pulverize, soak with ethanol water, extract, obtain extracting solution.
(2) column chromatography: the extracting solution that step (1) is obtained is concentrated, be dissolved in water, then by polarity, ascending extractant is extracted respectively, is extracted liquid.Extract is upper normal phase column after concentrated, with eluting solvent, carries out eluting.Collect eluent, drying, obtain cyperus iria L. rhizoma scirpi effective site.
Described extractant has ethyl acetate.
The eluting solvent that the petroleum ether that it is 100:1,100:10,100:12 that described eluting solvent at least comprises by volume ratio and ethyl acetate form.
2. the preparation method of cyperus iria L. rhizoma scirpi effective site according to claim 1, is characterized in that, in step (1), ethanol water used is 70%～95%.
3. the preparation method of cyperus iria L. rhizoma scirpi effective site according to claim 1, is characterized in that, in step (1), the extraction solvent that at every turn adds 3～4 times of weight that are equivalent to medical material, 90 ℃～100 ℃ heating and refluxing extraction, each extraction time is 2～3h, extracts 2～3 times.
4. the preparation method of cyperus iria L. rhizoma scirpi effective site according to claim 1, is characterized in that, described extractant comprises petroleum ether, ethyl acetate and n-butyl alcohol, during extraction, by the polarity size, uses successively the single solvent equal-volume to be extracted.
5. the preparation method of cyperus iria L. rhizoma scirpi effective site according to claim 1, is characterized in that, in step (2), described normal phase column filler used is 100～200 purpose column chromatography silica gels.
6. the preparation method of cyperus iria L. rhizoma scirpi effective site according to claim 1, it is characterized in that, the eluting solvent that the eluting solvent that the eluting solvent that the petroleum ether that described eluting solvent is at least 100:1 by volume ratio and ethyl acetate form, the petroleum ether that is 100:10 by volume ratio and ethyl acetate form, the petroleum ether that is 100:12 by volume ratio and ethyl acetate form, and by the ascending gradient elution that carries out of polarity.
7. prepare the application of cyperus iria L. rhizoma scirpi effective site in preparing the treating endotoxemia medicine according to the described preparation method of claim 1～6 any one.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105878872A (en) * | 2015-01-08 | 2016-08-24 | 南京中医药大学 | Applications of effective parts of common burreed rhizome in preparing medicines for treating cerebral hemorrhage |
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| CN101274050A (en) * | 2007-03-28 | 2008-10-01 | 复旦大学 | Application of rhizome of Common Burreed in preparation of medicament for curing virosis |
| CN102218058A (en) * | 2011-04-29 | 2011-10-19 | 南京中医药大学 | Application of sparstolenin B as TLR2 (Toll-like receptor 2)/TLR4 (Toll-like receptor 4) antagonist in pharmacy |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105878872A (en) * | 2015-01-08 | 2016-08-24 | 南京中医药大学 | Applications of effective parts of common burreed rhizome in preparing medicines for treating cerebral hemorrhage |
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Application publication date: 20131218 |