CN101066286A - Coastal glehnia root extract with function of antagonizing gastric ulcer and its prepn - Google Patents
Coastal glehnia root extract with function of antagonizing gastric ulcer and its prepn Download PDFInfo
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- CN101066286A CN101066286A CN 200710011592 CN200710011592A CN101066286A CN 101066286 A CN101066286 A CN 101066286A CN 200710011592 CN200710011592 CN 200710011592 CN 200710011592 A CN200710011592 A CN 200710011592A CN 101066286 A CN101066286 A CN 101066286A
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- radix glehniae
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Abstract
The present invention belongs to the field of medicine technology, and is especially Chinese medicinal material coastal glehnia root extract and its preparation process. The preparation process includes the main steps of water extraction, alcohol precipitation, macroporous resin adsorption, water washing and alcohol solution eluting. The extract contains three kinds of active component, including lignan glycoside, coumarin glycoside and cinepazid glycoside, and includes 21 kinds of compound, including glehlinoside A, bergaptol 5-O-beta-D-gentiobioside, etc. It has obvious effects of antagonizing gastro ulcer, resisting oxidation and relieving pain, and is used as material of medicine for treating gastric ulcer and chronic gastritis.
Description
Technical field
The present invention relates to medical technical field, relate to Chinese medicine Radix glehniae extract and preparation method thereof, the invention still further relates to the medical usage that Radix glehniae extract is used for anti-gastric-ulcer.
Background technology
Gastric ulcer is the digestive system common frdquently encountered disease, and sickness rate is in rising trend in recent years.Its pathophysiological process is comparatively complicated, summarize the attack factor of saying so to the destruction of gastric mucosa and defense factor to due to the dysequilibrium of the protective effect of gastric mucosa.Attack factor has gastric acid, pepsin, the anti-top intestinal fluid that flows, helicobacter pylori etc.; The protection factor comprises gastric mucosal barrier stomach function regulating mucus barrier.Gastric mucosal barrier not only refers to the protective effect of gastric epithelial, and has comprised gastric mucosal blood flow, the various gastric mucosal protection factor such as prostaglandin etc.; The gastric mucus barrier is a gastric mucus bicarbonate barrier.When any reason causes the attack factor reinforcement or the protection factor to weaken, all can cause gastric mucosa injury.In addition, find also that in recent years oxygen-derived free radicals combines lipid peroxide such as producing MDA with polyvalent unsaturated fatty acid, but failure line plastochondria and lysosome membrane cause cell death, form ulcer.Many Chinese medicines can effectively be removed oxygen-derived free radicals, suppress the lipid peroxidation in the gastric mucosa, thereby suppress ulcer.
At present, anti-ulcer medicament commonly used clinically still fails to solve the high problem of ulcer recurrence rate, and the untoward reaction problem exposes day by day.Market is urgent to novel anti medicine for ulcer demand efficient, low toxicity.In recent years, Chinese scholars has been carried out the experimentation of treatment by Chinese herbs gastric ulcer, demonstrate Chinese medicine in the advantage that strengthens aspects such as gastric mucosal defense ability, raising healing quality, minimizing recurrence and toxicity are low, therefore the mechanism of action of treatment by Chinese herbs gastric ulcer and the discussion on working substance basis more and more are subject to people's attention.
Radix Glehniae is nourishing lung and stomach deficiency of YIN Chinese medicine commonly used.Modern pharmacological research shows that Radix Glehniae and chemical constituent thereof have antioxidation, analgesia, and calmness, antibiotic, antifungal, restraint of tyrosinase, immunomodulating, and anticancer, many-sided effect such as mutation.Clinically, about the report of treatment syndrome of deficiency of stomach yin is mainly the compound decoction of Radix Glehniae and other drug compatibility, for treating the classics side of gastric abscess, evident in efficacy as decoction made from radix adenophorea, tuber of dwarf lilyturf and yin nourishing yiwei decoction.In addition, because the effect of its good curing syndrome of deficiency of stomach yin, the compound preparation and the health tea that contain Radix Glehniae have obtained multinomial national patent.The report of the relevant Radix Glehniae of Shang Weijian or its extract application in treatment gastric ulcer or chronic gastritis medicine.In recent years, we adopt the method for active spike, and Radix Glehniae is carried out the chemical research of system, therefrom separate having obtained 41 native compounds (Chem.Pharm.Bull., 2002,50 (1): 73-77; Chinese herbal medicine, 2002,33 (12): 1063-1065), comprise three classes have the chemical compound of new construction type (1,4-diaryl butane type lignanoid, 8-O-4 ' type neolignan and biphenyl ferulic acid ester are for its clinical practice provides scientific basis.
Summary of the invention
The object of the present invention is to provide the preparation method of extract that contains three active components such as the plain glycosides of lignans glycosides, coumarin glycoside and phenylpropyl alcohol in the Chinese medicine Radix Glehniae, and the medical usage of its treatment gastric ulcer proposed clearly, and provide a kind of science stable, be applicable to the method for preparing lignans glycosides and coumarin glycoside constituents of suitability for industrialized production.
The preparation method of Radix glehniae extract is after Radix Glehniae is pulverized, to decoct (or diafiltration) through water (rare alcohol), precipitate with ethanol, and absorption with macroporous adsorbent resin washes decontamination with water, obtains with pure liquid eluting.Its feature comprises following 3 steps:
A, water extraction: the Radix Glehniae coarse powder, add the water logging bubble that 6-10 doubly measures, heating and refluxing extraction, each 1-3 hour, extract 2-4 time, merge each time extracting solution, the concentrated solution relative density is 1.10-1.20 when being evaporated to 50 ℃.
B, precipitate with ethanol: in A step water extracting liquid, add ethanol, be 60-90%, place, filter to containing the alcohol amount, merging filtrate, decompression and solvent recovery to the concentration of the contained crude drug of solution is 3-5g/ml.
C, macroporous resin adsorption: B step gained solution is through absorption with macroporous adsorbent resin, and with rare alcohol (0-20%) flush away impurity, reuse 50-75% alcohol liquid eluting gets alcoholic solution, reclaims solvent and obtains this extract.
Further, this extract is through repeatedly Sephadex LH-20 column chromatography and anti-phase ODS column chromatography, and water-methanol mixed solvent gradient elution obtains 21 chemical compounds, through physics and chemistry method and nuclear magnetic resonance spectroscopy analysis, has determined their structure.Wherein, 7 lignans or different lignans compounds, dividing in addition is glehlinoside A, glehlinoside B, (-)-secoisolariciresinol4-O-β-D-glucopyranoside, (-)-secoisolariciresinol, glehlinoside C, hesperetin A (cirtrusin A), and (7R, 8S)-and dehydrodiconiferylalcohol4,9-di-O-β-D-glucopyranoside; 8 coumarin kind compounds, be respectively scopoletin (scopoletin), osthole (cnidilin), (3 ' R)-hydroxymarmesin 4 '-O-β-D-glucopyranoside, bergaptol 5-O-β-D-gentiobioside, marmesinin, bergaptol-O-β-D-glucopyranoside, xanthotoxol 8-O-β-D-glucopyran-oside, and 4 "-hydroxyimperatorin 4 "-O-β-D-glucopyranoside; 5 phenylpropyl alcohol chlorins compounds, be respectively praeroside (baihuaqianhuside), ligustrin (syring-in), icariside D, 2-(4 '-hydroxyphenol)-and glycol mono trans-ferulate, 4-[β-D-apiofuranosyl-(1 → 6)-β-D-glucopyranosyloxy]-3-methoxy-propiophenone.In addition, also separation obtains adenosine (adenosine).Glehlinoside A, glehlinoside B, glehlinoside C, 4-[β-D-apiofuranosyl-(1 → 6)-β-D-glucopyranosyloxy]-3-methoxypropiophenone, and bergaptol5-O-β-D-gentiobioside is the illustrated noval chemical compound of inventor.The separation of above-claimed cpd and structure are identified the material base of having illustrated this extract.
The inventor adopts the inductive mouse gastric ulcer model of HCl/EtOH, H respectively
2O
2/ Fe
2+The mensuration of system's Hydroxyl Radical Scavenging, acetic acid stimulate the mensuration of induced mice writhing response, have investigated anti-gastric-ulcer, antioxidation and the analgesic activity of extract.Experimental result shows that the Radix glehniae extract antiulcer action is similar to cimetidine, and has significant free radical scavenging effect and analgesic activity, and the mechanism of its treatment gastric ulcer may be the free radical scavenging that promotes gastric mucosa, alleviates lipid peroxidation.
In sum, extract of the present invention have working substance basis and the mechanism of action clear and definite, preparation technology is simple, the characteristics that are fit to suitability for industrialized production, can be used as treatment gastric ulcer and chronic gastritis medicine material, technology is made acceptable forms clinically such as tablet, capsule, granule or compound preparation routinely.
The specific embodiment
Below further specify the present invention by specific embodiment, embodiment only be used for the explanation, can not limit the scope of the invention.
Embodiment 1
Get Radix Glehniae coarse powder 5kg, add 35L water logging bubble, heating and refluxing extraction 3 times, extraction time was respectively 2,2,1 hours, merged aqueous extract, filtered, and 60 ℃ are evaporated to relative density is 1.20 (50 ℃), gets concentrated solution; Adding ethanol in concentrated solution, is 90% to containing the alcohol amount, places, filter, and merging filtrate, decompression and solvent recovery to the concentration of the contained crude drug of solution is 50g/ml, filters; Filtrate is through absorption with macroporous adsorbent resin, and resin demand 6kg distinguishes water and 20% ethanol flush away impurity, and reuse 50% ethanol liquid eluting is collected alcohol eluen, decompression and solvent recovery, and vacuum drying is pulverized, and obtains this extract 81g.
Embodiment 2
Get Radix Glehniae coarse powder 5kg, add 35L water logging bubble, heating and refluxing extraction 3 times, extraction time was respectively 2,2,1 hours, and merge extractive liquid, filters, and 60 ℃ are evaporated to relative density is 1.10 (50 ℃), gets concentrated solution; Adding ethanol in concentrated solution, is 60% to containing the alcohol amount, places, filter, and merging filtrate, decompression and solvent recovery to the concentration of the contained crude drug of solution is 25g/ml, filters; Filtrate is through absorption with macroporous adsorbent resin, and resin demand 10kg distinguishes water and 20% ethanol flush away impurity, and reuse 75% ethanol liquid eluting is collected alcohol eluen, decompression and solvent recovery, and vacuum drying is pulverized, and obtains this extract 153g.
Embodiment 3 Radix glehniae extracts are to the inhibitory action of the inductive mouse gastric ulcer of HCl/EtOH
(1) experiment material
Animal: (25 ± 2g) 28, fasting is 24 hours before the administration, freely drinks water for the male KM mice.
Reagent: 0.3M HCl/60%EtOH, 0.2%CMCNa, 5% formalin, normal saline, cimetidine.
Material and instrument: 1ml mouse stomach device, 1ml syringe, operating scissors, tweezers, milimeter scale, volumetric flask.
(2) experimental technique
Mice is divided into 4 groups at random, 10 every group: and negative control group (0.2%CMCNa, 10ml/kg, i.g.), positive controls (cimetidine, 100mg/kg
-1, i.g.), and the medicine group (200,400mg/kg, i.g.).After the administration 50 minutes, irritating stomach gives and 0.2m l, 0.3M HCl/60%EtOH causes ulcer, get stomach after 1 hour, inject the 1ml normal saline it is expanded, the formalin fixed with 5% is after 30 minutes, cut off along greater gastric curvature, parallel stomach long axis direction has the black-red tape of elongation on the macroscopic gastric mucosa, measures the length (mm) of each ulcer, and ulcer index (UI) is all ulcer length sums.
Suppression ratio calculates:
I (%)=[UI (matched group)-UI (administration group)]/UI (matched group) * 100%
(3) experimental result
The Radix glehniae extract (by mice body weight 50, the 100mg/kg administration) and the ulcer inhibition rate of positive controls are respectively 38.5%, 58.2% and 60.8%, demonstrate the antiulcer action similar to the positive drug cimetidine.The results are shown in Table 1.
Table 1 Radix glehniae extract is to the inhibitory action [x ± S.E.M. (n=10)] of the inductive mouse gastric ulcer of HCl/EtOH
| Group | Dosage (mg/kg) | Ulcer index (UI) | Suppression ratio (%) |
| 0.2%CMCNa cimetidine extract I extract II | -- 100 50 100 | 43.6±7.4 17.1±4.5* 26.8±3.7* 18.2±6.6* | -- 60.8 38.5 57.2 |
* compare p＜0.01 with model group
Embodiment 4 Radix glehniae extracts are to H
2O
2/ Fe
2+System produces the scavenging action of hydroxy radical
(1) test material
Reagent: 75mM orthophenanthroline ethanol solution, 1.0mM PBS solution, 7.5mM copperas solution, 0.6%H
2O
2Solution
Material and instrument: 721E visible spectrophotometer (Shanghai Spectrum Apparatus Co., Ltd.), 10ml centrifuge tube.
(2) experimental technique
With orthophenanthroline-Fe
2+Oxidizing process detects H
2O
2/ Fe
2+The hydroxy radical that system produces.With distilled water the orthophenanthroline ethanol solution of 75mM is diluted to 7.5mmol/L, the orthophenanthroline solution that adds the 7.5mmol/L of 0.1mL successively in the centrifuge tube of 10mL, 0.5mL the PBS solution of 1.0mmol/L, 0.1mL the copperas solution of 7.5mmol/L, quantity of sample solution, 0.6% the H of 0.125mL
2O
2Solution replenishes volume to 5.0mL with distilled water, and 37 ℃ of insulation reaction 60min measure absorbance A at the 510nm place.Below whenever add a reagent and all need mixing.Not only add sample solution but also add H
2O
2Solution be sample cell; Only add H
2O
2Managing of solution for damaging; Both all do not add not damage pipe.Every duplicate samples parallel assay 3 times is averaged and is calculated apparent hydroxy radical clearance rate S.Computing formula is as follows:
Scavenging (%)=[A (sample)-A (damage)]/[A (not damage)-A (damage)] * 100%
(3) experimental result
Hydroxyl Radical Scavenging to Radix glehniae extract is measured.The result shows, Radix glehniae extract (EC
50=0.11mg/ml) demonstrate certain antioxidation.
Embodiment 5 Radix glehniae extract Dichlorodiphenyl Acetates stimulate the influence of induced mice writhing response
(1) experimental technique
Get 30 of body weight 18-20g male mices, divide equally three groups, one group of ig 100mg/Kg, another group ig 50mg/Kg, matched group ig is with the volume normal saline, and pneumoretroperitoneum was injected 0.3% acetic acid 0.2ml in 1 hour, observed mouse writhing number of times in the 15min.
(2) experimental result
Radix glehniae extract can suppress the mouse writhing number of times that caused by acetic acid, shows analgesic activity.The results are shown in Table 2.
Table 2 Radix glehniae extract stimulates the influence [x ± S.E.M. (n=10)] of induced mice writhing response to Dichlorodiphenyl Acetate
| Group | Dosage (mg/kg) | Turn round body number of times (30min) |
| Normal saline extraction thing I extract II | -- 50 100 | 35.3±9.1 28.8+8.6 21.7±7.5* |
* compare p＜0.05 with model group
Through the anxious malicious evidence of routine, Radix glehniae extract avirulence.
Claims (5)
1, the Radix glehniae extract that has the anti-gastric-ulcer function, it is characterized in that: this extract extracts from the Chinese medicine Radix Glehniae, separates and refining obtaining, include plain glycosides three active components of lignans glycosides, coumarin glycoside and phenylpropyl alcohol, also separate obtaining adenosine.
2, the Radix glehniae extract with anti-gastric-ulcer function according to claim 1, it is characterized in that: the lignans glycosides is respectively glehlinoside A, glehlinoside B, (-)-secoisolariciresinol 4-O-β-D-glucopyranos-ide, (-)-secoisolariciresinol, glehlinoside C, hesperetin A (cirtrusinA), and (7R, 8S)-dehydrodiconiferylalcohol 4,9-di-O-β-D-glucopyr-anoside; Be respectively scopoletin (scopoletin), osthole (cnidilin), (3 ' R)-hydroxymarmesin 4 '-O-β-D-glucopyranoside, bergaptol5-O-β-D-gentiobioside, marmesinin, bergaptol-O-β-D-glucopyranoside, xanthotoxol8-O-β-D-glucopyranoside, and 4 "-hydroxyimperatorin4 "-O-β-D-glucopyranoside; Be respectively praeroside (baihuaqianhuside), ligustrin (syringin), icariside D, 2-(4 '-hydroxyphenol)-and glycol monotrans-ferulate, 4-[β-D-apiofuranosyl-(1 → 6)-β-D-glucopyranosyloxy]-3-methoxypropiophenone.
3, have the Radix glehniae extract of anti-gastric-ulcer function, it is characterized in that: this extract can be used as effective ingredient, mixes with pharmaceutically acceptable carrier, and technology is made tablet, capsule, granule or compound preparation routinely.
4, have the preparation method of the Radix glehniae extract of anti-gastric-ulcer function, comprise pulverizing, boil or diafiltration through decocting, precipitate with ethanol, absorption with macroporous adsorbent resin washes decontamination with water, with pure liquid eluting, it is characterized in that: prepared by following method:
Step 1: the Radix Glehniae coarse powder adds the water logging bubble that 7-10 doubly measures, heating and refluxing extraction, and each 1-3 hour, extract 2-4 time, merge each time extracting solution, the concentrated solution relative density is 1.10-1.20 when being evaporated to 50 ℃.
Step 2: in the water extracting liquid of step 1 gained, add ethanol, be 60-90%, place, filter to containing the alcohol amount, merging filtrate, decompression and solvent recovery to the concentration of the contained crude drug of solution is 3-5g/ml.
Step 3: step gained solution is through absorption with macroporous adsorbent resin, and with rare alcohol (0-20%) flush away impurity, reuse 50-75% alcohol liquid eluting gets alcoholic solution, reclaims solvent and obtains this extract.
5, have the purposes of the Radix glehniae extract of anti-gastric-ulcer function, it is characterized in that: include the application of Radix glehniae extract in preparation anti-gastric-ulcer disease medicament of the plain glycosides active component of lignans glycosides, coumarin glycoside and phenylpropyl alcohol.
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|---|---|---|---|
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| CN101066286B CN101066286B (en) | 2011-12-14 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101757061A (en) * | 2010-01-26 | 2010-06-30 | 沈阳药科大学 | Radix glehniae total lignin as well as preparation method and application thereof |
| CN102526143A (en) * | 2012-02-07 | 2012-07-04 | 杨军 | Preparation method of radix glehniae lung clearing and yin nourishing medicinal granules |
| CN103610991A (en) * | 2013-12-12 | 2014-03-05 | 山东新希望六和集团有限公司 | Medicine for treating swine gastric ulcer and preparation method thereof |
| CN104151373A (en) * | 2013-05-13 | 2014-11-19 | 四川万安石斛产业开发有限公司 | Lignan glycoside compounds and preparation method thereof |
| CN105535784A (en) * | 2016-01-07 | 2016-05-04 | 大连大学 | Traditional Chinese medicine composition for treating stomach illness and application thereof |
| CN105998702A (en) * | 2016-07-11 | 2016-10-12 | 甘肃鑫晟源生物科技开发有限责任公司 | Traditional Chinese medicine Chinese rhubarb gastric floating tablets for treating alimentary tract hemorrhage and preparation method thereof |
-
2007
- 2007-06-07 CN CN2007100115927A patent/CN101066286B/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101757061A (en) * | 2010-01-26 | 2010-06-30 | 沈阳药科大学 | Radix glehniae total lignin as well as preparation method and application thereof |
| CN102526143A (en) * | 2012-02-07 | 2012-07-04 | 杨军 | Preparation method of radix glehniae lung clearing and yin nourishing medicinal granules |
| CN104151373A (en) * | 2013-05-13 | 2014-11-19 | 四川万安石斛产业开发有限公司 | Lignan glycoside compounds and preparation method thereof |
| CN103610991A (en) * | 2013-12-12 | 2014-03-05 | 山东新希望六和集团有限公司 | Medicine for treating swine gastric ulcer and preparation method thereof |
| CN103610991B (en) * | 2013-12-12 | 2015-08-12 | 山东新希望六和集团有限公司 | Medicine being used for the treatment of swine gastric ulcer and preparation method thereof |
| CN105535784A (en) * | 2016-01-07 | 2016-05-04 | 大连大学 | Traditional Chinese medicine composition for treating stomach illness and application thereof |
| CN105998702A (en) * | 2016-07-11 | 2016-10-12 | 甘肃鑫晟源生物科技开发有限责任公司 | Traditional Chinese medicine Chinese rhubarb gastric floating tablets for treating alimentary tract hemorrhage and preparation method thereof |
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