CN101317941A - Medicament for promoting diuresis and easing pain - Google Patents
Medicament for promoting diuresis and easing pain Download PDFInfo
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- CN101317941A CN101317941A CNA2007101106766A CN200710110676A CN101317941A CN 101317941 A CN101317941 A CN 101317941A CN A2007101106766 A CNA2007101106766 A CN A2007101106766A CN 200710110676 A CN200710110676 A CN 200710110676A CN 101317941 A CN101317941 A CN 101317941A
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Abstract
The invention discloses a diuresis analgesia drug extracted from China root and the preparation method and usage thereof. In the method, China root is added with ethanol for the reflux extraction. After the concentration, ethyl acetate is added for extraction. The extract is arranged on silica gel column to be departed to obtain the drug.
Description
Technical field
The present invention relates to the field of Chinese medicines, particularly, relate to a kind of promoting diuresis and easing pain medicine Preparation Method And The Use that from Rhizoma Smilacis Glabrae, extracts.
Background technology
Rhizoma Smilacis Glabrae is the dry rhizome of liliaceous plant smilacis glabra (Smilax glabra Roxb.), claims Limonitum, white surplus grain, kadsurae coccineae etc. again.Used Rhizoma Smilacis Glabrae mostly is red Rhizoma Smilacis Glabrae greatly in the commodity.Sweet in the mouth, light, flat; Return stomach, Liver Channel.Rhizoma Smilacis Glabrae has the effect of dehumidifying, detoxifcation, easing joint movement, is used for the treatment of syphilis, muscles and bones spasm and pain, oedema due to nephritis, stranguria with turbid discharge, leukorrhagia, damp and hot sore, carbuncle, scrofula etc.
Astilbin (astilbin) is a kind of flavanonol glycosides compound that contains in the Rhizoma Smilacis Glabrae.Modern pharmacology studies show that astilbin can obviously increase the total amount of urinating of rat, and dose-response relationship is arranged, and 1h can increase urine Na after the administration
+Output, but to urine K
+Not obviously change of discharge [Wu Liming opens quick. the diuresis of Astilbin and analgesic activity in the Rhizoma Smilacis Glabrae.Chinese crude drug, 1995; 18 (12): 627].In addition, it also has and suppresses aldose reductase, protects the liver, antioxidation, improves effect such as immunologic liver injury.
Mainly concentrated on the research aspect of compound recipe for the report of Rhizoma Smilacis Glabrae, for almost not reporting at Rhizoma Smilacis Glabrae medicine itself in the past.
Summary of the invention
Main purpose of the present invention is, overcomes deficiency of the prior art, and a kind of medicine that extracts from the Chinese medicine Rhizoma Smilacis Glabrae is provided.
Another object of the present invention is to provide manufacturing method for above mentioned medicine.
Another purpose of the present invention has been to provide and has contained the pharmaceutical composition of this medicine as active component.
Another purpose of the present invention is to provide the aforementioned pharmaceutical compositions preparation method.
Another purpose of the present invention has been to provide the application of this medicine in preparation promoting diuresis and easing pain medicine.
Medicine of the present invention is to be prepared from by following method, comprises the steps:
A. rhizoma smilacis glabrae medicinal material is pulverized, the alcohol reflux with 70%～95% is condensed into extractum with the gained extracting solution;
B. with behind the gained extractum water suspendible in the step (a), use ethyl acetate extraction;
C. carry out silica gel column chromatography after gained acetic acid ethyl ester extract in the step (b) being concentrated, eluent carries out eluting, and thin layer chromatography detects to be followed the tracks of, and merges eluent, concentrates and obtains medicine I of the present invention.
Wherein, extracting the used concentration of alcohol of medical material in step a is 70%～95%, preferred 70% ethanol; Its consumption is 6-20 a times of used medical material, preferred 10 times; The number of times of medical material reflux, extract, is 1-4 time, preferred 3 times; Extraction time is 0.5-3 hour, preferred 1.5 hours.
The number of times of ethyl acetate extraction can be 1-6 time in step b, preferred 4 times.
Silica gel is 200～300 orders in step c; Eluent is the mixed liquor of dichloromethane, ethyl acetate and formic acid, and their volume ratio is 500: 500: 0.5～100: 900: 0.5, is preferably 333: 666: 0.5; Adopt thin layer chromatography to detect and follow the tracks of stream part of containing astilbin, its thin layer condition is: selecting silica gel G for use is immobile phase, and mobile phase is dichloromethane: ethyl acetate: formic acid (200: 800: 0.5).
The content height of astilbin among the medicine I of the present invention that said method obtains.For the ease of understanding, we adopt normalization method, according to 2005 editions high performance liquid chromatography of the Pharmacopoeia of the People's Republic of China medicine I of the present invention are measured, and the content of its astilbin reaches more than 80%.
Concrete assay method is as follows:
Testing sample: the method according to embodiment 1 is prepared.
Chromatographic condition: Agilent1100 high performance liquid chromatograph; Chromatographic column: YMC-Pack ODS-A (4.6 * 250mm); Mobile phase: acetonitrile-0.05% phosphoric acid (18: 82); Detect wavelength: 290nm; Column temperature: 25 ℃; Sample size: 10 μ L.
Press peak area and calculate according to normalization method, the content of astilbin is 82%.The HPLC spectrogram is seen accompanying drawing 1.
Said method can also comprise purification step d.
D. the resulting medicine of preceding method is carried out the silicagel column second time (200～300 order) chromatography, with chloroform: methanol (8: 1～4: 1) eluting, concentrate, place, separate out yellow crystal, again through recrystallization, medicine II of the present invention.
Wherein, used eluant is a chloroform in the steps d: methanol, volume ratio are between 8: 1～4: 1, and preferred chloroform: methanol is 6: 1～5: 1; The used organic solvent of recrystallization can be the mixed solution of ethanol, methanol, ethyl acetate or chloroform and methanol, is preferably chloroform: methanol (6: 1); The number of times of recrystallization can be 1-4 time, preferred 2 times.
The content height of astilbin in the medicine of the present invention that said method obtains.For the ease of understanding, we carry out medicine II of the present invention is measured according to 2005 editions high performance liquid chromatography of the Pharmacopoeia of the People's Republic of China, and wherein the content of astilbin reaches more than 95%.Concrete assay method is as follows:
Testing sample: the method according to embodiment 7 is prepared.
Chromatographic condition: Agilent1100 high performance liquid chromatograph; Chromatographic column: YMC-Pack ODS-A (4.6 * 250mm); Mobile phase: acetonitrile-0.05% phosphoric acid (18: 82); Detect wavelength: 290,254 and 330nm; Column temperature: 25 ℃; Sample size: 10 μ L.
Press peak area and calculate according to normalization method, the content of astilbin is more than 95%.The HPLC spectrogram is seen accompanying drawing 2.
Pharmaceutical composition of the present invention also can contain one or more pharmaceutical carriers, and described carrier can be a known common carrier in the pharmaceutical field.Described carrier for example is liquid or solid excipient, diluent, wetting agent, antiseptic, sweeting agent, correctives and coloring agent etc.When the preparation oral formulations, the most frequently used pharmaceutical carrier for example is starch, lactose, Pulvis Talci and/or dextrin etc.
Can carry out according to the general knowledge of pharmaceutical field the kind of pharmaceutical carrier and/or the selection of consumption.Usually, the consumption of carrier can great changes have taken place, and for example, by weight, the consumption of pharmaceutical carrier can be several times of the 1%-of crude drug total amount.
Another purpose of the present invention is to provide described preparation of drug combination method, comprises said medicine I or II are added required pharmaceutical carrier, makes required preparation according to a conventional method.
The Rhizoma Smilacis Glabrae plant resources is abundant, and widely distributed, all there is growth each provinces and regions, the south of the River, and reserves are big, low price.The content height of astilbin has good market application prospect in the medicine of the present invention.
The preparation method of medicine I of the present invention may further comprise the steps:
A. rhizoma smilacis glabrae medicinal material is pulverized, the alcohol reflux with 70%～95% is condensed into extractum with the gained extracting solution;
B. with behind the gained extractum water suspendible in the step (a), use ethyl acetate extraction;
C. carry out silica gel column chromatography after gained acetic acid ethyl ester extract in the step (b) being concentrated, eluent carries out eluting, and thin layer chromatography detects to be followed the tracks of, and merges eluent, concentrates and obtains medicine I of the present invention.
Wherein, extracting the used concentration of alcohol of medical material in step a is 70%～95%, preferred 70% ethanol; Its consumption is 6-20 a times of used medical material, preferred 10 times; The number of times of medical material reflux, extract, is 1-4 time, preferred 3 times; Extraction time is 0.5-3 hour, preferred 1.5 hours.
The number of times of ethyl acetate extraction can be 1-6 time in step b, preferred 4 times.
Silica gel is 200～300 orders in step c; Eluent is the mixed liquor of dichloromethane, ethyl acetate and formic acid, and their volume ratio is 500: 500: 0.5～100: 900: 0.5, is preferably 333: 666: 0.5; Adopt thin layer chromatography to detect the content of following the tracks of astilbin, its thin layer condition is: selecting silica gel G for use is immobile phase, and mobile phase is dichloromethane: ethyl acetate: formic acid (200: 800: 0.5).
Said method can also comprise purification step d, prepares medicine II of the present invention.
D. the resulting medicine of preceding method is carried out the silicagel column second time (200～300 order) chromatography, with chloroform: methanol (8: 1～4: 1) eluting, concentrate, place, separate out yellow crystal, again through recrystallization, medicine of the present invention.
Wherein, used eluant is a chloroform in the steps d: methanol, volume ratio are between 8: 1～4: 1, and preferred chloroform: methanol is 6: 1～5: 1; The used organic solvent of recrystallization can be the mixed solution of ethanol, methanol, ethyl acetate or chloroform and methanol, is preferably chloroform: methanol (6: 1); The number of times of recrystallization can be 1-4 time, preferred 2 times.
Preparation method of the present invention is simple, quick.The content height of astilbin in the extract of preparation.The Rhizoma Smilacis Glabrae plant resources is abundant, and widely distributed, all there is growth each provinces and regions, the south of the River, and reserves are big, low price, and wherein higher this method of content of astilbin has good market prospect.
Medicine I of the present invention and II have good diuresis, analgesic effect.
1 material
1.1 trial drug and reagent: medicine I of the present invention and II, adopt the method preparation of the embodiment of the invention 1 and 7 respectively, provide by Beijing University of Chinese Medicine's laboratory, be made into desired concn with preceding with aseptic NS; Furosemide injection, lot number: 020102, Xi'an Pharmaceutical joint-stock company; Scorching pain 25m/g lot number: 0206052, Jiangsu vast stretch of wooded country pharmaceutcal corporation, Ltd.Carrageenin and uric acid sodium (MSU) are SIGMA company and produce, and prepare with aseptic NS with preceding.
1.2 animal: the SD rat is male, body weight 160 ± 20g. one-level.The quality certification number: the real moving word in capital 2002-32 number; Kunming mouse. body weight 20 ± 2g or 28 ± 2g, one-level, the quality certification number: the real moving word in capital 2002-33 number. provide by laboratory animal room of Beijing University of Chinese Medicine.
2 methods and result
2.1 little bloated influence due to the xylol: 50 of mices, male and female half and half .20 ± 2g is divided into 5 groups at random, ig administration, totally 4 days every day 1 time.40min after the last administration is coated with 30ul caused by dimethylbenzene xylene inflammation at mouse right ear, puts to death animal behind the 30min, cuts ears. and get the ears sheet with 6mm diameter card punch and weigh respectively, the difference of two auricles is the swelling degree.Results model contrast, medicine I of the present invention, II and hydrocortisone 20mg/kg group swelling degree are respectively 11.50 ± 3.21mg, 7.30 ± 2.28mg (P＜0.01), 7.80 ± 2.04mg (P＜0.05) and 5.10 ± 2.41nag (P＜0.01), show that medicine I of the present invention and II xylol induced mice ear swelling have remarkable inhibitory action.
2.2 the influence to Ovum Gallus domesticus album and the foot swelling of carrageenin induced mice: 40 of mices are male, body weight 28 ± 2g, ig administration, totally 4 days every day 1 time.30min after the last administration, the right foot of every Mus is annotated people 10% Ovum Gallus domesticus album 30IA and is caused inflammation, behind the 1h under ankle joint 0.5cm cut at place that pair the metapedes sole of the foot is subcutaneous weighs. with left and right sides heavy sensation in the foot difference is the swelling degree.Other gets 40 of mices, and is male. and grouping and administration are the same. and 30min. causes inflammation at the right foot injection of mice 1% carrageenin 30 μ l after the last administration, claims biped heavy by last method behind the 3.5h, obtains the swelling degree.As seen from Table 1, medicine I of the present invention, II and hydrocortisone all can obviously suppress the mice foot swelling due to Ovum Gallus domesticus album and the carrageenin.
Table 1, to the influence of Ovum Gallus domesticus album and the foot swelling of carrageenin induced mice (X ± s, n=8)
Annotate: compare with matched group
*P＜0.05,
*P＜0.01 (down together)
2.3 influence: 50 of rats selecting to be suitable for the diuresis experiment with rat metabolic cage method to rat urine amount, body weight 160 ± 10g, male. rat freely drinks water before the experiment, fasting 18h, ig NS 25ml/kg carries out the water load, and the tail vein injects medicinal liquid or NS, and the administration volume is 2ml/kg, put people rat metabolic cage after the administration. per hour collect urine once, all gently press the rat lower abdomen to drain surplus urine before and after the collection urine.1h, 2h, 3h and 4h total volume of urine after the record administration calculate the urine amount that rat per 100 restrains body weight.From table 2 result as seen, medicine I of the present invention, II all can obviously increase rat urine amount.
Table 2, to the influence of rat urine amount (X ± s, n=10)
2.4 the Dichlorodiphenyl Acetate induced mice is turned round the influence of body: 50 male and female half and half of mice.20 ± 2g intravenous injection NS medicinal liquid, the every Mus ip of 15min injects 0.7% acetic acid 10ml/kg after the administration, and aspirin ig every day is administered once, and continuous 2 days, the same method injection of last administration 1h acetic acid, mouse writhing number of times in the record 15mim.As shown in table 3, medicine I of the present invention and II and aspirin Dichlorodiphenyl Acetate induced mice writhing response all have obvious inhibitory action.
Table 3, Dichlorodiphenyl Acetate induced mice are turned round the influence (X ± s) of body
By above-mentioned experiment, medicine I of the present invention as can be seen and II all have good analgesia, diuretic actions.
Description of drawings
Fig. 1, medicine I high-efficient liquid phase chromatogram of the present invention
Fig. 2, the high-efficient liquid phase chromatogram of medicine II of the present invention under three different wave lengths
The specific embodiment
Embodiment 1
A. the Poria medical material that fetches earth is pulverized, and adds the alcohol reflux 3 times of 10 times of amounts 95% of medical material amount, and each 1.5 hours, merge extractive liquid, was condensed into extractum with the gained extracting solution;
B. with behind the gained extractum water suspendible in the step (a), use ethyl acetate extraction 4 times;
C. carry out silica gel column chromatography after gained acetic acid ethyl ester extract in the step (b) being concentrated, silica filler is 200～300 orders, adopt the mixed liquor of dichloromethane, ethyl acetate and formic acid (333: 666: 0.5) to carry out eluting, adopting thin layer chromatography to detect follows the tracks of, its thin layer condition is: selecting silica gel G for use is immobile phase, mobile phase is dichloromethane: ethyl acetate: formic acid (200: 800: 0.5), merge eluent, and concentrate and obtain medicine I of the present invention.
A. the Poria medical material that fetches earth is pulverized, and adds the alcohol reflux 1.5 hours of 6 times of amounts 70% of medical material amount, collects extracting solution, and the gained extracting solution is condensed into extractum;
B. with behind the gained extractum water suspendible in the step (a), use ethyl acetate extraction 1 time;
C. carry out silica gel column chromatography after gained acetic acid ethyl ester extract in the step (b) being concentrated, silica filler is 200～300 orders, adopt the mixed liquor of dichloromethane, ethyl acetate and formic acid (500: 500: 0.5) to carry out eluting, adopting thin layer chromatography to detect follows the tracks of, its thin layer condition is: selecting silica gel G for use is immobile phase, mobile phase is dichloromethane: ethyl acetate: formic acid (200: 800: 0.5), merge eluent, and concentrate and obtain medicine I of the present invention.
Embodiment 3
A. the Poria medical material that fetches earth is pulverized, and adds the alcohol reflux 2 times of 20 times of amounts 95% of medical material amount, and each 0.5 hour, merge extractive liquid, was condensed into extractum with the gained extracting solution;
B. with behind the gained extractum water suspendible in the step (a), use ethyl acetate extraction 5 times;
C. carry out silica gel column chromatography after gained acetic acid ethyl ester extract in the step (b) being concentrated, silica filler is 200～300 orders, adopt the mixed liquor of dichloromethane, ethyl acetate and formic acid (100: 900: 0.5) to carry out eluting, adopting thin layer chromatography to detect follows the tracks of, its thin layer condition is: selecting silica gel G for use is immobile phase, mobile phase is dichloromethane: ethyl acetate: formic acid (200: 800: 0.5), merge eluent, and concentrate and obtain medicine I of the present invention.
Embodiment 4
A. the Poria medical material that fetches earth is pulverized, and adds the alcohol reflux 2 times of 15 times of amounts 80% of medical material amount, and each 0.5 hour, merge extractive liquid, was condensed into extractum with the gained extracting solution;
B. with behind the gained extractum water suspendible in the step (a), use ethyl acetate extraction 5 times;
V. carry out silica gel column chromatography after gained acetic acid ethyl ester extract in the step (b) being concentrated, silica filler is 200～300 orders, adopt the mixed liquor of dichloromethane, ethyl acetate and formic acid (100: 900: 0.5) to carry out eluting, adopting thin layer chromatography to detect follows the tracks of, its thin layer condition is: selecting silica gel G for use is immobile phase, mobile phase is dichloromethane: ethyl acetate: formic acid (200: 800: 0.5), merge eluent, and concentrate and obtain medicine I of the present invention.
A. the Poria medical material that fetches earth is pulverized, and adds the alcohol reflux 2 times of 20 times of amounts 95% of medical material amount, and each 0.5 hour, merge extractive liquid, was condensed into extractum with the gained extracting solution;
B. with behind the gained extractum water suspendible in the step (a), use ethyl acetate extraction 5 times;
C. carry out silica gel column chromatography after gained acetic acid ethyl ester extract in the step (b) being concentrated, silica filler is 200～300 orders, adopt the mixed liquor of dichloromethane, ethyl acetate and formic acid (500: 500: 0.5) to carry out eluting, adopting thin layer chromatography to detect follows the tracks of, its thin layer condition is: selecting silica gel G for use is immobile phase, mobile phase is dichloromethane: ethyl acetate: formic acid (200: 800: 0.5), merge eluent, and concentrate and obtain medicine I of the present invention.
Embodiment 6
A. the Poria medical material that fetches earth is pulverized, and adds the alcohol reflux 2 times of 8 times of amounts 85% of medical material amount, and each 2.5 hours, merge extractive liquid, was condensed into extractum with the gained extracting solution;
B. with behind the gained extractum water suspendible in the step (a), use ethyl acetate extraction 4 times;
C. carry out silica gel column chromatography after gained acetic acid ethyl ester extract in the step (b) being concentrated, silica filler is 200～300 orders, adopt the mixed liquor of dichloromethane, ethyl acetate and formic acid (333: 666: 0.5) to carry out eluting, adopting thin layer chromatography to detect follows the tracks of, its thin layer condition is: selecting silica gel G for use is immobile phase, mobile phase is dichloromethane: ethyl acetate: formic acid (200: 800: 0.5), merge eluent, and concentrate and obtain medicine I of the present invention.
Embodiment 7
A. the Poria medical material that fetches earth is pulverized, and adds the alcohol reflux 3 times of 10 times of amounts 70% of medical material amount, and each 1.5 hours, merge extractive liquid, was condensed into extractum with the gained extracting solution;
B. with behind the gained extractum water suspendible in the step (a), use ethyl acetate extraction 4 times;
C. carry out silica gel column chromatography after gained acetic acid ethyl ester extract in the step (b) being concentrated, silica filler is 200～300 orders, adopt the mixed liquor of dichloromethane, ethyl acetate and formic acid (333: 666: 0.5) to carry out eluting, adopting thin layer chromatography to detect follows the tracks of, its thin layer condition is: selecting silica gel G for use is immobile phase, mobile phase is dichloromethane: ethyl acetate: formic acid (200: 800: 0.5), merge eluent, and concentrate and obtain medicine crude product of the present invention;
D. the resulting medicine crude product of preceding method is carried out the silicagel column second time (200～300 order) chromatography, with chloroform: methanol (6: 1) eluting concentrates, place, separate out yellow crystal, again with chloroform: methanol (6: 1) is solvent recrystallization 2 times, gets medicine II of the present invention.
Embodiment 8
A. the Poria medical material that fetches earth is pulverized, and adds the alcohol reflux 3 times of 10 times of amounts 95% of medical material amount, and each 1.5 hours, merge extractive liquid, was condensed into extractum with the gained extracting solution;
B. with behind the gained extractum water suspendible in the step (a), use ethyl acetate extraction 4 times;
C. carry out silica gel column chromatography after gained acetic acid ethyl ester extract in the step (b) being concentrated, silica filler is 200～300 orders, adopt the mixed liquor of dichloromethane, ethyl acetate and formic acid (333: 666: 0.5) to carry out eluting, adopting thin layer chromatography to detect follows the tracks of, its thin layer condition is: selecting silica gel G for use is immobile phase, mobile phase is dichloromethane: ethyl acetate: formic acid (200: 800: 0.5), merge eluent, and concentrate and obtain medicine crude product of the present invention;
D. the resulting medicine crude product of preceding method is carried out the silicagel column second time (200～300 order) chromatography, with chloroform: methanol (6: 1) eluting, concentrate, place, separate out yellow crystal, be solvent recrystallization 1 time again with ethanol, medicine II of the present invention.
Embodiment 9
A. the Poria medical material that fetches earth is pulverized, and adds the alcohol reflux 3 times of 10 times of amounts 95% of medical material amount, and each 1.5 hours, merge extractive liquid, was condensed into extractum with the gained extracting solution;
B. with behind the gained extractum water suspendible in the step (a), use ethyl acetate extraction 4 times;
C. carry out silica gel column chromatography after gained acetic acid ethyl ester extract in the step (b) being concentrated, silica filler is 200～300 orders, adopt the mixed liquor of dichloromethane, ethyl acetate and formic acid (333: 666: 0.5) to carry out eluting, adopting thin layer chromatography to detect follows the tracks of, its thin layer condition is: selecting silica gel G for use is immobile phase, mobile phase is dichloromethane: ethyl acetate: formic acid (200: 800: 0.5), merge eluent, and concentrate and obtain medicine crude product of the present invention;
D. the resulting medicine crude product of preceding method is carried out the silicagel column second time (200～300 order) chromatography, with chloroform: methanol (5.5: 1) eluting, concentrate, place, separate out yellow crystal, be solvent recrystallization 3 times again with methanol, medicine II of the present invention.
A. the Poria medical material that fetches earth is pulverized, and adds the alcohol reflux 3 times of 10 times of amounts 95% of medical material amount, and each 1.5 hours, merge extractive liquid, was condensed into extractum with the gained extracting solution;
B. with behind the gained extractum water suspendible in the step (a), use ethyl acetate extraction 4 times;
C. carry out silica gel column chromatography after gained acetic acid ethyl ester extract in the step (b) being concentrated, silica filler is 200～300 orders, adopt the mixed liquor of dichloromethane, ethyl acetate and formic acid (333: 666: 0.5) to carry out eluting, adopting thin layer chromatography to detect follows the tracks of, its thin layer condition is: selecting silica gel G for use is immobile phase, mobile phase is dichloromethane: ethyl acetate: formic acid (200: 800: 0.5), merge eluent, and concentrate and obtain medicine crude product of the present invention;
D. the resulting medicine crude product of preceding method is carried out the silicagel column second time (200～300 order) chromatography, with chloroform: methanol (5.5: 1) eluting, concentrate, place, separate out yellow crystal, be solvent recrystallization 4 times again with the ethyl acetate, medicine II of the present invention.
Embodiment 11
A. the Poria medical material that fetches earth is pulverized, and adds the alcohol reflux 3 times of 10 times of amounts 95% of medical material amount, and each 1.5 hours, merge extractive liquid, was condensed into extractum with the gained extracting solution;
B. with behind the gained extractum water suspendible in the step (a), use ethyl acetate extraction 4 times;
C. carry out silica gel column chromatography after gained acetic acid ethyl ester extract in the step (b) being concentrated, silica filler is 200～300 orders, adopt the mixed liquor of dichloromethane, ethyl acetate and formic acid (333: 666: 0.5) to carry out eluting, adopting thin layer chromatography to detect follows the tracks of, its thin layer condition is: selecting silica gel G for use is immobile phase, mobile phase is dichloromethane: ethyl acetate: formic acid (200: 800: 0.5), merge eluent, and concentrate and obtain medicine crude product of the present invention;
D. the resulting medicine crude product of preceding method is carried out the silicagel column second time (200～300 order) chromatography, with chloroform: methanol (6: 1) eluting concentrates, place, separate out yellow crystal, the mixed solution (1: 1) with chloroform and methanol is solvent recrystallization 4 times again, gets medicine II of the present invention.
Embodiment 12
A. the Poria medical material that fetches earth is pulverized, and adds the alcohol reflux 3 times of 10 times of amounts 95% of medical material amount, and each 1.5 hours, merge extractive liquid, was condensed into extractum with the gained extracting solution;
B. with behind the gained extractum water suspendible in the step (a), use ethyl acetate extraction 4 times;
C. carry out silica gel column chromatography after gained acetic acid ethyl ester extract in the step (b) being concentrated, silica filler is 200～300 orders, adopt the mixed liquor of dichloromethane, ethyl acetate and formic acid (333: 666: 0.5) to carry out eluting, adopting thin layer chromatography to detect follows the tracks of, its thin layer condition is: selecting silica gel G for use is immobile phase, mobile phase is dichloromethane: ethyl acetate: formic acid (200: 800: 0.5), merge eluent, and concentrate and obtain medicine crude product of the present invention;
D. the resulting medicine crude product of preceding method is carried out the silicagel column second time (200～300 order) chromatography, with chloroform: methanol (6: 1) eluting concentrates, place, separate out yellow crystal, the mixed solution (6: 1) with chloroform and methanol is solvent recrystallization 2 times again, gets medicine II of the present invention.
Embodiment 13
A. the Poria medical material that fetches earth is pulverized, and adds the alcohol reflux 3 times of 10 times of amounts 95% of medical material amount, and each 1.5 hours, merge extractive liquid, was condensed into extractum with the gained extracting solution;
B. with behind the gained extractum water suspendible in the step (a), use ethyl acetate extraction 4 times;
C. carry out silica gel column chromatography after gained acetic acid ethyl ester extract in the step (b) being concentrated, silica filler is 200～300 order orders, adopt the mixed liquor of dichloromethane, ethyl acetate and formic acid (333: 666: 0.5) to carry out eluting, adopting thin layer chromatography to detect follows the tracks of, its thin layer condition is: selecting silica gel G for use is immobile phase, mobile phase is dichloromethane: ethyl acetate: formic acid (200: 800: 0.5), merge eluent, and concentrate and obtain medicine crude product of the present invention;
D. the resulting medicine crude product of preceding method is carried out the silicagel column second time (200～300 order) chromatography, with chloroform: methanol (4: 1) eluting concentrates, place, separate out yellow crystal, the mixed solution (6: 1) with chloroform and methanol is solvent recrystallization 2 times again, gets medicine II of the present invention.
Embodiment 14
A. the Poria medical material that fetches earth is pulverized, and adds the alcohol reflux 3 times of 10 times of amounts 95% of medical material amount, and each 1.5 hours, merge extractive liquid, was condensed into extractum with the gained extracting solution;
B. with behind the gained extractum water suspendible in the step (a), use ethyl acetate extraction 4 times;
C. carry out silica gel column chromatography after gained acetic acid ethyl ester extract in the step (b) being concentrated, silica filler is 200～300 orders, adopt the mixed liquor of dichloromethane, ethyl acetate and formic acid (333: 666: 0.5) to carry out eluting, adopting thin layer chromatography to detect follows the tracks of, its thin layer condition is: selecting silica gel G for use is immobile phase, mobile phase is dichloromethane: ethyl acetate: formic acid (200: 800: 0.5), merge eluent, and concentrate and obtain medicine crude product of the present invention;
D. the resulting medicine crude product of preceding method is carried out the silicagel column second time (200～300 order) chromatography, with chloroform: methanol (8: 1) eluting concentrates, place, separate out yellow crystal, the mixed solution (6: 1) with chloroform and methanol is solvent recrystallization 2 times again, gets medicine II of the present invention.
The medicine adding starch of preparation among the embodiment 1 is made tablet.
Embodiment 16
The medicine of preparation among the embodiment 1 is added dextrin, and wet granulation incapsulates and makes capsule.
Embodiment 17
The medicine adding starch of preparation among the embodiment 7 is made tablet.
Embodiment 18
The medicine of preparation among the embodiment 7 is added dextrin, and wet granulation incapsulates and makes capsule.
Claims (14)
1. the medicine of a promoting diuresis and easing pain is characterized in that adopting following step to be prepared from:
A. rhizoma smilacis glabrae medicinal material is pulverized, the alcohol reflux with 70%～95% is condensed into extractum with the gained extracting solution;
B. with behind the gained extractum water suspendible in the step (a), use ethyl acetate extraction;
C. carry out silica gel column chromatography after gained acetic acid ethyl ester extract in the step (b) being concentrated, eluent carries out eluting, and thin layer chromatography detects to be followed the tracks of, and merges eluent, concentrates and obtains medicine I of the present invention.
2. medicine according to claim 1, wherein extracting the used concentration of alcohol of medical material among the step a is 70%～95%; Its consumption is 6-20 a times of used medical material; The number of times of medical material reflux, extract, is 1-4 time; Extraction time is 0.5-3 hour.
3. medicine according to claim 2, wherein extracting the used concentration of alcohol of medical material among the step a is 70%; Its consumption is 10 times of used medical material; The number of times of medical material reflux, extract, is 3 times; Extraction time is 1.5 hours.
4. medicine according to claim 1, wherein the number of times of ethyl acetate extraction can be 1-6 time among the step b.
5. medicine according to claim 4, wherein the number of times of ethyl acetate extraction can be 4 times among the step b.
6. medicine according to claim 1, wherein silica gel is 200～300 orders among the step c; Eluent is the mixed liquor of dichloromethane, ethyl acetate and formic acid, and volume ratio is 500: 500: 0.5～100: 900: 0.5; Adopt thin layer chromatography to detect and follow the tracks of stream part of containing astilbin, its thin layer condition is: selecting silica gel G for use is immobile phase, and mobile phase is dichloromethane: ethyl acetate: formic acid (200: 800: 0.5).
7. medicine according to claim 6, wherein eluent is the mixed liquor of dichloromethane, ethyl acetate and formic acid among the step c, volume ratio is 333: 666: 0.5.
8. medicine according to claim 1 is characterized in that comprising purification step d: medicine I is carried out the silicagel column second time (200～300 order) chromatography, with chloroform: methanol (8: 1～4: 1) eluting, concentrate, place, separate out yellow crystal, through recrystallization, get medicine II of the present invention again.
9. medicine according to claim 8, wherein used eluent is a chloroform in the steps d: methanol, volume ratio are 8: 1～4: 1; The used organic solvent of recrystallization is the mixed solution of ethanol, methanol, ethyl acetate or chloroform and methanol; The number of times of recrystallization can be 1-4 time.
10. medicine according to claim 9, wherein used eluant is the mixed liquor of chloroform and methanol in the steps d, its volume ratio is 6: 1～5: 1; The used organic solvent of recrystallization is the mixed liquor of chloroform and methanol, and its volume ratio is 6: 1; The number of times of recrystallization can be 2 times.
11. a pharmaceutical composition, comprising arbitrary medicine among the claim 1-10 is active component and conventional pharmaceutical carrier.
12. the preparation method of the medicine of a promoting diuresis and easing pain comprises the steps:
A. rhizoma smilacis glabrae medicinal material is pulverized, the alcohol reflux with 70%～95% is condensed into extractum with the gained extracting solution;
B. with behind the gained extractum water suspendible in the step (a), use ethyl acetate extraction;
C. carry out silica gel column chromatography after gained acetic acid ethyl ester extract in the step (b) being concentrated, eluent carries out eluting, and thin layer chromatography detects to be followed the tracks of, and merges eluent, concentrates and obtains medicine I of the present invention.
13. method according to claim 12, it is characterized in that to comprise purification step d: medicine I is carried out the silicagel column second time (200～300 order) chromatography, with chloroform: methanol (8: 1～4: 1) eluting, concentrate, place, separate out yellow crystal,, get medicine II of the present invention again through recrystallization.
14. the application of arbitrary medicine in preparation promoting diuresis and easing pain medicine in the claim 1～10.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102964407A (en) * | 2012-12-15 | 2013-03-13 | 广东世信药业有限公司 | Method for extracting astilbin from rhizoma smilacis glabrae and astilbin prepared thereby |
| CN104991031A (en) * | 2015-07-23 | 2015-10-21 | 河北中医学院 | Rapid multiple information thin-layer identification method of smilax glabra and water extract thereof |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100336542C (en) * | 2005-11-01 | 2007-09-12 | 南京大学 | Glabrous greenbrier total saponin extract and its prepn and use |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102964407A (en) * | 2012-12-15 | 2013-03-13 | 广东世信药业有限公司 | Method for extracting astilbin from rhizoma smilacis glabrae and astilbin prepared thereby |
| CN104991031A (en) * | 2015-07-23 | 2015-10-21 | 河北中医学院 | Rapid multiple information thin-layer identification method of smilax glabra and water extract thereof |
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