CN101380356B - Tibetan medicine Duyiwei total flavone extract and extraction method and use thereof - Google Patents
Tibetan medicine Duyiwei total flavone extract and extraction method and use thereof Download PDFInfo
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- CN101380356B CN101380356B CN 200810228070 CN200810228070A CN101380356B CN 101380356 B CN101380356 B CN 101380356B CN 200810228070 CN200810228070 CN 200810228070 CN 200810228070 A CN200810228070 A CN 200810228070A CN 101380356 B CN101380356 B CN 101380356B
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- 229930003944 flavone Natural products 0.000 title claims abstract description 32
- 235000011949 flavones Nutrition 0.000 title claims abstract description 32
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 title claims abstract description 23
- 150000002212 flavone derivatives Chemical class 0.000 title claims abstract description 23
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 title claims abstract description 23
- 239000003814 drug Substances 0.000 title claims abstract description 19
- 239000000284 extract Substances 0.000 title claims description 40
- 238000000605 extraction Methods 0.000 title claims description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 97
- 238000000034 method Methods 0.000 claims abstract description 45
- 239000011347 resin Substances 0.000 claims abstract description 24
- 229920005989 resin Polymers 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 32
- 230000001476 alcoholic effect Effects 0.000 claims description 28
- 239000003480 eluent Substances 0.000 claims description 25
- 239000012141 concentrate Substances 0.000 claims description 19
- 238000002360 preparation method Methods 0.000 claims description 17
- 238000010828 elution Methods 0.000 claims description 14
- 239000012535 impurity Substances 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 11
- 239000012567 medical material Substances 0.000 claims description 11
- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 claims description 10
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 10
- 239000003208 petroleum Substances 0.000 claims description 10
- 238000001035 drying Methods 0.000 claims description 9
- 238000010992 reflux Methods 0.000 claims description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 229910021529 ammonia Inorganic materials 0.000 claims description 4
- 239000000470 constituent Substances 0.000 claims description 4
- 239000012488 sample solution Substances 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 4
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 3
- 239000000920 calcium hydroxide Substances 0.000 claims description 3
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 239000003937 drug carrier Substances 0.000 claims 1
- 239000002904 solvent Substances 0.000 abstract description 13
- 238000000926 separation method Methods 0.000 abstract description 11
- 208000002193 Pain Diseases 0.000 abstract description 8
- 230000036407 pain Effects 0.000 abstract description 8
- 241001191006 Phlomoides rotata Species 0.000 abstract description 3
- 239000004615 ingredient Substances 0.000 abstract description 2
- 238000005202 decontamination Methods 0.000 abstract 2
- 230000003588 decontaminative effect Effects 0.000 abstract 2
- 239000000463 material Substances 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 23
- 238000000746 purification Methods 0.000 description 19
- 239000012153 distilled water Substances 0.000 description 14
- 241000699670 Mus sp. Species 0.000 description 12
- 230000000202 analgesic effect Effects 0.000 description 12
- BSYNRYMUTXBXSQ-UHFFFAOYSA-N Aspirin Chemical compound CC(=O)OC1=CC=CC=C1C(O)=O BSYNRYMUTXBXSQ-UHFFFAOYSA-N 0.000 description 10
- 229960001138 acetylsalicylic acid Drugs 0.000 description 10
- 150000002213 flavones Chemical class 0.000 description 9
- -1 iridoids Natural products 0.000 description 8
- 238000012360 testing method Methods 0.000 description 8
- 239000002253 acid Substances 0.000 description 7
- 238000004090 dissolution Methods 0.000 description 7
- 239000000796 flavoring agent Substances 0.000 description 7
- 235000019634 flavors Nutrition 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- 239000010413 mother solution Substances 0.000 description 7
- 230000003252 repetitive effect Effects 0.000 description 7
- 238000010025 steaming Methods 0.000 description 7
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
- 238000002474 experimental method Methods 0.000 description 6
- 239000000706 filtrate Substances 0.000 description 6
- 238000012449 Kunming mouse Methods 0.000 description 4
- 229940079593 drug Drugs 0.000 description 4
- 230000002496 gastric effect Effects 0.000 description 4
- 235000008216 herbs Nutrition 0.000 description 4
- 238000001802 infusion Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000000523 sample Substances 0.000 description 3
- 238000003809 water extraction Methods 0.000 description 3
- 208000000114 Pain Threshold Diseases 0.000 description 2
- 230000036592 analgesia Effects 0.000 description 2
- 210000000988 bone and bone Anatomy 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000556 factor analysis Methods 0.000 description 2
- 229930003935 flavonoid Natural products 0.000 description 2
- 150000002215 flavonoids Chemical class 0.000 description 2
- 235000017173 flavonoids Nutrition 0.000 description 2
- 239000004519 grease Substances 0.000 description 2
- 230000023597 hemostasis Effects 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 230000037040 pain threshold Effects 0.000 description 2
- 239000013641 positive control Substances 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 238000009333 weeding Methods 0.000 description 2
- 208000006820 Arthralgia Diseases 0.000 description 1
- 208000032843 Hemorrhage Diseases 0.000 description 1
- 208000025747 Rheumatic disease Diseases 0.000 description 1
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- 238000010521 absorption reaction Methods 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
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- 229940030225 antihemorrhagics Drugs 0.000 description 1
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- 230000017531 blood circulation Effects 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 239000003518 caustics Substances 0.000 description 1
- 230000004087 circulation Effects 0.000 description 1
- 239000000287 crude extract Substances 0.000 description 1
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- 238000011978 dissolution method Methods 0.000 description 1
- 239000002552 dosage form Substances 0.000 description 1
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- 238000002481 ethanol extraction Methods 0.000 description 1
- 230000000025 haemostatic effect Effects 0.000 description 1
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- Medicines Containing Plant Substances (AREA)
Abstract
The invention belongs to the technical field of medicine, and provides a Tibetan pharmaceutical, lamiophlomis rotata total flavone extractive as well as an extracting method and the application thereof. The method uses Tibetan pharmaceutical lamiophlomis rotata as raw material, uses ethanol prepared by alkalescence solution with different pH values as solvent, and adopts a backflow method for extracting. After two steps of decontamination and the separation and enrichment of macropore resin, the total flavone extractive with the purity being 50 to 95 percent can be obtained from extracting solution. In the process of separation and enrichment, after the two steps of decontamination and the separation and enrichment of macropore resin, a sample with high purity can be obtained and the purity of the total flavone in the sample can be 95 percent at most, wherein, the percentage is higher than the number reported in documents. The invention also provides the application of the total flavone as pain killer medicine and stanch medicine. The paper optimizes and improves the extracting method so as to increase the transfer rate of effective ingredient, improve the utilization rate of medicinal materials and save a great amount of cost effectively, thus having high economical benefit.
Description
Technical field
The invention belongs to medical technical field, relate to Tibetan medicine Duyiwei total flavone extract and method for distilling thereof and purposes.
Background technology
Radix Lamiophlomidis Rotatae [Lamiophlomis rotata (Ben thl) kudo] is one of national folks such as China Tibetan, illiteracy, Nahsi medical herbs commonly used; Effect with hemostasis, analgesia detumescence, blood circulation promoting and blood stasis dispelling, benefit marrow, circulation of qi promoting, reunion of fractured tendons and bones; The clinical edge of a knife pain behind the multiple surgical operation, hemorrhage that is mainly used in; Exogenous injury, muscles and bones is sprained, diseases such as rheumatic arthralgia.
Up to the present, the known chemical composition mainly contains flavonoid, iridoids, triterpene saponin etc. in the bibliographical information Radix Lamiophlomidis Rotatae, discovers, contained total flavonoid composition has the effect of tangible pain easing and hemostasis.Common lamiophlomis root prepn comprises Radix Lamiophlomidis Rotatae capsule, Radix Lamiophlomidis Rotatae sheet, Duyiwei soft capsule etc.Preparation technology's method of present commercially available common lamiophlomis root prepn is outmoded, all is the preparations that are prepared from through simple extraction back gained crude extract the Radix Lamiophlomidis Rotatae medical material, and active constituent content is low, and day clothes dosage is big.CN1559550A discloses Radix Lamiophlomidis Rotatae extract novel form and preparation method thereof, adopts that decocting boils, concentrates, exsiccant method prepares its extract, and the prepared extract active constituent content of the method is low, and taking dose is big.For reducing taking dose, improving drug effect, reach safe, effective, controlled purpose, the present invention adopts new method that Radix Lamiophlomidis Rotatae is carried out extraction separation; Obtain more highly purified extract; To improve active constituent content in the preparation, reduced taking dose, improve curative effect.
For the separation and concentration of natural product, macroreticular resin absorbing method is a kind of method of very effective suitable suitability for industrialized production.This method begins to carry out remove impurity from sample treatment; Remove alcohol insoluble matter impurity through the hot ethanol dissolution method; After petroleum ether extraction weeding of grease solubility impurity; The sample upper prop carries out the sample that separation and concentration obtains higher degree after above-mentioned two step remove impurity, and total flavones purity is higher than the finding bibliographical information up to 95%.
Summary of the invention
The object of the present invention is to provide a kind of total flavones that from Tibet medicine lamivphlomis root, extracts and method for distilling and purposes.
The objective of the invention is to realize through following technical scheme:
The method for distilling of Duyiwei total flavone comprises following processing step: 1. get drying, the Radix Lamiophlomidis Rotatae medical material of pulverizing uses 6-10 doubly to measure concentration and is the alcoholic solution 40-100 ℃ of water-bath reflux, extract, of 5%-95% 2-4 time, filters, and filtrating concentrates.2. get above-mentioned concentrate,, put cold with 50-70% alcoholic solution heating for dissolving.Remove by filter alcohol insoluble matter impurity, keep filtrating, remove ethanol, keeping sample solution.3. get above-mentioned sample solution and add water and heating for dissolving, put coldly,, keep macroporous resin column absorption on the water layer, leave standstill 12h with 2-4 weeding of grease soluble components of petroleum ether extraction.4. use 0%-15% alcoholic solution eluting macroporous resin column colourless to eluent, eluent is collected with the alcoholic solution eluting of 10%-95% in the back, reclaims ethanol, steams to the extractum shape, and vacuum drying is pulverized, and gets Radix Lamiophlomidis Rotatae extract.
The step 1. ethanol extraction solution of described 5%-95% can be weakly alkaline solutions such as ammonia, calcium hydroxide, the sodium carbonate preparation of 7.5-10 with pH value.
Low polar macroporous resin such as D-101 resin etc. during the 3. described macroporous resin of step can be.
Content of total flavone is between 50%-95% in the extract of step described in 4..
Said Radix Lamiophlomidis Rotatae extract is as the analgesia and the application of haemostatic medicament: with the total flavones is active component, is equipped with pharmaceutic adjuvant, can be prepared into any dosage form on the pharmaceutics with known method.
The present invention has investigated optimum extraction process, first high spot reviews the alcoholic solution of weak caustic solutions such as the ammonia of different pH value, calcium hydroxide, sodium carbonate preparations to extracting result's influence.The result shows that the alcoholic solution of different weak base and the preparation of different pH value solution all has very big influence to extracting the result, the rate of transform approximately from 57% be increased to 91%, extraction ratio improves 60% approximately.Use through investigating the method for distilling of being selected for use and extract, the extraction ratio of total flavones and the rate of transform all are higher than the finding bibliographical information in the resulting extract.
This method is convenient and swift, is fit to big production.Because the optimization of method for distilling improves, and has improved the rate of transform of effective ingredient, and then has improved the utilization rate of medical material, has practiced thrift a large amount of production costs effectively, has very high economic benefit.
The specific embodiment
Embodiment 1:
Get Radix Lamiophlomidis Rotatae medical material 2kg, pulverize, cross 20 mesh sieves, adding 20000ml, to use pH value be that the volume fraction of 9 aqua calcis preparation is 5% alcoholic solution, and reflux, extract, 1 hour is filtered and also preserved filtrating, and repetitive operation 4 times merges secondary filtrating, and filtrating concentrates.Get above-mentioned concentrate, with 50% ethanol heating for dissolving, put coldly, remove by filter insoluble impurities, filtrating is revolved and is boiled off ethanol.Get the above-mentioned steaming liquid that revolves, use water dissolution,, keep water layer with petroleum ether extraction four times.Handle the macroporous resin column of (to adorn post behind the 95% soak with ethanol 12h, again with 95% ethanol elution 2-4 volumes, the back is eluted to eluent with distilled water does not have the alcohol flavor) on the mother solution well, flow velocity 1ml/min.It is colourless to be eluted to eluent with a large amount of distilled water, with 10% ethanol elution, 5 volumes, collects 10% alcoholic acid eluent, concentrates and drying, gets Radix Lamiophlomidis Rotatae purification thing, and general flavone content is about 55%.
Embodiment 2:
Get Radix Lamiophlomidis Rotatae medical material 2kg, pulverize, cross 20 mesh sieves, adding 20000ml, to use pH value be that the volume fraction of 8 aqua calcis preparation is 10% alcoholic solution, and reflux, extract, 1 hour is filtered and also preserved filtrating, and repetitive operation 4 times merges filtrating four times, and it is concentrated to filtrate.Get above-mentioned concentrate, with 60% ethanol heating for dissolving, put coldly, remove by filter insoluble impurities, filtrating is revolved and is boiled off ethanol.Get the above-mentioned steaming liquid that revolves, use water dissolution, use the petroleum ether extraction secondary, keep water layer.Handle the macroporous resin column of (to adorn post behind the 95% soak with ethanol 12h, again with 95% ethanol elution 2-4 volumes, the back is eluted to eluent with distilled water does not have the alcohol flavor) on the mother solution well, flow velocity 1ml/min.It is colourless to be eluted to eluent with a large amount of distilled water, takes off 5 volumes with 30% ethanol, collects 30% alcoholic acid eluent, concentrates and drying, gets Radix Lamiophlomidis Rotatae purification thing, and general flavone content is about 66%.
Embodiment 3:
Get Radix Lamiophlomidis Rotatae medical material 2kg, pulverize, cross 20 mesh sieves, adding 20000ml, to use pH value be that the volume fraction of 8 ammonia spirit preparation is 30% alcoholic solution, and reflux, extract, 1 hour is filtered and also preserved filtrating, and repetitive operation 4 times merges filtrating four times, and it is concentrated to filtrate.Get above-mentioned concentrate, with 70% ethanol heating for dissolving, put coldly, remove by filter insoluble impurities, filtrating is revolved and is boiled off ethanol.Get the above-mentioned steaming liquid that revolves, with water dissolution (the about 5mgml of flavones content
-1), with petroleum ether extraction three times, keep water layer.Handle the macroporous resin column of (to adorn post behind the 95% soak with ethanol 12h, again with 95% ethanol elution 2-4 volumes, the back is eluted to eluent with distilled water does not have the alcohol flavor) on the mother solution well, flow velocity 1ml/min.It is colourless to be eluted to eluent with a large amount of distilled water, with 30% ethanol elution, 5 volumes, collects 30% alcoholic acid eluent, concentrates and drying, gets Radix Lamiophlomidis Rotatae purification thing, and general flavone content is about 64%.
Embodiment 4:
Get Radix Lamiophlomidis Rotatae medical material 2kg, pulverize, cross 20 mesh sieves, adding 20000ml, to use pH value be that the volume fraction of 9 aqua calcis preparation is 50% alcoholic solution, and reflux, extract, 1 hour is filtered and also preserved filtrating, and repetitive operation 4 times merges filtrating four times, and it is concentrated to filtrate.Get above-mentioned concentrate, with 50% ethanol heating for dissolving, put coldly, remove by filter insoluble impurities, filtrating is revolved and is boiled off ethanol.Get the above-mentioned steaming liquid that revolves, with water dissolution (the about 5mgml of flavones content
-1), with petroleum ether extraction three times, keep water layer.Handle the macroporous resin column of (to adorn post behind the 95% soak with ethanol 12h, again with 95% ethanol elution 2-4 volumes, the back is eluted to eluent with distilled water does not have the alcohol flavor) on the mother solution well, flow velocity 1ml/min.It is colourless that alcoholic solution with 5% is eluted to eluent, with 50% ethanol elution, 5 volumes, collects 50% alcoholic acid eluent, concentrates and drying, gets Radix Lamiophlomidis Rotatae purification thing, and general flavone content is about 74%.
Embodiment 5:
Get Radix Lamiophlomidis Rotatae medical material 2kg, pulverize, cross 20 mesh sieves, adding 20000ml, to use pH value be that the volume fraction of 9 aqua calcis preparation is 70% alcoholic solution, and reflux, extract, 1 hour is filtered and also preserved filtrating, and repetitive operation 4 times merges filtrating four times, and it is concentrated to filtrate.Get above-mentioned concentrate, with 60% ethanol heating for dissolving, put coldly, remove by filter insoluble impurities, filtrating is revolved and is boiled off ethanol.Get the above-mentioned steaming liquid that revolves, with water dissolution (the about 5mgml of flavones content
-1), with petroleum ether extraction four times, keep water layer.Handle the macroporous resin column of (to adorn post behind the 95% soak with ethanol 12h, again with 95% ethanol elution 2-4 volumes, the back is eluted to eluent with distilled water does not have the alcohol flavor) on the mother solution well, flow velocity 1ml/min.It is colourless to be eluted to eluent with 10% alcoholic solution, with 70% ethanol elution, 5 volumes, collects 70% alcoholic acid eluent, concentrates and drying, gets Radix Lamiophlomidis Rotatae purification thing, and general flavone content is about 82%.
Embodiment 6:
Get Radix Lamiophlomidis Rotatae medical material 2kg, pulverize, cross 20 mesh sieves, adding 20000ml, to use pH value be that the volume fraction of 10 aqua calcis preparation is 90% alcoholic solution, and reflux, extract, 1 hour is filtered and also preserved filtrating, and repetitive operation 4 times merges filtrating four times, and it is concentrated to filtrate.Get above-mentioned concentrate, with 70% ethanol heating for dissolving, put coldly, remove by filter insoluble impurities, filtrating is revolved and is boiled off ethanol.Get the above-mentioned steaming liquid that revolves, with water dissolution (the about 5mgml of flavones content
-1), with petroleum ether extraction four times, keep water layer.Handle the macroporous resin column of (to adorn post behind the 95% soak with ethanol 12h, again with 95% ethanol elution 2-4 volumes, the back is eluted to eluent with distilled water does not have the alcohol flavor) on the mother solution well, flow velocity 1ml/min.It is colourless that alcoholic solution with 15% is eluted to eluent, with 95% ethanol elution, 5 volumes, collects 95% alcoholic acid eluent, concentrates and drying, gets Radix Lamiophlomidis Rotatae purification thing, and general flavone content is about 88%.
Embodiment 7:
Get Radix Lamiophlomidis Rotatae medical material 2kg, pulverize, cross 20 mesh sieves, adding 20000ml, to use pH value be that the volume fraction of 10 sodium carbonate liquor preparation is 90% alcoholic solution, and reflux, extract, 1 hour is filtered and also preserved filtrating, and repetitive operation 4 times merges filtrating four times, and it is concentrated to filtrate.Get above-mentioned concentrate, with 70% ethanol heating for dissolving, put coldly, remove by filter insoluble impurities, filtrating is revolved and is boiled off ethanol.Get the above-mentioned steaming liquid that revolves, with water dissolution (the about 5mgml of flavones content
-1), with petroleum ether extraction four times, keep water layer.Handle the macroporous resin column of (to adorn post behind the 95% soak with ethanol 12h, again with 95% ethanol elution 2-4 volumes, the back is eluted to eluent with distilled water does not have the alcohol flavor) on the mother solution well, flow velocity 1ml/min.It is colourless that alcoholic solution with 15% is eluted to eluent, with 95% ethanol elution, 5 volumes, collects 95% alcoholic acid eluent, concentrates and drying, gets Radix Lamiophlomidis Rotatae purification thing, and general flavone content is about 92%.
Embodiment 8:
The active screening of Duyiwei total flavone effective kind part
Adopt water extraction method to obtain that extract F1 (the 1g extract is equivalent to raw medicinal herbs 4.0g), alkaline alcohol solution extraction method obtain extract F2 (the 1g extract is equivalent to raw medicinal herbs 3.0g), macroporous resin separation and purification method obtains purification thing F3 (the 1g extract is equivalent to raw medicinal herbs 20.9g).Adopt hot plate method and writhing method test model to its pharmacology screening active ingredients that eases pain.
1), acetic acid twisting method
The group one, get kunming mice (20 ± 2g) 50, random packet, experimental mice give water extraction method respectively and obtain extract F1, the alkaline alcohol solution extraction method obtains extract F2 and macroporous resin separation and purification method obtains purification thing F3, wherein F1 290mgkg
-1, F2 390mgkg
-1, F3 56mgkg
-1Positive drug matched group and solvent control group mice give aspirin 100mgkg respectively
-1With with volume distilled water, 10mlkg
-1The volume gastric infusion, successive administration 5 days.
Measure behind the last administration 30min, record is turned round the body number of times in the 15min.
The group two, get kunming mice (20 ± 2g) 50, male and female half and half are divided into 5 groups at random, the macroporous resin separation and purification method that experimental mice gives high, medium and low three dosage respectively obtains purification thing F3, is respectively 112mgkg
-1, 56mgkg
-1, 28mgkg
-1Positive drug matched group and solvent control group mice give aspirin 100mgkg respectively
-1With with volume distilled water, 10mlkg
-1The volume gastric infusion, successive administration 5 days.Measure behind the last administration 30min, record is turned round the body number of times in the 15min.
Experimental data representes that with meansigma methods ± standard deviation significance test adopts one factor analysis of variance between the group of measurement data, relatively adopts the t check in twos, and < 0.05 for there being significant difference, and < 0.01 for there being significant differences, and the result sees table one, table two for P for P.
Acetic acid twisting method experimental result, positive control medicine aspirin has showed tangible analgesic activities under institute's amount of reagent, with the matched group comparing difference highly significant property (P < 0.01) is arranged after the administration.
Experiment has all showed analgesic activities in various degree after the administration of the different process of the clinical equivalent dosage that tries extraction Radix Lamiophlomidis Rotatae composition, and wherein F2 and F3 and matched group comparing difference have highly significant (P < 0.01), and F1 has significance (P < 0.05).Result of the test, the used dosage of Radix Lamiophlomidis Rotatae F3 component testing is lower, and analgesic activity is strong and stable.
Experiment has all showed analgesic activities in various degree behind the Radix Lamiophlomidis Rotatae F3 different experiments dosed administration, and wherein high dose and middle dosage and matched group comparing difference have highly significant (P < 0.01), and low dosage has significance (P < 0.05).
2), hot plate test
Group one, choose pain threshold 50 of the female kunming mices of 5-30s; Be divided into 5 groups at random, experimental mice does not give water extraction method and obtains extract F1, and the alkaline alcohol solution extraction method obtains extract F2; Obtain purification thing F3, wherein F1290mgkg with macroporous resin separation and purification method
-1, F2390mgkg
-1, F356mgkg
-1Positive drug matched group and solvent control group mice give aspirin 100mgkg respectively
-1With with volume distilled water, 10mlkg
-1The volume gastric infusion, successive administration 5 days.
Measure behind the last administration 30min, lick the indicator reaction of metapedes, the time that mice reacts hot plate bitterly after the observation administration for " pain " with mice.
Group two, choose pain threshold 50 of the female kunming mices of 5-30s, be divided into 5 groups at random, the macroporous resin separation and purification method that experimental mice gives high, medium and low three dosage respectively obtains purification thing F3, is respectively 112mgkg
-1, 56mgkg
-1, 28mgkg
-1Positive drug matched group and solvent control group mice give aspirin 100mgkg respectively
-1With with volume distilled water, 10mlkg
-1The volume gastric infusion, successive administration 5 days.
Measure behind the last administration 30min, lick the indicator reaction of metapedes, the time that mice reacts hot plate bitterly after the observation administration for " pain " with mice.
Experimental data representes that with meansigma methods ± standard deviation significance test adopts one factor analysis of variance between the group of measurement data, relatively adopts the t check in twos, and < 0.05 for there being significant difference, and < 0.01 for there being significant differences, and the result sees table three, table four for P for P.
The hot plate method experimental result, positive control medicine aspirin has showed tangible analgesic activities under institute's amount of reagent, with the matched group comparing difference highly significant property (P < 0.01) is arranged behind the medicine.
Experiment has all showed analgesic activities in various degree after the administration of the different process of the clinical equivalent dosage that tries extraction Radix Lamiophlomidis Rotatae composition, and wherein F2 and F3 and matched group comparing difference have highly significant (P < 0.01), and F1 has significance (P < 0.05).Result of the test, the used dosage of Radix Lamiophlomidis Rotatae F3 component testing is lower, and analgesic activity is strong and stable.
Experiment has all showed analgesic activities in various degree behind the Radix Lamiophlomidis Rotatae F3 different experiments dosed administration, and wherein high dose and middle dosage and matched group comparing difference have significance and highly significant (P < 0.01), low dosage unknown significance.
Table 1: different extraction processes get Radix Lamiophlomidis Rotatae extract writhing method analgesic activities experimental result
| Group | Dosage (mgkg -1) | Example number (n) | Turn round the body number of times |
| The solvent contrast | —— | 10 | 25.5±5.5 ? |
| F1 | 290 ? | 10 | 19±5.3* ? |
| F2 | 390 ? | 10 | 15.4±3.3** |
| F3 | 56 | 10 | 16±4.5** |
| Aspirin | 100 ? | 10 | 9.1±2.3** |
Annotate: compare with the solvent matched group
*P<0.05,
*P<0.01.
Table 2: not commensurability Radix Lamiophlomidis Rotatae purification thing writhing method analgesic activities experimental result
| Group | Dosage (mgkg -1) | Example number (n) | Turn round the body number of times |
| The solvent contrast | —— | 10 | 24.3±5.3 ? |
| Low dosage | 28 | 10 | 19.6±3.6* |
| Middle dosage | 56 | 10 | 16.6±3.5** |
| High dose | 112 ? | 10 | 14.5±4.0** |
| Aspirin | 100 ? | 10 | 9.7±2.0** |
Annotate: compare with the solvent matched group
*P<0.05,
*P<0.01.
Table 3: different extraction processes get Radix Lamiophlomidis Rotatae extract hot plate method analgesic activities experimental result
| Group | Dosage (mgkg -1) | Example number (n) | The pain response time |
| The solvent contrast | —— | 10 | 10.57±3.2 ? |
| F1 | 290 ? | 10 | 13.87±2.6* |
| F2 | 390 ? | 10 | 16.41±3.8** ? |
| F3 | 56 | 10 | 15.69±2.7** ? |
| Aspirin | 100 ? | 10 | 20.89±2.87** |
Annotate: compare with the solvent matched group
*P<0.05,
*P<0.01.
Table 4: not commensurability Radix Lamiophlomidis Rotatae purification thing hot plate method analgesic activities experimental result
| Group | Dosage (mgkg -1) | Example number (n) | The pain response time |
| The solvent contrast | —— | 10 | 25.5±5.5 |
| Low dosage | 28 | 10 | 19±5.3 ? |
| Middle dosage | 56 | 10 | 15.4±3.3** |
| High dose | 112 ? | 10 | 16±4.5** |
| Aspirin | 100 ? | 10 | 9.1±2.3** ? |
Annotate: compare with the solvent matched group
*P<0.05,
*P<0.01.
Claims (4)
1. the method for preparing of Tibetan medicine Duyiwei total flavone extract is characterized in that: comprise the steps:
(1) get the Radix Lamiophlomidis Rotatae medical material of drying and crushing, using 6～10 times of concentration is that 90%～95% alcoholic solution extracts, and it is 7.5～10 ammonia, calcium hydroxide or sodium carbonate liquor preparation that alcoholic solution uses PH, and 100 ℃ of reflux, extract, 2-4 time are filtered, and filtrating is concentrated;
(2) get above-mentioned concentrate,, put coldly, remove by filter alcohol insoluble matter impurity, keep filtrating, remove ethanol, keeping sample solution with 50-70% alcoholic solution heating for dissolving;
(3) above-mentioned sample solution adds an amount of and heating for dissolving of water, puts coldly, removes liposoluble constituent 2-4 time with petroleum ether extraction, and macroporous resin column is adsorbed on the reservation water layer; Leave standstill 12h;
(4) colourless to eluent with 15% alcoholic solution eluting macroporous resin column, eluent is collected with 95% ethanol elution in the back, reclaims ethanol, evaporate to dryness to extractum shape, and vacuum drying is pulverized, and gets Radix Lamiophlomidis Rotatae extract.
2. the method for preparing of Tibetan medicine Duyiwei total flavone extract according to claim 1 is characterized in that:
Described macroporous resin is the D-101 resin.
3. the method for preparing of Tibetan medicine Duyiwei total flavone extract according to claim 1 is characterized in that:
Content of total flavone is between 50-95% in this extract.
4. the method for preparing of Tibetan medicine Duyiwei total flavone extract according to claim 1 is characterized in that:
The extractive of general flavone and the pharmaceutically acceptable carrier of preparation are processed acceptable clinically preparation.
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