CN1398869A - Process of extracting tannic acid from Geranium wilfordii root and the use of the extractive - Google Patents
Process of extracting tannic acid from Geranium wilfordii root and the use of the extractive Download PDFInfo
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- CN1398869A CN1398869A CN 02133698 CN02133698A CN1398869A CN 1398869 A CN1398869 A CN 1398869A CN 02133698 CN02133698 CN 02133698 CN 02133698 A CN02133698 A CN 02133698A CN 1398869 A CN1398869 A CN 1398869A
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- tannic acid
- geranium wilfordii
- wilfordii root
- root
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- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 title claims abstract description 46
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- 239000000243 solution Substances 0.000 claims description 9
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 6
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- 239000008215 water for injection Substances 0.000 description 6
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- CUBCNYWQJHBXIY-UHFFFAOYSA-N benzoic acid;2-hydroxybenzoic acid Chemical compound OC(=O)C1=CC=CC=C1.OC(=O)C1=CC=CC=C1O CUBCNYWQJHBXIY-UHFFFAOYSA-N 0.000 description 4
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- JGSARLDLIJGVTE-UHFFFAOYSA-N 3,3-dimethyl-7-oxo-6-[(2-phenylacetyl)amino]-4-thia-1-azabicyclo[3.2.0]heptane-2-carboxylic acid Chemical compound O=C1N2C(C(O)=O)C(C)(C)SC2C1NC(=O)CC1=CC=CC=C1 JGSARLDLIJGVTE-UHFFFAOYSA-N 0.000 description 2
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- Medicines Containing Plant Substances (AREA)
Abstract
An extraction process of tannic acid from Geranium wilfordii tuber root as raw material includes washing, drying, crushing to 0.2-5 mm granules, extracting by adding water of 3-10 times the material weight or ethanol of 30-90 vol% concentration at 20-70 deg.C, filtering the extracted liquid, concentrating the filtrate to obtain clear cream, water or alcohol deposition, laying a side at 2-8 deg.C, centrifugating, filtering, concentrating the filtrate while recovering ethanol, spray drying or vacuum drying the concentrated liquid to obtain the product with tannic acid content over 50%. The extractive of the present invention has obvious effects of resisting inflammation, stopping pain, stopping bleeding, etc..
Description
Technical field:
What the present invention relates to is a kind of extracting method of efficient part tannic acid and purposes of extract thereof extracted from Chinese medicinal materials Herba Erodii piece root.
Background technology:
Herba Erodii is a kind of conventional Chinese medicine material.Chinese Pharmacopoeia (2000 editions, one one) the Herba Erodii kind recorded is yak seedling section plant yak (Erodium Stephanianum Willd), Herba Erodii (Geranium wilfordii Maxim) or Carolina Cranesbill Herb (Geranium Carolinianum L.) dry aerial parts, has the function of wind-damp dispelling, the meridian dredging, antidiarrheal dysentery.Be mainly used in rheumatic arthralgia, numbness contracture, muscles and bones is ached, illnesss such as dysentery.Main preparation is unguentum geranii (functions such as anti-inflammatory, detoxifcation, convergence, myogenic).
The western Sichuan minority area, the piece root portion of Herba Erodii commonly used among the people (drying, abrasive dust) is anti-treats for stomachache and single proved recipe of pharyngolaryngitis.Use inconvenience, and curative effect is not remarkable.
Summary of the invention:
The objective of the invention is in order to provide a kind of easy to use, have the extracting method of tannic acid from Geranium wilfordii root of effects such as significant anti-inflammatory, pain relieving, hemostasis and the purposes of extract thereof.
The object of the present invention is achieved like this:
Extracting method of the present invention is that the underground part piecemeal root of employing Herba Erodii is a raw material, the particulate state that it is clean, dry, as to be ground into 0.2～5mm, in addition consumption be 3～10 times water of raw material weight or concentration expressed in percentage by volume be 30～90% ethanol 20～70 ℃ down warm lixiviates get, extracting solution is filtered, concentrating filter liquor is to clear paste, again through depositing in water or alcohol precipitation, in 2～8 ℃ of placements, through centrifugal, filtration, filtrate is through reclaiming ethanol, concentrate, and the spray-dried or vacuum-drying of concentrated solution makes the tannic acid from Geranium wilfordii root extract of tannic acid content 〉=50%.
Above-mentioned water or ethanol consumption are 4～8 times of raw material weight, and the alcoholic acid concentration expressed in percentage by volume is 50～60%, and leaching temperature is 40～50 ℃, and extraction effect is better.
Above-mentioned Herba Erodii is adopted piece root Herba Erodii or a high mountain mutation Herba Erodii or a husky Herba Erodii.
It is 1～3% the aqueous solution that the above-mentioned tannic acid from Geranium wilfordii root extract that contains tannic acid content 〉=50% is mixed with concentration expressed in percentage by weight with water, by being housed, handles large pore macromolecular polymeric adsorbent adsorption column, after distilled water drip washing, the employing concentration expressed in percentage by volume is 30～95% ethanol elution, elutriant makes the high purity tannic acid from Geranium wilfordii root extract of tannic acid content 〉=80% through ethanol, recovery, concentrated, spray-dried or vacuum-drying, can be used as the injection preparation raw material.
The above-mentioned aqueous solution concentration expressed in percentage by weight that is mixed with is 1～5%.
Above-mentioned large pore macromolecular polymeric adsorbent is the multipolymer of Vinylstyrene and nitrogenous polar monomer, as Vinylstyrene or strong polar Vinylstyrene or the strong polar Vinylstyrene and the monomeric multipolymer of nitrogenous property (GD * 403 of adopting middle polarity; 501; 601) multipolymer of Vinylstyrene that polarity is stronger and nitrogenous polar monomer (C101 or C102, D101 or D102
The purposes of tannic acid from Geranium wilfordii root extract of the present invention is to be used to prepare anti-inflammatory, pain relieving, hematostatic medicament.
Above-mentioned medicament is to carry tablet, capsule, oral liquid, vina, granule, the injection liquid that thing is mixed with tannic acid from Geranium wilfordii root.
The used Herba Erodii of the present invention is meant piece root Herba Erodii (Geraniumdahuricum D.C) or high mountain mutation Herba Erodii (G.dahuricum D.Cvar alpinum Bar etSKV) or a husky Herba Erodii (the G.yezoense Francl et Sav that non-pharmacopeia is recorded.) underground root portion.With Herba Erodii piece root is raw material, puies forward the heavy method technology of an alcohol (water) with water (or ethanol) and extracts efficient part (tannic acid is higher than 50%) or further refining with the large pore macromolecular polymeric adsorbent, prepares high-quality extract; And be equipped with new pharmaceutical excipient according to a conventional method respectively combined preparation become tablet, capsule, oral solutions, granule or injection etc.
Introduce the extract pharmaceutical excipient new that adopts extracting method of the present invention to extract below and make up the peaceful craft screening effect experiment report of the gastritis of making for the pharmaceutical preparation composition is equipped with.
1, experiment purpose
By the peaceful extract of gastritis and the dregs of a decoction thereof, mouse analgesic test and Whitfield's ointment are caused observation, the analysis of rat acute gastritis model, for the preparation process screening provides the pharmacodynamics foundation.
2, experiment condition
Three grades of Animal Lab.s, 20～25 ℃ of room temperatures, air-conditioning constant temperature.
3, experiment material
The peaceful extract of gastritis, the dregs of a decoction provide by the Drug Manufacturing Room of the hospital of traditional Chinese hospital of Sichuan Institute of Tradition Chinese Medicine.During test, add the suspension that an amount of tragcanth is mixed with 8% concentration.
Zhushalian Capsule, big thousand pharmaceutcal corporation, Ltds in Leshan, Sichuan, lot number: 000708, during test, be mixed with suspension.
Kunming mouse, the SD rat provides by Sichuan Province's antibiotic industrial research institute Experimental Animal Center, and the dispensing feed, conformity certification number: 99-30,99-32
4, experimental technique
4.1 analgesic activity (acetic acid twisting method) to mouse
Choose 40 of body weight 18-22 gram Kunming mouses, male and female half and half, be divided into four groups such as distilled water group, Zhushalian Capsule group, the peaceful extract group of gastritis, dregs of a decoction group at random, gavage administration 0.5ml/20g, behind the medicine 30 minutes, the equal abdominal injection 0.5% acetum 0.2ml/ of each mouse only observes that writhing response mouse number of elements appears in each group in 10 minutes, calculates each medicine percentage that eases pain.The results are shown in Table 1.
The peaceful extract of table 1 gastritis and the dregs of a decoction thereof are to the analgesic activity (writhing method) of mouse (XSD)
Group dosage number of animals writhing response is counted analgesia rate P value
(g/kg) (only) (inferior) (%)
Distilled water group--10 30.1 ± 10.0----
Zhushalian Capsule group 2.0 10 14.0 ± 5.0 53.49＜0.001
The peaceful extract group 2.0 10 11.4 of gastritis ± 4.6 62.13＜0.001
Dregs of a decoction group 2.0 10 23.1 ± 7.0 23.26＞0.05
The result: table 1 result shows, the number of times that the peaceful extract of gastritis has obvious inhibition acetic acid induced mice writhing response to take place compares P＜0.001 with the distilled water control group.Dregs of a decoction Dichlorodiphenyl Acetate induced mice writhing response frequency has inhibition, but compares with the distilled water control group, learns by statistics and handles its P of no significant difference＞0.05.
4.2 Whitfield's ointment is caused the influence of rat acute gastritis model
Choose 80 of body weight 150g ± 20g rat, every group each 10, male and female half and half.Establish the normal control group respectively, model group, the peaceful extract group of gastritis (8%), four groups such as dregs of a decoction group with the 1m/100g body weight, gavage administration, normal group model group distilled water, continuous 10 days, fasting was 24 hours in the 9th day, administration is 1 time again, uses 20mmol/L Whitfield's ointment (0.05% Xylo-Mucine) suspension oral gavage, dosage 100mg/kg after 1 hour, put to death animal after 4 hours, take out full stomach, fix 15 fens with 10% formaldehyde solution and cut off after the kind, observe the gastritis situation.Judge classification: "-" no gastritis takes place: "+" contrafluxion, and mild inflammation: " ++ " is serious congested, and local inflammation is obvious; " +++" the visible diffuse inflammation variation of full stomach.Be designated as 0,1,2,3 fen respectively.The results are shown in Table 2.
Acid causes the influence of rat gastritis model to water for the peaceful extract of table 2 gastritis and the dregs of a decoction thereof
The scoring of group dosage number of animals gastritis
(g/kg) (only)
Normal group--10 0
Model group--10 20
The peaceful extract group 0.8 10 2 of gastritis
Dregs of a decoction group 0.8 10 14
The result: table 2 is the result show, the peaceful extract of gastritis has very significant protective effect to the acid gastritis of bigcatkin willow.
5, conclusion
The firstfruits of above-mentioned two pharmacodynamic experiments shows: the pain of the peaceful extract Dichlorodiphenyl Acetate of gastritis induced mice writhing response, analgesic effect (P＜0.001) is arranged, and Whitfield's ointment is caused rat gastritis model significant protective effect; And the dregs of a decoction aspect these two in, analgesic activity and provide protection are all not obvious.
Show through preliminary toxicology, pharmacodynamic study: extract of the present invention and preparation have effects such as tangible anti-inflammatory, pain relieving, hemostasis.For further new drug research provides rational processing method.Easy to use.
Embodiment:
Embodiment 1:
The extraction of water-soluble efficient part:
Take by weighing and purify, exsiccant Herba Erodii piece root 5kg is ground into coarse grain (0.3-2mm) adding distil water 25000ml and soaks, and be incubated 50 ℃, stirs and leaches 2 hours, and suction filtration goes out immersion liquid; In the dregs of a decoction, add 25000ml distilled water (extracting repeatedly three times) again; Merge three times filtrate, filtrate pumps into vacuum concentration pot, through vacuum concentration (0.085Mpa; 50 ℃) to clear paste (medicinal material weight: concentrated solution weight=24～1: 1), add 5000-10000ml.95% ethanol after stirring evenly, was placed 24 hours in low temperature (2-8 ℃); Incline and get supernatant liquid, filter (or centrifugal), filtrate is through decompression recycling ethanol (0.085Mpa; 30-40 ℃), be concentrated into 5000ml (proportion 1.05-1.08).The spray-dried brown ceramic powder 0.8-1.2kg (containing tannic acid 50-60%) that gets of concentrated solution.
Embodiment 2:
The extraction of alcohol dissolubility efficient part.
Take by weighing purify, dry Herba Erodii piece root 5kg, be ground into coarse particles shape (0.3-2mm) and add 60% (V/V) ethanol 25000ml and soak, be incubated 40 ℃, stir leaching 1.5 hours, the extraction leach liquor; In the dregs of a decoction, add 25000ml 60% ethanol (three times repeatedly) again; Merge three times and leach immersion liquid, filtrate pumps in the vacuum concentration pot, decompression recycling ethanol (0.085Mpa; 30-40 ℃), be concentrated into (1: 1), about 5000ml adds distilled water 10000ml mixing; (2-8 ℃) placed 24 hours; Centrifugal (4000prm), filtration, filtrate is through concentrating under reduced pressure (0.085mMpa; 50-60 ℃), be concentrated into 5000ml (proportion 1.05-1.08).Concentrated solution is spray-dried, gets brown ceramic powder 0.7-0.9kg (containing tannic acid 50-60%).
Embodiment 3:
The preparation of high-content Herba Erodii piece root efficient part:
Herba Erodii efficient part (the containing tannic acid 50-60%) 100g that gets [embodiment 1] preparation adds distilled water 1000-2000ml, abundant stirring and dissolving, and low temperature (2～8) was placed 24 hours; Solution is got supernatant liquid through centrifugal (4000prm), filters; In large pore macromolecular polymeric adsorbent (D101) post that handled filtrate adding; Pass through resin column by flow velocity (500ml/ hour); Is colourless with distilled water drip washing (flow velocity 500-1000ml/ hour) to leacheate; With 60% ethanol eluate (flow velocity 500ml/ hour) wash-out, collect elutriant (is faint yellow to flowing out elutriant) again.Elutriant is through decompression recycling ethanol (0.085mpa; 30-40 ℃), (0.085mpa; 50-60 ℃), spraying drying gets brown ceramic powder (tannic acid content 〉=80%).
Embodiment 4:
The preparation of the capsule of treatment chronic gastritis
Herba Erodii piece root efficient part powder or the particle (dry granulation) of getting (embodiment 1 or 2) extraction directly incapsulate in the portioning machine; Quantitatively packing, make.[every capsules contains effective position (tannic acid) 0.2g].
Embodiment 5:
The preparation of treatment acute pharyngolaryngitis buccal tablet
Get Herba Erodii piece root efficient part (powder) 100g that (embodiment 1 or 2) extracts, add Icing Sugar 500g and dextrin 100g.Make particle by well-established law; After the drying, sift out the parts of fine particle, admix ethanolic soln (0.75g and the 0.5g) mixing of spearmint oil brain and peppermint, again this powder and other particles and Magnesium Stearate are mixed; The particle compressing tablet, every contains effective position 0.1g.
Embodiment 6:
The injection liquid preparation of treatment hemorrhoid and underarm odor
Prescription:
The extract of Herba Erodii (containing tannic acid 50%) 400g
EDTA-Na (Na2EDTA salt) 3g
Water for injection 1000ml
Method for making:
Take by weighing EDTA-2Na3g, add water for injection 600ml, stirring makes dissolving fully, take by weighing Herba Erodii extract (containing tannin 50%) 400g again, mixing stirs and makes dissolving fully (in case of necessity, 60 ℃ of heating in the water-bath) after, add water for injection to 1000ml, mixing is after behind the glass sand-bed filter (G3 and G6), secondary filter, filtrate quantitatively (1ml) can in ampoule or cillin bottle.After cryogenic freezing, place in the freeze drier lyophilize 24 hours.The sealing by fusing ampoule (or the lid rubber plug, aluminium lid, tying), promptly get powder injection (every bottle contains the tannic acid amount is 0.2g).
Embodiment 7:
The injection liquid preparation of treatment hemorrhoid and underarm odor
Contain the preparation of compound tannic acid powder injection
Prescription:
Galla Chinensis extract (containing tannic acid 80%) 62.5-187.5g
Herba Erodii extract (containing tannic acid 50%) 100-300g
EDTA-2Na 3g
Water for injection adds to 1000ml
Method for making:
Take by weighing EDTA-2Na3g, add among the water for injection 600ml, stirring makes the Turkey-galls effective part extract that adds a certain proportion of (weight ratio) after the dissolving respectively and Herba Erodii effective part extract (generally by 125: 200,178.5: 100 or 62.5: 300), heating (50-60 ℃) is stirred and is made dissolving fully in water-bath, add and add to the full amount of water for injection, placed liquid in low temperature (2-8 ℃) behind the mixing, next day, centrifugal (4000prm) and with glass sand-bed filter (G3, G6) filter, filtrate quantitatively (0.5-1ml) is filled into ampoule (or in cillin bottle), after cryogenic freezing, place in the freeze drier (cold-trap coil temperature-35-40 ℃ of lyophilize 24 hours, highest attainable vacuum 20pa) sealing by fusing ampoule (or gag, tying) promptly.
(every dose contains tannic acid 0.1-0.2g)
Claims (10)
1, the extracting method of tannic acid from Geranium wilfordii root, it is characterized in that adopting the underground part piecemeal root of Herba Erodii is raw material, it is cleaned, dry, be ground into the particulate state of 0.2～5mm, in addition consumption be 3～10 times water of raw material weight or concentration expressed in percentage by volume be 30～90% ethanol 20～70 ℃ down warm lixiviates get, extracting solution is filtered, concentrating filter liquor is to clear paste, again through depositing in water or alcohol precipitation, in 2～8 ℃ of placements at least 24 hours, through centrifugal, filter, filtrate is through reclaiming ethanol, concentrate, the spray-dried or vacuum-drying of concentrated solution makes the tannic acid from Geranium wilfordii root extract of tannic acid content 〉=50%.
2, the extracting method of tannic acid from Geranium wilfordii root according to claim 1 is characterized in that water or ethanol consumption are 4～8 times of raw material weight, and the alcoholic acid concentration expressed in percentage by volume is 50～60%, and leaching temperature is 40～50 ℃.
3, the extracting method of tannic acid from Geranium wilfordii root according to claim 1 and 2 is characterized in that Herba Erodii employing piece root Herba Erodii or high mountain mutation Herba Erodii or the old stork of husky head.
4, the extracting method of tannic acid from Geranium wilfordii root according to claim 1 and 2, it is 1～20% the aqueous solution that the tannic acid from Geranium wilfordii root extract that it is characterized in that tannic acid content 〉=50% is mixed with concentration expressed in percentage by weight with water, by being housed, handles large pore macromolecular polymeric adsorbent adsorption column, after distilled water drip washing, adopting concentration expressed in percentage by weight is 30～95% ethanol elution, and elutriant makes the high purity tannic acid from Geranium wilfordii root extract of tannic acid content＞80% through ethanol elution, recovery, concentrated, spray-dried or vacuum-drying.
5, the extracting method of tannic acid from Geranium wilfordii root according to claim 4 is characterized in that the aqueous solution concentration expressed in percentage by weight that is mixed with is 1～5%.
6, the extracting method of tannic acid from Geranium wilfordii root according to claim 4 is characterized in that the large pore macromolecular polymeric adsorbent is the multipolymer of Vinylstyrene and nitrogenous polar monomer.
7, the purposes of the tannic acid from Geranium wilfordii root extract of the extracting method of employing claim 1 or 2 described tannic acid from Geranium wilfordii root extraction is characterized in that being used to prepare anti-inflammatory, pain relieving, hematostatic medicament.
8, the purposes of tannic acid from Geranium wilfordii root extract according to claim 7 is characterized in that medicament is to carry tablet, capsule, oral liquid, vina, granule, the injection liquid that thing is mixed with tannic acid from Geranium wilfordii root.
9, the purposes of the tannic acid from Geranium wilfordii root extract of the extracting method extraction of the described tannic acid from Geranium wilfordii root of employing claim 4 is characterized in that being used to prepare anti-inflammatory, pain relieving, hematostatic medicament.
10, the purposes of the extract of tannic acid from Geranium wilfordii root according to claim 9 is characterized in that medicament is tablet, capsule, oral liquid, vina, granule, the injection liquid that is mixed with the tannic acid from Geranium wilfordii root extract.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021336989A CN1159326C (en) | 2002-09-03 | 2002-09-03 | Process of extracting tannic acid from Geranium wilfordii root and the use of the extractive |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB021336989A CN1159326C (en) | 2002-09-03 | 2002-09-03 | Process of extracting tannic acid from Geranium wilfordii root and the use of the extractive |
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| CN1398869A true CN1398869A (en) | 2003-02-26 |
| CN1159326C CN1159326C (en) | 2004-07-28 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1313475C (en) * | 2003-04-22 | 2007-05-02 | 上海大学 | Method for extracting polygonum cuspidatum tannic acid |
| EP2086561A4 (en) * | 2006-11-15 | 2010-05-12 | Arthritis Relief Plus Ltd | Topical formulation and uses thereof |
| CN107158071A (en) * | 2017-06-05 | 2017-09-15 | 云南摩尔农庄生物科技开发有限公司 | A kind of preparation method of walnut tannin |
-
2002
- 2002-09-03 CN CNB021336989A patent/CN1159326C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1313475C (en) * | 2003-04-22 | 2007-05-02 | 上海大学 | Method for extracting polygonum cuspidatum tannic acid |
| EP2086561A4 (en) * | 2006-11-15 | 2010-05-12 | Arthritis Relief Plus Ltd | Topical formulation and uses thereof |
| EP3284470A1 (en) * | 2006-11-15 | 2018-02-21 | Arthritis Relief Plus Ltd. | Topical formulation comprising comfrey extract |
| US10322155B2 (en) | 2006-11-15 | 2019-06-18 | Arthritis Relief Plus Ltd. | Topical formulation and uses thereof |
| US11844820B2 (en) | 2006-11-15 | 2023-12-19 | Arthritis Relief Plus Ltd. | Topical formulation and uses thereof |
| CN107158071A (en) * | 2017-06-05 | 2017-09-15 | 云南摩尔农庄生物科技开发有限公司 | A kind of preparation method of walnut tannin |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1159326C (en) | 2004-07-28 |
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