CN101332216B - Xingsiang Tuerfeng total phenolic acid extract and preparation method thereof - Google Patents
Xingsiang Tuerfeng total phenolic acid extract and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an extract of frangrant ainsliaea herb total phenolic acids and the preparation method thereof, after the medicinal materials of frangrant ainsliaea herb are extracted by 70% ethanol through reflux, the ethanol extract is concentrated to small volume and the ethanol content in the solution is controlled to be 20% - 40%, after the pH is adjusted to be 1-3 by hydrochloric acid, the solution stands still and is filtered, then the solution is clear and concentrated, the material obtained is put on a macroporous absorption resin column and eluted by ethanol after washed, and then ethanol eluent is collected, concentrated and dried, thus the extract of the invention is obtained. The content of total phenolic acids in the extract can be up to over 60%, and the chlorogenic acid in the extract can be more than 3%. The extract of the invention has the effects of antiinflammatory action and can be used for preparing the drugs that can treat gynae phlegmasia.
Description
Technical field
The present invention relates to a kind of Xingsiang Tuerfeng total phenolic acid extract and preparation method thereof, belong to natural drug effective ingredient preparation field.
Background technology
Ainsliasa fragrans Champ (Ainsliaea fragrans Champ.) is a Compositae Ainsliaea fragrans Champ. platymiscium; Have effects such as heat-clearing and toxic substances removing, dampness removing, hemostasis; Among the people with all herbal medicine; Be used to treat illness such as pulmonary tuberculosis haematemesis, traumatic injury, nameless gall, cavity inflammation, edema, chronic cervicitis, for " Jiangxi Province's Chinese crude drug standard " version in 1996 is recorded, its patent medicine compound recipe Ainsliasa fragrans Champ granule and sheet are Chinese medicine protection kind.There is report that golden Portugal bacterium, group B streptococcus, poliovirus, simple cellulitis exanthema virus (HSV-1), Measles virus etc. are had inhibitory action.
Modern study shows; The Ainsliasa fragrans Champ medical material contains compositions such as phenols, flavonoid, organic acid, sesquiterpene lactones class, triterpenes; Comprising chlorogenic acid, caffeoylquinic acids, freidelin ketone, lacceroic acid, cupreol, flavone compound Ramulus et Folium Tamaricis element and glycosides thereof etc.; Wherein phenolic acid compound is its effective antiviral ingredients, the quality control index of chlorogenic acid Chang Zuowei Ainsliaea fragrans Champ..In the existing dosage form, Ainsliaea fragrans Champ. often is the direct unit's of processing mechanism after the thick step extracts, and day dose is big.In the one Chinese patent application 200510087008.7; A kind of method for preparing the Ainsliaea fragrans Champ. total organic acids is disclosed; What it adopted is in concentrated solution, to add hydrochloric acid accent pH after water extraction concentrates, and in the Ainsliaea fragrans Champ. medical material, has the less relatively organic liposoluble ingredient of some agent property; Free back dissolubility is not that fine, such extraction operation can cause some loss of active ingredients in water.
Summary of the invention
The object of the present invention is to provide a kind of method for preparing Xingsiang Tuerfeng total phenolic acid extract; When extracting, the present invention adopts ethanol extraction; Recovery liquid after the extraction adds hydrochloric acid and transfers pH to make liposoluble ingredient therefrom free and be dissolved in the alcoholic solution under the situation that contains ethanol about 30%; Overcome some polar phase are difficult for being dissolved in edema to less liposoluble ingredient and with the defective of deposition loss, and final extract yield is high, phenolic content also improves a lot in the extract.
Ainsliasa fragrans Champ phenolic acids preparation method of extract of the present invention can prepare through following mode and gets, and the dry medical material of Ainsliasa fragrans Champ is ground into coarse powder, with the ethanol extraction of 40%-70%, filters; Get filtrating, filtrate decompression concentrates, and adding ethanol, to make the solution concentration of alcohol be 20%-40%, and every ml soln is equivalent to crude drug 0.8-1.0g; In solution, add hydrochloric acid accent pH to 1.0-3.0, leave standstill, placed 12-24 hour at cold place, centrifugal or filtration; Get clear liquid, clear liquid is evaporated to does not have alcohol, and the dissolving of concentrate adding distil water disperses, with on the disperse object with on the macroporous adsorptive resins of handling well; It is thin out earlier to be eluted to the water lotion color with deionized water, uses the aquiferous ethanol eluting instead, is negative to the phenolic acid chromogenic reaction, collects ethanol elution; Merge, concentrating under reduced pressure, drying promptly gets the Ainsliaea fragrans Champ. phenolic acid extract.
Among the present invention, when transferring pH to make phenolic acid free fully with hydrochloric acid, preferably pH is transferred to about 1.0.
Among the present invention, the used filler of macroporous adsorptive resins can be selected from AB-8 type, NKA-9 type, D-101 type, HP-20 type macroporous resin, and during the eluting resin column, employed ethanol is preferably 70% ethanol.
Adopt the inventive method to prepare in the resulting Ainsliasa fragrans Champ extract, the total phenolic content of extract comprises organic phenolic acid and some flavones ingredients greater than 60% in total phenolic acid; Extract is in chlorogenic acid, and chlorogenic acid contents is not less than 1%, and its content range is between 1%～5%; The difference of its content is looked medical material and the difference in the different places of production, and the present invention adopts Jiangxi to produce Ainsliasa fragrans Champ, and chlorogenic acid content is about 0.25% in its medical material; In extract obtained, chlorogenic acid content is about 3.6%.
Among the present invention, the medical material that extracts total phenolic acids composition is except that can also being other Ainsliaea fragrans Champ. medical material during Ainsliaea fragrans Champ. belongs to for the Ainsliasa fragrans Champ.
Extract of the present invention has the antiviral effect of antiinflammatory, can be used for preparing having the medicine that antiinflammatory is seen virus.
The concrete extraction scheme of Ainsliasa fragrans Champ medical material effective ingredient is:
Get the dry medical material 1000g of Ainsliasa fragrans Champ, be ground into coarse powder, add 70% the alcohol reflux 3 times of 8 times of amounts, each 1.5 hours; Filter, merge each time and extract filtrating, 60 ℃ of concentrating under reduced pressure add ethanol and transfer in the concentrated solution; Make medicinal liquid finally contain the alcohol amount and be about 30%, every milliliter of medicinal liquid is equivalent to the about 0.9g of Ainsliasa fragrans Champ crude drug, and the hydrochloric acid that adds 1N then transfers pH to pH to be about 1.0, stirs; Room temperature was placed 18 hours, and is centrifugal, gets supernatant, and supernatant continues to be evaporated to does not have alcohol; With the AB-8 type macroporous absorption fat post of having handled well on the concentrate, it is thin out to be eluted to water elution liquid color with deionized water earlier, uses 70% ethanol elution instead; Be negative to the FeCl3 chromogenic reaction, merge 70% ethanol elution part, concentrating under reduced pressure; Vacuum drying gets Ainsliasa fragrans Champ phenolic acid extract 51.3g, and method prepares three lot sample article according to this.
The mensuration of chlorogenic acid content in the extract.
The chromatographic condition chromatographic column: the DiamonsilTMC18ODS post (5 μ m, 200mm * 4.6mm), and mobile phase: methanol-2% glacial acetic acid (20: 80), flow velocity 1ml/min detects wavelength 327nm, and column temperature: 25 ℃, theoretical cam curve must not be lower than 3000. by chlorogenic acid
The configuration of the preparation reference substance solution of reference substance, test sample: it is an amount of that precision takes by weighing the chlorogenic acid reference substance, puts in the brown volumetric flask, adds 50% methanol and process every milliliter and contain 30 μ g chlorogenic acids; The configuration of need testing solution: precision takes by weighing Ainsliasa fragrans Champ extract 0.1g, puts in the 100ml volumetric flask, and add dissolve with methanol and be settled to scale, filtering with microporous membrane, subsequent use.
Chlorogenic acid content in each batch of sequentially determining extract, the result sees table 1
Determination of chlorogenic acid result in three batches of Ainsliasa fragrans Champ extract of table 1
Batch chlorogenic acid content
Ainsliasa fragrans Champ medical material 0.257%
Ainsliasa fragrans Champ extract one 3.82%
Ainsliasa fragrans Champ extract 2 3.49%
Ainsliasa fragrans Champ extract 3 3.58%
The average content of chlorogenic acid in extract is 3.63% in the three lot sample article.
The mensuration of total phenolic content in the extract.
The drafting of standard curve: precision takes by weighing in protocatechualdehyde reference substance 10.4mg to the 50ml volumetric flask that is dried to constant weight, adds anhydrous alcohol solution, is diluted to scale.Draw 0.2,0.4,0.6,0.8 respectively, in 1.0mL to the 10mL volumetric flask, add dehydrated alcohol, add 0.3% sodium lauryl sulphate 0.8mL and 0.6% ferric chloride-0.9% potassium ferricyanide (1: 0.9) mixed solution 0.4mL more respectively to 2mL; Mixing is in the dark placed 5min, and the HCl solution that adds 0.1mol/L is to scale; 20min is placed in the dark place, and the retinue ethanol solution is done blank, with ultraviolet-visible spectrophotometer in the 500nm place sequentially determining absorbance; Each concentration trap is followed successively by 0.122,0.256,0.376,0.498,0.621, is abscissa with concentration, and trap is a vertical coordinate drawing standard curve; Regression equation is A=0.024C+0.0026; A is a trap, and C is a concentration, R=0.9998.Curve such as accompanying drawing 6
The preparation of sample solution: precision takes by weighing Ainsliasa fragrans Champ extract 40.2,40.8,40.5mg, puts in the 50mL volumetric flask, and anhydrous alcohol solution also is settled to scale; Cross 0.5 μ m microporous filter membrane; Subsequent use, each accurate absorption in 0.5mL to the 10mL volumetric flask of three duplicate samples, process color is handled with reference substance; Measure its trap with the 500nm place, calculate total phenolic content.The assay result sees table 1
The total phenolic content of three batches of extracts of table 1 is measured the result
The average content of total phenolic acid extract is 65.77% in the three lot sample article extracts.
Description of drawings
Fig. 1 is a chlorogenic acid reference substance liquid chromatogram of the present invention;
Fig. 2 is an Ainsliasa fragrans Champ liquid chromatogram of the present invention;
Fig. 3 is first Xingsiang Tuerfeng total phenolic acid extract liquid chromatogram of the present invention;
Fig. 4 is second batch of Xingsiang Tuerfeng total phenolic acid extract liquid chromatogram of the present invention;
Fig. 5 is the 3rd batch of Xingsiang Tuerfeng total phenolic acid extract liquid chromatogram of the present invention;
Fig. 6 is a protocatechualdehyde ultraviolet-visible spectrophotometric canonical plotting.
Specific embodiment
Below prepare embodiment simple declaration the present invention from extract, but cited embodiment is not meant to limit the present invention embodiment.
Embodiment 1
Get the dry medical material 1000g of Ainsliasa fragrans Champ, be ground into coarse powder, add 40% the alcohol reflux 3 times of 10 times of amounts, each 2 hours; Filter, merge each time and extract filtrating, 60 ℃ of concentrating under reduced pressure add ethanol and transfer in the concentrated solution; Make medicinal liquid finally contain the alcohol amount and be about 20%, every milliliter of medicinal liquid is equivalent to the about 1.0g of Ainsliasa fragrans Champ crude drug, and the hydrochloric acid that adds 1N then transfers pH to pH to be about 2.0, stirs; Room temperature was placed 24 hours, and is centrifugal, gets supernatant, and supernatant continues to be evaporated to does not have alcohol; With the NKA-9 type macroporous absorption fat post of having handled well on the concentrate, it is thin out to be eluted to water elution liquid color with deionized water earlier, uses 60% ethanol elution instead, to FeCl
3Chromogenic reaction is negative, and merges 60% ethanol elution part, concentrating under reduced pressure, and vacuum drying gets Ainsliasa fragrans Champ phenolic acid extract 55.7g.
Embodiment 2
Get the dry medical material 1000g of Ainsliaea fragrans Champ., be ground into coarse powder, add 60% the alcohol reflux 3 times of 12 times of amounts, each 1 hour; Filter, merge each time and extract filtrating, 60 ℃ of concentrating under reduced pressure add ethanol and transfer in the concentrated solution; Make medicinal liquid finally contain the alcohol amount and be about 40%, every milliliter of medicinal liquid is equivalent to the about 0.8g of Ainsliasa fragrans Champ crude drug, and the hydrochloric acid that adds 1N then transfers pH to pH to be about 1.5, stirs; Room temperature was placed 12 hours, and is centrifugal, gets supernatant, and supernatant continues to be evaporated to does not have alcohol; With the HP-20 type macroporous absorption fat post of having handled well on the concentrate, it is thin out earlier to be eluted to water elution liquid color with deionized water, uses 70% ethanol elution instead, is negative to the FeCl3 chromogenic reaction; Merge 70% ethanol elution part, concentrating under reduced pressure, vacuum drying gets Ainsliasa fragrans Champ phenolic acid extract 48.7g.
Embodiment 3
Effect to rat chronic pelvic inflammatory disease due to the escherichia coli
40 of Wister rats are divided into four groups at random, are followed successively by sham operated rats, model group, Xingsiang Tuerfeng total phenolic acid extract group and FUKE QIANJIN PIAN group, and the Ainsliasa fragrans Champ dosage is 60mg/kg.d
-1, administration every day 1 time, successive administration 21 days is measured the rat immunity function then and is carried out the rat uterus morphological observation, and the result shows, Xingsiang Tuerfeng total phenolic acid extract administration 60mg/kg.d
-1, it is 85.8 ± 1.7 that agglutinin is tired, and compares with model group (36.9 ± 1.7), the rat blood serum agglutinin is tired and is significantly raise P＜0.01; Extract administration group lymphocyte transformation index of the present invention is 1.6 ± 0.6, compares with model group 1.2 ± 0.2, has significant difference, P＜0.01, and the lymphocyte transformation index obviously improves.
Tectology is observed and is found; Model group perusal uterus swelling, harden,, form scleroma with the surrounding tissue adhesion; See palace wall mucosa and flesh layer structural fuzzy under the mirror; Most epithelial cell degeneration necrosis come off, and wall each layer tissue congestion and edema in palace is followed a large amount of eosinophilic granulocytes and a small amount of lymphocyte cellular infiltration, has volume fibroblast proliferation administration group rat chronic pelvic inflammatory disease pathological change obviously to alleviate in mucous layer, the flesh layer; Ainsliasa fragrans Champ 60mg/kg.d
-1Group, naked eyes are seen the uterus and are increased slightly, and each layer of palace wall structure is still clear under the mirror, the minority epithelial cell shedding, and the congestion and edema companion of inner membrance shallow layer tissue moderate the eosinophilic granulocyte soak into, and the minute quantity fibroblast proliferation is only arranged in the mucosa.
The above results explanation Xingsiang Tuerfeng total phenolic acid extract has obvious therapeutic action to rat chronic pelvic inflammatory disease due to the escherichia coli.
Claims (9)
1. an Xingsiang Tuerfeng total phenolic acid extract is characterized in that said extract prepares through following method: get the dry medical material of Ainsliasa fragrans Champ, be ground into coarse powder, with the ethanol extraction of 40%-70%; Filter, get filtrating, filtrate decompression concentrates, and adding ethanol, to make the solution concentration of alcohol be 20%-40%; Every ml soln is equivalent to crude drug 0.8-1.0g, in solution, adds hydrochloric acid accent pH to 1.0-3.0, leaves standstill, and placed 12-24 hour at cold place; Centrifugal or filter, get clear liquid, clear liquid is evaporated to does not have alcohol, and the dissolving of concentrate adding distil water disperses; On the macroporous adsorptive resins of having handled well on the disperse object, the type of macroporous resin is AB-8 type, NKA-9 type, D-101 type or HP-20 type, and it is thin out to be eluted to the water lotion color with deionized water earlier, uses 70% ethanol elution instead; Be negative to the phenolic acid chromogenic reaction, collect ethanol elution, merge; Concentrating under reduced pressure, drying promptly gets the Ainsliaea fragrans Champ. phenolic acid extract.
2. phenolic acid extract according to claim 1 is characterized in that the aquiferous ethanol that the eluting post is used is preferably 70% ethanol.
3. phenolic acid extract according to claim 1 is characterized in that adding the hydrochloric acid adjust pH and is preferably 1.0.
4. phenolic acid extract according to claim 1 is characterized in that described phenolic acid extract contains organic phenolic acids and flavones ingredient.
5. phenolic acid extract according to claim 4 is characterized in that described organic liposoluble ingredient comprises chlorogenic acid.
6. phenolic acid extract according to claim 1, the content that it is characterized in that total phenolic acid in the described phenolic acid extract is greater than 60%.
7. phenolic acid extract according to claim 1 is characterized in that in chlorogenic acid, and chlorogenic acid contents is 1%～5% in the extract.
8. phenolic acid extract according to claim 6 is characterized in that chlorogenic acid contents is 2%～4% in the extract.
9. like the application of each described Xingsiang Tuerfeng total phenolic acid extract among the claim 1-8 in preparation treatment gynecological inflammation medicine.
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| CN108129436A (en) * | 2017-12-28 | 2018-06-08 | 长沙湘资生物科技有限公司 | From the method for Frangrant Ainsliaea Herb chlorogenic acid extracting and apiolin |
| CN113197927A (en) * | 2021-01-29 | 2021-08-03 | 中国药科大学 | Application of Ainsliaea fragrans extract in preparation of medicine for treating primary dysmenorrhea |
| CN113125629B (en) * | 2021-03-24 | 2022-08-16 | 贵州医科大学 | Method for simultaneously identifying multiple sources of lepriasis |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1709417A (en) * | 2005-06-16 | 2005-12-21 | 江西汇仁药业有限公司 | Ainsliaea fragrans champ extract and its preparing method |
| CN1899337A (en) * | 2005-07-22 | 2007-01-24 | 陈正道 | Extracting method and use of ainsliaea fragrans champ-extract |
| CN101293003A (en) * | 2008-06-17 | 2008-10-29 | 江西天佑药业有限公司 | Effect section of frangrant ainsliaea herb, preparation method and application thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1709417A (en) * | 2005-06-16 | 2005-12-21 | 江西汇仁药业有限公司 | Ainsliaea fragrans champ extract and its preparing method |
| CN1899337A (en) * | 2005-07-22 | 2007-01-24 | 陈正道 | Extracting method and use of ainsliaea fragrans champ-extract |
| CN101293003A (en) * | 2008-06-17 | 2008-10-29 | 江西天佑药业有限公司 | Effect section of frangrant ainsliaea herb, preparation method and application thereof |
Non-Patent Citations (5)
| Title |
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| .《中草药》.2006,第37卷(第3期),347-348. * |
| 刘波.《杏香兔耳风的活性成分研究》.《中国优秀博硕士学位论文全文数据库(硕士)工程科技I辑》.2005,(第4期),B016-105. * |
| 张锐等.《杏香兔耳风的化学成分研究(II)> * |
| 张锐等.《杏香兔耳风的化学成分研究(II)>.《中草药》.2006,第37卷(第3期),347-348. |
| 易剑锋.《杏香兔耳风对宫颈炎大鼠宫颈黏膜PGE_2及外周血T淋巴细胞亚群表达的影响》.《中华中医药杂志》.2007,第22卷(第11期),806-808. * |
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