CN102895386B - Method for performing extraction on angelica dahurica, common cnidium fruit, Chinese red pepper and elecampane inula root and pharmaceutical application - Google Patents
Method for performing extraction on angelica dahurica, common cnidium fruit, Chinese red pepper and elecampane inula root and pharmaceutical application Download PDFInfo
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Abstract
The invention belongs to the technical field of Chinese medicines and aims to provide a method for performing extraction on angelica dahurica, common cnidium fruit, Chinese red pepper and elecampane inula root and a prepared medicine. The technical scheme is that the method comprises the following steps of: distilling four cleaned and crushed Chinese medicinal herbs, namely angelica dahurica, common cnidium fruit, Chinese red pepper and elecampane inula root for 2 to 4 hours by using straight-through steam, and extracting volatile oil; and performing reflux extraction on decoction dregs obtained after the volatile oil is extracted for 2 to 3 times by using 70 to 80 percent ethanol in an amount which is 6 to 8 times the amount of the decoction dregs, refluxing for 1 to 3 hours every time, and concentrating to obtain an extract. By optimizing the mixing ratio of the four Chinese medicinal herbs and borneol, the volatile oil obtained through extraction, the extract and the borneol are prepared into an ointment, a gel, a lotion and the like, and are used for preparing a medicine for treating tinea pedis, mycotic dermatitis, gynecological inflammation and the like. By the method, active ingredients of the four Chinese medicinal herbs are furthest extracted, the extraction efficiency is improved, and the prepared formulation form and the treatment range of diseases are developed.
Description
Technical field
The invention belongs to technical field of Chinese medicines, be specifically related to extracting method and the application of extract in pharmacy thereof of a kind of Radix Angelicae Dahuricae, Fructus Cnidii, Pericarpium Zanthoxyli, Radix Inulae raw medicinal material.
Background technology
The Radix Angelicae Dahuricae: property and flavor of peppery and warm fragrance, there is wind-damp dispelling, a function of the evacuation of pus of invigorating blood circulation, granulation promoting pain relieving, can be used for headache, toothache, nasal sinusitis, hemorrhoidal hamorrhage anal fistula, leucorrhea with red and white discharge, ulcer sores, skin pruritus.
Fructus Cnidii: warm in nature, acrid in the mouth, hardship, have warming the kidney to invigorate YANG, dampness, dispel the wind, the function of parasite killing, for sexual impotence, cold womb, cold-damp leukorrhagia, arthralgia chiefly caused by damp pathogen lumbago; External treatment vulval eczema, married woman's pudendal pruritus, trichomonal vaginitis.
Pericarpium Zanthoxyli: nature and flavor are pungent, hot, has the effect of fragrant stomach invigorating, warming spleen and stomach for dispelling cold, removing damp and stopping pain, parasite killing removing toxic substances, antipruritic solution raw meat.
Radix Inulae: nature and flavor acrid, bitter, warm, Radix Inulae quintessence oil has calmness, sterilize, bring down a fever and the effect of anthelmintic, can be used as antibiotic medicine, anti-microbial agents.
About containing the application of above-mentioned four taste Chinese medicines, as just disclosed respectively a kind of external preparation for the treatment of gynecological inflammation in CN101926875A, CN1823990A, the two has all used the Radix Angelicae Dahuricae, Fructus Cnidii, Pericarpium Zanthoxyli, another Borneolum Syntheticum in addition, but the former uses Radix Inulae, the latter uses Radix Aristolochiae, and Radix Inulae is the simple replacement of Radix Aristolochiae.In CN102068508A, CN102641368A, disclose respectively a kind of Chinese medicine for the treatment of beriberi, all used the Radix Angelicae Dahuricae and Fructus Cnidii two taste raw medicinal materials.
About the extracting method of above-mentioned four taste Effective Component of Chinese Medicines, content as disclosed in CN101926875A, CN1823990A, mainly by decocting with water acquisition volatile oil, and to the decocting method that for liquid, ethanol (being decoction and alcohol sedimentation technique) extracts.
And the method for extracting volatile oil in prior art has four kinds conventionally: (1) way of distillation; (2) solvent method; (3) milling process; (4) supercritical CO
2fluid extraction method.Steam distillation in the way of distillation specifically has again four kinds of distillation modes: water distillation, distilling above water, open steam distillation (i.e. straight-through steaming process), water diffusion steam distillation.Wherein open steam distillation refers to: a band orifice ring line pipe is installed under sieve plate, by external steam, by aperture, is directly sprayed, enter sieve aperture raw material is heated.
The method of solvent extraction Effective Component of Chinese Medicine has again infusion process, percolation, decocting method, reflux extraction etc., for different Chinese medicine, takes different extracting method, should consider that effective ingredient is not damaged, and considers again the problem of extraction efficiency.
Though many to the achievement in research of related drugs formula and extraction process in existing, all do not have to make a breakthrough in extraction efficiency.Namely could not obtain to a greater extent effective ingredient wherein, and improve extraction efficiency.Especially for some certain drug, need to adopt specific extracting method just can obtain good effect, improve extract active substance content.Otherwise dosage form prepared by extract and the developing of disease treatment scope have just been limited.
Summary of the invention
The present invention aims to provide extracting method and the application of extract in pharmacy of a kind of Radix Angelicae Dahuricae, Fructus Cnidii, Pericarpium Zanthoxyli, Radix Inulae.This extracting method is effective component extracting to a greater extent, and improves extraction efficiency.
For achieving the above object, the present invention is by screening and great many of experiments, unexpected discovery when extracting the Radix Angelicae Dahuricae, Fructus Cnidii, Pericarpium Zanthoxyli, Radix Inulae, by straight-through steam distillation, extract volatile oil, alcohol reflux residue medicinal residues, through the concentrated mode that obtains extractum, can significantly improve amount and the efficiency of effective component extracting again.
Particularly, this extracting method comprises the steps:
1) get the raw medicinal material Radix Angelicae Dahuricae, Fructus Cnidii, Pericarpium Zanthoxyli, Radix Inulae, choose decontamination, smash or shred;
2) with straight-through steaming process distillation 2～4 hours, collect volatile oil;
3) extract 70%～80% alcohol reflux of 6～8 times of amounts 2～3 times for medicinal residues after volatile oil, reflux 1～3 hour at every turn;
4) extracting solution filters, and merging filtrate reclaims ethanol concentrating under reduced pressure, obtains extractum.
Wherein, step 2), 3), 4), the Radix Angelicae Dahuricae, Fructus Cnidii, Pericarpium Zanthoxyli, Radix Inulae four Chinese medicine material are processed simultaneously.
The extracting method of the described Radix Angelicae Dahuricae, Fructus Cnidii, Pericarpium Zanthoxyli, Radix Inulae, what step (1) adopted is smashing or chopping method of conventional raw medicinal material, this step raw medicinal material is prepared into thinner, the time of straight-through steam distilled time of step (2) and step (3) alcohol reflux is just shorter, the corresponding raising of extraction efficiency.
Further, described step 2) the preferably 3 hours time of straight-through steaming process distillating extracting oil.
Further, described step 3) is extracted the medicinal residues after volatile oil, preferably uses 75% alcohol reflux 2 times, 75% alcohol reflux of 8 times of amounts of the 1st use 2 hours, 75% alcohol reflux of 6 times of amounts of the 2nd use 2 hours.
The extracting method of straight-through steaming process provided by the invention and ethanol refluxing process, add the extracting method that thermal distillation+water extract-alcohol precipitation extracts and compare with the disclosed water that adds of prior art, the amount of extracting volatile oil can increase more than 38%, the amount of extracting osthole can increase more than 40%, has obviously improved the amount of the effective ingredient obtaining.
Volatile oil and extractum that the present invention obtains, can be merged together, and adds other adjuvants, is further prepared into various dosage forms, as being prepared as ointment, gel, lotion etc. according to general preparation principle.As, the volatile oil of above-mentioned acquisition and extractum can be prepared into gel with Borneolum Syntheticum and disodiumedetate, carbomer, propylene glycol, ethanol, azone and ethyl hydroxybenzoate and suitable quantity of water, this gel can be used for treating gynecological inflammation.
While preparing the above-mentioned medicine containing the Radix Angelicae Dahuricae, Fructus Cnidii, Pericarpium Zanthoxyli, Radix Inulae raw medicinal material extract and Borneolum Syntheticum, the consumption of front four taste raw medicinal materials and Borneolum Syntheticum, according to weight proportion, be: 120～160 parts of the Radixs Angelicae Dahuricae, 120～160 parts of Fructus Cnidiis, 120～160 parts, Pericarpium Zanthoxyli, 20～50 parts of Radix Inulaes, 20～50 parts of Borneolum Syntheticums, preferred weight proportioning is: 145 parts of the Radixs Angelicae Dahuricae, 145 parts of Fructus Cnidiis, 145 parts, Pericarpium Zanthoxyli, 30 parts of Radix Inulaes, 30 parts of Borneolum Syntheticums.
By further research, find, owing to extracting the effective ingredient concentration of the Radix Angelicae Dahuricae, Fructus Cnidii, Pericarpium Zanthoxyli, Radix Inulae by the inventive method, increase, and preferred prescription.After merging with extractum, the volatile oil that discovery extraction obtains together with Borneolum Syntheticum, the dermatosiss such as tinea pedis, mycotic dermatitis are had to good curative effect.Meanwhile, in the treatment of gynecological inflammation, also can show better therapeutic effect.Therefore can be prepared as the related drugs containing the Radix Angelicae Dahuricae, Fructus Cnidii, Pericarpium Zanthoxyli, the extraction of Radix Inulae raw medicinal material and Borneolum Syntheticum, for the treatment of tinea pedis, mycotic dermatitis, gynecological inflammation etc.
And in the present invention, take straight-through steaming process, distillation time is short, in the process of distillation, just can carry out oil-water separation, has simplified subsequent purification operation, further saves preparation time; Adopt ethanol reflux extraction, a large amount of production also can adopt the mode of continuous circumfluence extraction, and subsequent treatment is easier, has saved the permanent standing time of decoction and alcohol sedimentation technique, in extraction efficiency, is significantly improved.
Therefore, useful technique effect of the present invention is: in technical scheme of the present invention, with straight-through steaming process and ethanol refluxing process extract the Radix Angelicae Dahuricae, Fructus Cnidii, Pericarpium Zanthoxyli, Radix Inulae raw medicinal material, by controlling the number of times etc. of distillation time, concentration of alcohol, ethanol consumption and alcohol reflux, obtain to a greater extent effective ingredient wherein, and improved extraction efficiency.Simultaneously, increase due to the inventive method extraction four Chinese medicine material effective ingredient concentration, by optimizing the proportioning of four taste raw medicinal materials and Borneolum Syntheticum, extract the volatile oil obtaining and be prepared as ointment, gel, lotion etc. with extractum together with Borneolum Syntheticum, for the preparation of the medicine for the treatment of tinea pedis, mycotic dermatitis, gynecological inflammation etc.
The specific embodiment
Below the invention will be further described by specific embodiment, but not in order to limit the present invention, all within the present invention's spirit and principle, any modification of doing, is equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Embodiment 1-3
According to the extracting method of straight-through steaming process+ethanol refluxing process provided by the invention, add the method that thermal distillation and water extract-alcohol precipitation extract and carry out three groups of parallel contrast experiments with the existing water that adds, experimentation and result are as follows:
Get Radix Angelicae Dahuricae 145g, Fructus Cnidii 145g, Pericarpium Zanthoxyli 145g, Radix Inulae 30g, choose decontamination, shred standby.
Extracting method of the present invention (straight-through steaming process+ethanol refluxing process): straight-through steaming process distillation 3 hours, collect volatile oil; Extract 75% alcohol reflux 2 times for medicinal residues after volatile oil, 75% alcohol reflux of 8 times of amounts of the 1st use 2 hours, 75% alcohol reflux of 6 times of amounts of the 2nd use 2 hours; Extracting solution filters, and merging filtrate reclaims ethanol concentrating under reduced pressure, obtains extractum.
Prior art extracting method (add water heating the way of distillation+decoction and alcohol sedimentation technique): to the water distillation 3.5 hours that adds 10 times of amounts in clean system and the broken Radix Angelicae Dahuricae, Fructus Cnidii, Pericarpium Zanthoxyli, Radix Inulae four taste raw medicinal materials, collect respectively Aromatic water and decocting liquid; Aromatic water is carried out to redistillation 30 minutes, obtain rectification liquid.Above-mentioned decocting liquid is filtered, and filtrate is concentrated into relative density 1.20(25 ℃); Add ethanol and make alcohol content be 70%, standing, get 10% sodium hydroxide solution adjust pH to 8.0 for supernatant, standing over night, gets supernatant, reclaims ethanol to without alcohol taste, obtains medicinal liquid.
Detected respectively adding of volatilization oil mass that the present invention obtains and the prior art oil mass of volatilizing in the rectification liquid that the water heating way of distillation obtains; Content of Osthole in the medicinal liquid that the extractum obtaining with high performance liquid chromatography detection the present invention and the decoction and alcohol sedimentation technique of prior art obtain, result is as follows:
From above contrast test, straight-through steaming process+ethanol refluxing process extracting method provided by the invention, the amount of extracting volatile oil has increased more than 38%, extract osthole amount increase more than 40%, obviously improved the amount of the effective ingredient obtaining.
Embodiment 4
Get Radix Angelicae Dahuricae 145g, Fructus Cnidii 145g, Pericarpium Zanthoxyli 145g, Radix Inulae 30g, choose decontamination, shred standby; Straight-through steaming process distillation 3.5 hours, collects volatile oil 6.1ml.Extract 70% alcohol reflux 3 times for medicinal residues after volatile oil, use 70% alcohol reflux 2 hours of 7 times of amounts at every turn; Extracting solution filters, and merging filtrate reclaims ethanol concentrating under reduced pressure, obtains extractum, and the content that records osthole in extractum is 0.51g.
Embodiment 5
Get Radix Angelicae Dahuricae 145g, Fructus Cnidii 145g, Pericarpium Zanthoxyli 145g, Radix Inulae 30g, choose decontamination, shred standby; Straight-through steaming process distillation 2.5 hours, collects volatile oil 6.0ml.Extract 80% alcohol reflux 2 times for medicinal residues after volatile oil, 80% alcohol reflux of 8 times of amounts of the 1st use 3 hours, 80% alcohol reflux of 6 times of amounts of the 2nd use 1 hour; Extracting solution filters, and merging filtrate reclaims ethanol concentrating under reduced pressure, obtains extractum, and the content that records osthole in extractum is 0.51g.
Embodiment 6
After getting disodiumedetate 0.2g and adding water and make to dissolve, add carbomer 20g, stir evenly, standing 12～24 hours, shake up, obtain carbomer gel.Get propylene glycol 500g, add successively ethanol 120g, azone 10g, ethyl hydroxybenzoate 1g, Borneolum Syntheticum 30g, and volatile oil and the extractum of embodiment 1 the inventive method (straight-through steaming process+ethanol refluxing process) acquisition, after mixing, merge with carbomer gel, stir evenly, add suitable quantity of water and make 1000g, obtain gel preparation.
After getting disodiumedetate 0.2g and adding water and make to dissolve, add carbomer 20g, stir evenly, standing 12～24 hours, shake up, obtain carbomer gel.Get propylene glycol 500g, add successively ethanol 120g, azone 10g, ethyl hydroxybenzoate 1g, Borneolum Syntheticum 30g, and rectification liquid and medicinal liquid that in embodiment 1, the method (adding the water heating way of distillation+decoction and alcohol sedimentation technique) of prior art obtains, after mixing, merge with carbomer gel, stir evenly, add suitable quantity of water and make 1000g, obtain gel preparation.
The gel preparation that the method extract of prior art in the inventive method extract and embodiment 1 is made respectively according to above-mentioned steps, is respectively used to the treatment of vaginitis (gynecological inflammation a kind of), is applied to clean affected part, 2～4 times on the one.Within 30th, be a course for the treatment of, statistics curative effect.
Symptom disappears completely for curing;
Symptom improves or cures as effectively;
The gel preparation that the inventive method extract makes, result cure rate is 86%, effective percentage is 97%.And healing case had no recurrence in 4 weeks.Total case 100 examples.
Art methods is extracted the gel preparation making, and result cure rate is 69%, and effective percentage is 90%.Total case 100 examples.
Embodiment 7
Get stearic acid, lanoline, triethanolamine, glycerol, laurocapram and make ointment base, volatile oil, extractum and Borneolum Syntheticum 30g with embodiment 2 acquisitions, by emulsion process, be mixed with emulsifiable paste, make every gram of emulsifiable paste containing crude drug 0.495g, treatment for tinea pedis, be applied to clean affected part, 2 times on the one, evident in efficacy.
Claims (8)
1. an extracting method for the Radix Angelicae Dahuricae, Fructus Cnidii, Pericarpium Zanthoxyli, Radix Inulae, is characterized in that comprising the steps:
1) get the raw medicinal material Radix Angelicae Dahuricae, Fructus Cnidii, Pericarpium Zanthoxyli, Radix Inulae, choose decontamination, smash or shred;
2) with straight-through steaming process distillation 2～4 hours, collect volatile oil;
3) extract 70%～80% alcohol reflux of 6～8 times of amounts 2～3 times for medicinal residues after volatile oil, reflux 1～3 hour at every turn;
4) extracting solution filters, and merging filtrate reclaims ethanol concentrating under reduced pressure, obtains extractum;
Wherein, step 2), 3), 4), four Chinese medicine material is processed simultaneously.
2. the extracting method of the Radix Angelicae Dahuricae, Fructus Cnidii, Pericarpium Zanthoxyli, Radix Inulae as claimed in claim 1, is characterized in that described step 2) in distillation time be 3 hours.
3. the extracting method of the Radix Angelicae Dahuricae, Fructus Cnidii, Pericarpium Zanthoxyli, Radix Inulae as claimed in claim 1, is characterized in that in described step 3) reflux, extract, 2 times, 75% alcohol reflux of 8 times of amounts of the 1st use 2 hours, 75% alcohol reflux of 6 times of amounts of the 2nd use 2 hours.
4. adopt profit to require the application in pharmacy of extract that described in 1, extracting method obtains, it is characterized in that the volatile oil and the extractum that extract can merge, and are further prepared as ointment, gel or lotion.
5. the application of the extract that described in employing claim 1, extracting method obtains in pharmacy, is characterized in that the volatile oil and the extractum that extract can merge, and are prepared as the medicine for the treatment of tinea pedis and mycotic dermatitis together with Borneolum Syntheticum.
6. the application of the extract that described in employing claim 1, extracting method obtains in pharmacy, is characterized in that the volatile oil and the extractum that extract can merge, and are prepared as the medicine for the treatment of gynecological inflammation together with Borneolum Syntheticum.
7. the application of extract in pharmacy as described in claim 5 or 6, the consumption that it is characterized in that the Radix Angelicae Dahuricae, Fructus Cnidii, Pericarpium Zanthoxyli, Radix Inulae, Borneolum Syntheticum raw medicinal material, according to weight proportion is: 20～50 parts of 120～160 parts of the Radixs Angelicae Dahuricae, 120～160 parts of Fructus Cnidiis, 120～160 parts, Pericarpium Zanthoxyli, Radix Inulae 20～50, Borneolum Syntheticum.
8. the application of extract in pharmacy as claimed in claim 7, the consumption that it is characterized in that the Radix Angelicae Dahuricae, Fructus Cnidii, Pericarpium Zanthoxyli, Radix Inulae, Borneolum Syntheticum raw medicinal material, weight proportion is: 145 parts of the Radixs Angelicae Dahuricae, 145 parts of Fructus Cnidiis, 145 parts, Pericarpium Zanthoxyli, 30 parts of Radix Inulaes, 30 parts of Borneolum Syntheticums.
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| CN201210428512.9A CN102895386B (en) | 2012-10-31 | 2012-10-31 | Method for performing extraction on angelica dahurica, common cnidium fruit, Chinese red pepper and elecampane inula root and pharmaceutical application |
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| CN201210428512.9A CN102895386B (en) | 2012-10-31 | 2012-10-31 | Method for performing extraction on angelica dahurica, common cnidium fruit, Chinese red pepper and elecampane inula root and pharmaceutical application |
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| CN102895386A CN102895386A (en) | 2013-01-30 |
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| CN111686188A (en) * | 2020-07-16 | 2020-09-22 | 兴安界首骨伤医院有限公司 | Cooling paste and preparation method and application method thereof |
| CN113384631A (en) * | 2021-07-20 | 2021-09-14 | 吉林玉仁制药股份有限公司 | Antibacterial liquid and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101926875A (en) * | 2009-09-22 | 2010-12-29 | 贵州健兴药业有限公司 | Gel for treating gynecologic inflammation and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101926875A (en) * | 2009-09-22 | 2010-12-29 | 贵州健兴药业有限公司 | Gel for treating gynecologic inflammation and preparation method thereof |
Non-Patent Citations (2)
| Title |
|---|
| 刘继鑫等.水蒸气蒸馏法提取中药挥发油存在的问题及解决方法.《时珍国医国药》.2008,第19卷(第1期),97-98. |
| 水蒸气蒸馏法提取中药挥发油存在的问题及解决方法;刘继鑫等;《时珍国医国药》;20080131;第19卷(第1期);97-98 * |
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Denomination of invention: An extraction method and pharmaceutical application of Angelica dahurica, Cnidium monnieri, Zanthoxylum bungeanum and cihuaxiang Effective date of registration: 20210508 Granted publication date: 20140305 Pledgee: Guiyang Branch of Shanghai Pudong Development Bank Co.,Ltd. Pledgor: GUIZHOU JIANXING PHARMACEUTICAL Co.,Ltd. Registration number: Y2021520000003 |
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