CN101485701B - Method for preparing total polyphenol of Loropetalum chinense (R. Br.) Oliver for treating burn and scald - Google Patents
Method for preparing total polyphenol of Loropetalum chinense (R. Br.) Oliver for treating burn and scald Download PDFInfo
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- CN101485701B CN101485701B CN2009101110544A CN200910111054A CN101485701B CN 101485701 B CN101485701 B CN 101485701B CN 2009101110544 A CN2009101110544 A CN 2009101110544A CN 200910111054 A CN200910111054 A CN 200910111054A CN 101485701 B CN101485701 B CN 101485701B
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Abstract
The invention discloses a method for preparing loropetalum chinense total polyphenol for treating burn and scald, and relates to a drug for treating the burn and scald. The invention provides the method for preparing the loropetalum chinense total polyphenol for treating the burn and scald, which comprises that: Loropetalum chinense leaves are pulverized, are added with acetone, are soaked, and are filtered to obtain filtrate and filter residue; the filter residue is added with the acetone, is soaked, is extracted for at least one time, and is filtered; the filtrate is combined and is condensed to obtain an upper column solution; the acetone is reclaimed; the upper column solution is added to a macroporous resin column and is eluted with water or ethanol till an eluant is close to colorless; the eluant is collected; and the ethanol is reclaimed is condensed, and is dried to obtain the loropetalum chinense total polyphenol. The preparation method is simple and suitable for industrialized production; and in-vivo/in-vitro tests prove that the prepared loropetalum chinense total polyphenol extract with mass percentage of total polyphenol of more than or equal to 50 percent has good functions of resisting inflammation, relieving heat, easing pain, resisting bacteria, and the like, and can be applied to the preparation of a drug for treating burn, sunburn and trauma. The loropetalum chinense total polyphenol can be prepared into soft plaster, gel, troche, capsule, soft capsule, oral liquid, syrup, drop pill, injection, and other preparations.
Description
Technical field
The present invention relates to a kind of treatment burn and scald medicine, especially relate to a kind of preparation method for the treatment of the Loropetalum chinense (R. Br.) Oliv. total polyphenols of burn, sunburn, wound.
Background technology
Burn, sunburn, wound are a kind of commonly encountered diseases, often take place in daily life, and burn sickness rate such as fire, gas explosion burn and water, oil scald are very high, are approximately 2%.Sunburn is a kind of often out in the cold, but has a strong impact on the disease of human health, the lighter's redness, decortication, and weight person causes skin carcinoma, and particularly long-term work is outdoor workman, peasant, soldier etc., and the number incidence rate that ultraviolet is burnt and tanned severely is higher.Along with environment degenerates, greenhouse effect, ultraviolet intensity is more and more higher, and sunburn all the more causes people's attention.Up to the present, do not see the medicine of anti-sunburn on the market.This shows that the potential of demand of burn, sunburn medicine is very big.At present, domestic and international treatment for burn, sunburn, traumatic hemorrhage roughly is divided into operative therapy and conservative treatment two classes.At home, the main pharmaceutical dosage form of conservative treatment is patch and ointment etc., except that medicines such as YUNNAN BAIYAO and Scald Ointment, still lacks a kind of determined curative effect, short treating period, cure rate height, untoward reaction is little and economy medicine easily on the market.Need clinically a kind of with Chinese characteristics, can go abroad, determined curative effect, steady quality, technology advanced person, toxic and side effects is little, cost is low, rapid-action, specially good effect quick curing medicine that using method is easy is as the regeneration product of treatment burn and traumatic hemorrhage.
Loropetalum chinense (R. Br.) Oliv. (Loropetalum chinense (R.Brown) Oliv.), use Chinese herbal medicine for China is among the people, it is Hamamelidaceae Hamamelis plant, grow in hills or the deserted mountain shrubbery, be distributed widely in the Changjiang river, on the south the downstream, area to the north of the tropic of cancer, all there is rich in natural resources on ground such as Anhui, Soviet Union, Zhejiang, Jiangxi, Hunan, Hubei Province, river, Guizhou Province, Fujian, Guangdong, osmanthus, Yunnan, and potentiality to be exploited is very big.The flat bitter in the mouth of its leaf, puckery has effects such as hemostasis, antidiarrheal, pain relieving and granulation promoting.Commonly used its among the people controlled burn, wound and hemorrhage etc., then is used for the treatment of diseases such as metrorrhagia and diarrhoea clinically, has better hemostasis, excited uterus, effect such as antibacterial.Pharmacological evaluation shows that Loropetalum chinense (R. Br.) Oliv. mixture and Folium Loropetali dry powder break to animal blood vessels and the femoral artery otch all has anastalsis.The extract of Loropetalum chinense (R. Br.) Oliv. all has bacteriostasis to streptococcus, staphylococcus, typhoid fever and escherichia coli in vitro.Contained Loropetalum chinense (R. Br.) Oliv. polyphenol is to streptococcus, staphylococcus aureus, Staphylococcus albus, micrococcus catarrhalis, and typhoid fever, paratyphoid fever, dysentery, modification, escherichia coli all have inhibitory action.The Loropetalum chinense (R. Br.) Oliv. polyphenol is compared with other burn medicines, has many-sided advantages such as resource, kind, curative effect and technology.
Publication number is that the application for a patent for invention of CN101153303 discloses a kind of method for producing Baihuajimu flavone, comprises successively that the branch and leaf that will spend Loropetalum chinense (R. Br.) Oliv. in vain, flower are pulled an oar and squeezed the juice, cryoconcentration, protease decomposition, microbial fermentation, centrifugalize, low temperature spray drying operation obtain Loropetalum chinense (R. Br.) Oliv. flavone crystal.This method has the characteristics of extraction ratio height, pollution-free, suitable suitability for industrialized production.
Publication number is that the application for a patent for invention of CN101181525 discloses a kind of external used medicine for the treatment of burn and scald, and it is the Pseudobulbus Bletillae (Rhizoma Bletillae), Radix Sanguisorbae, Herba Artemisiae Anomalae, Radix Sophorae Flavescentis, Fructus Gardeniae, Indigo Naturalis, Loropetalum chinense (R. Br.) Oliv., Radix Ilicis Pubescentis that the prescription of this medicine is formed.Use this its effective percentage 100% of invention Drug therapy burn and scald, cure rate 97%.This invention medicine processing technology is simple, is the ideal medicament of treatment burn and scald.
Publication number is that the application for a patent for invention of CN101214333 discloses a kind of medicine for the treatment of burn and scald, and the prescription composition of this medicine is: Rhizoma Coptidis (parched), stir-fry Fructus Forsythiae, Gypsum Fibrosum Preparatum, Cortex Jujubae charcoal, charred Radix Sanguisorbae, Loropetalum chinense (R. Br.) Oliv., Radix Ilicis Pubescentis, pine bark charcoal.Olibanum (parched), Myrrha (parched), Sanguis Draxonis, Radix Rumicis Patientiae.Use this invention Drug therapy burn and scald curative effect obvious, remove rapid by the burn and scald skin symptom, easy to use, nontoxic pair and stimulation, its effective percentage 100%, cure rate 97%.This invention medicine processing technology is simple, is the ideal medicament of treatment burn and scald.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method for the treatment of the Loropetalum chinense (R. Br.) Oliv. total polyphenols of burn and scald.
Prepared Loropetalum chinense (R. Br.) Oliv. total polyphenols can be made into the treatment burn and scald medicine of dosage forms such as ointment, gel, tablet, capsule, soft capsule, oral liquid, syrup, drop pill, injection.
The present invention includes following steps:
1) Folium Loropetali is pulverized, added acetone and soak, filter, get filtrate and filtering residue;
2) add acetone in filtering residue and soak, extracts at least 1 time, filter, filtrate merges, concentrate upper prop liquid, and recovery acetone;
3) upper prop liquid is added on the macroporous resin column, water or closely colourless to eluent with ethanol elution is collected eluent, reclaims ethanol and concentrated, and drying promptly gets the Loropetalum chinense (R. Br.) Oliv. total polyphenols.
In step 1), press mass ratio, the addition of acetone is preferably 8~20 times of Folium Loropetali, and by mass percentage, the concentration of acetone is preferably 20%~70%, and the time that adds the acetone immersion is preferably 1~10 day.
In step 2) in, press mass ratio, the amount that adds acetone is preferably 8~15 times of filtering residue, and by mass percentage, the concentration of acetone is preferably 20%~70%, and each time of soaking is preferably 1~10 day; Described concentrating preferably is concentrated into by volume crude drug: water is (1~2): 1.
In step 3), described near colourless can to adopt Diluted Alcohol to be eluted to eluent earlier closely colourless to eluent with ethanol elution, and reuse high concentration ethanol eluting resin column is closely colourless to eluent.Percentage ratio by volume, the concentration of Diluted Alcohol can adopt 1%~10%.
In gallic acid, above-mentioned prepared Loropetalum chinense (R. Br.) Oliv. total polyphenols records total polyphenols content 〉=50% with colorimetry.
Preparation method provided by the present invention is simple, is suitable for suitability for industrialized production; Prepared total polyphenols quality percentage composition is 〉=50% Loropetalum chinense (R. Br.) Oliv. total polyphenols extract, proves that through internal and external test it has good antiinflammatory, analgesic, analgesia, effect such as antibiotic, can use in preparation treatment burn, sunburn, wound medicine.Can make preparations such as ointment, gel, tablet, capsule, soft capsule, oral liquid, syrup, drop pill, injection as required.
The specific embodiment
Embodiment 1
(1) get the Folium Loropetali 5kg that dries in the shade, pulverize, drop into multi-function extractor, add 8 times of amount 70% acetone soaking at room temperature 1 day, filter, filtrate is squeezed into concentration tank; Filtering residue adds 8 times again and measures 70% acetone soaking at room temperature extraction 3 times, soaks 1 day at every turn, filters, and filtrate is squeezed into concentration tank, merges vacuum concentration with the 1st extracting solution, and reclaim acetone and also be concentrated into crude drug: water volume ratio is 2: 1, gets upper prop liquid.
(2) press crude drug: resin volume ratio=1: 1, the upper prop liquid that extraction is obtained is added on the D101 type macroporous adsorptive resins of having handled well, use 10% Diluted Alcohol, it is closely colourless to be eluted to eluent, and reuse 30% ethanol-eluting resin column is closely colourless to eluent, collect 40% ethanol elution, recovery ethanol also concentrates and obtains concentrated solution, and vacuum drying obtains Loropetalum chinense (R. Br.) Oliv. total polyphenols 210g, in gallic acid, it is 62% that colorimetry records total polyphenols content.
Embodiment 2
(1) get fresh Folium Loropetali 7kg, pulverize, drop into multi-function extractor, add 20 times of amount 20% acetone soaking at room temperature 10 days, filter, filtrate is squeezed into concentration tank; Medicinal residues add 15 times of amount 70% acetone soaking at room temperature 10 days again, filter, and filtrate is squeezed into concentration tank, merge vacuum concentration with the 1st extracting solution, and reclaim acetone and be concentrated into crude drug: water volume ratio is 1: 1, gets upper prop liquid.
(2) press crude drug: resin volume ratio=3: 1, the upper prop liquid that extraction workshop section is obtained is added on the HPD100 type macroporous adsorptive resins of having handled well, it is closely colourless that water is eluted to eluent, reuse 60% ethanol-eluting resin column is closely colourless to eluent, collects 60% ethanol elution, reclaims ethanol and concentrate to obtain concentrated solution, lyophilization, obtain Loropetalum chinense (R. Br.) Oliv. total polyphenols 369g, in gallic acid, it is 55% that colorimetry records total polyphenols content.
Embodiment 3
(1) get fresh Folium Loropetali 10kg, pulverize, drop into multi-function extractor, add 10 times of amount 30% acetone soaking at room temperature 7 days, filter, filtrate is squeezed into concentration tank; Medicinal residues add 8 times again and measure 30% acetone soaking at room temperature extraction 2 times, and each 7 days, to filter, filtrate is squeezed into concentration tank, merges vacuum concentration with the 1st extracting solution, and reclaim acetone and also be concentrated into crude drug: water volume ratio is 1.5: 1, gets upper prop liquid.
(2) press crude drug: resin volume ratio=2: 1, the upper prop liquid that extraction workshop section is obtained is added on the HP20 type macroporous adsorptive resins of having handled well, it is closely colourless that water is eluted to eluent, reuse 40% ethanol-eluting resin column is closely colourless to eluent, collects 40% ethanol elution, reclaims ethanol and concentrate to obtain concentrated solution, lyophilization, obtain Loropetalum chinense (R. Br.) Oliv. total polyphenols 472g, in gallic acid, it is 85% that colorimetry records total polyphenols content.
The total polyphenols for preparing according to embodiment 1~3 can be made into preparations such as ointment, gel, tablet, capsule, soft capsule, oral liquid, syrup, drop pill, injection.
Test example 1: the anti-inflammatory activity of Loropetalum chinense (R. Br.) Oliv. total polyphenols
The Loropetalum chinense (R. Br.) Oliv. total polyphenols extract that material: embodiment 1 obtains.
Adopt of the influence of mice dimethylbenzene ear swelling experimentation Loropetalum chinense (R. Br.) Oliv. extract to mice dimethylbenzene ear swelling.The Loropetalum chinense (R. Br.) Oliv. total polyphenols is 25.0,50.0,100.0mg/kg, Dexamethasone group 1.0mg/kg, and the blank group is irritated the 0.5%CMC (0.2ml/10g) that stomach waits capacity, every day 1 time, successive administration 5 days.30min after last 1 administration, every Mus left side ear drips 20 μ l dimethylbenzene, each 10 μ l of positive and negative.45min takes off cervical vertebra execution mice after giving dimethylbenzene, cuts ears along auricle, alignment, and the ear same area is laid auricle with the 9mm card punch in the left and right sides, and precision is weighed, and calculates swelling degree (mg) and suppression ratio (%).
The inhibitory action result of the xylol induced mice ear swelling of Loropetalum chinense (R. Br.) Oliv. total polyphenols is as shown in table 1, the suppression ratio of positive control medicine dexamethasone is 31.1%, the Loropetalum chinense (R. Br.) Oliv. total polyphenols has a good restraining activity to mouse ear is swollen in the dosage range of 50~100mg/kg, and active and dosage has certain dose-effect relationship, and Loropetalum chinense (R. Br.) Oliv. total polyphenols 50.0,100.0mg/kg are respectively 44% and 50.7% to the suppression ratio of mice dimethylbenzene ear swelling.
Table 1
Compare with model group:
*, P<0.01
Test example 2: the antibacterial activity of Loropetalum chinense (R. Br.) Oliv. total polyphenols
The Loropetalum chinense (R. Br.) Oliv. total polyphenols extract that material: embodiment 1 obtains.
Adopt the agarose doubling dilution to carry out drug sensitive test, investigate the external minimum inhibitory concentration of Loropetalum chinense (R. Br.) Oliv. total polyphenols (MIC) different strains.The final concentration of Loropetalum chinense (R. Br.) Oliv. total polyphenols is respectively 30.00,10.00,3.00,1.00mg/ml; The blank group is to wait the distilled water of capacity, and positive drug is an ampicillin, inoculum concentration 10
5The CFU/ point is put and is cultivated observed result behind the 18h in 37 ℃ of constant incubators.The aseptic long Cmin of being born is minimum inhibitory concentration (MIC).
The result shows that the Loropetalum chinense (R. Br.) Oliv. total polyphenols has inhibitory action to staphylococcus aureus, Streptococcus viridans, coli strain, and is stronger to the bacteriostasis of staphylococcus aureus and Streptococcus viridans, and its minimum inhibitory concentration (MIC) is 3mg/ml.
Claims (4)
1. preparation method for the treatment of the Loropetalum chinense (R. Br.) Oliv. total polyphenols of burn and scald is characterized in that may further comprise the steps:
1) Folium Loropetali is pulverized, added acetone and soak, filter, get filtrate and filtering residue, press mass ratio, the addition of acetone is 8~20 times of Folium Loropetali, and by mass percentage, the concentration of acetone is 20%~70%, and the time that adds the acetone immersion is 1~10 day;
2) add acetone in filtering residue and soak, extract at least 1 time, filter, filtrate merges, concentrate upper prop liquid, and reclaim acetone, press mass ratio, the amount of adding acetone is 8~15 times of filtering residue, by mass percentage, the concentration of acetone is 20%~70%, and each time of soaking is 1~10 day;
3) upper prop liquid is added on the macroporous resin column, water or closely colourless to eluent with ethanol elution is collected eluent, reclaims ethanol and concentrated, and drying promptly gets the Loropetalum chinense (R. Br.) Oliv. total polyphenols.
2. a kind of preparation method for the treatment of the Loropetalum chinense (R. Br.) Oliv. total polyphenols of burn and scald as claimed in claim 1 is characterized in that in step 2) in, describedly be concentrated into by volume crude drug: water is 1~2: 1.
3. a kind of preparation method for the treatment of the Loropetalum chinense (R. Br.) Oliv. total polyphenols of burn and scald as claimed in claim 1, it is characterized in that in step 3), described with ethanol elution to eluent near colourless be that to adopt Diluted Alcohol to be eluted to eluent earlier closely colourless, reuse high concentration ethanol eluting resin column is closely colourless to eluent.
4. a kind of preparation method for the treatment of the Loropetalum chinense (R. Br.) Oliv. total polyphenols of burn and scald as claimed in claim 3 is characterized in that in step 3), percentage ratio by volume, and the concentration of Diluted Alcohol is 1%~10%.
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CN102579524A (en) * | 2012-03-28 | 2012-07-18 | 江西徳宇集团 | Application of white flower loropetalum chinense in preparing healing medicine |
CN102716157A (en) * | 2012-07-06 | 2012-10-10 | 江西本草天工科技有限责任公司 | White flowered Loropetalum chinense total phenol extractive and preparation method and application thereof |
CN103977043A (en) * | 2014-05-19 | 2014-08-13 | 湖南农业大学 | Method for extracting red-flowered loropetalum polyphenol from red-flowered loropetalum leaves |
CN105287659B (en) * | 2014-06-23 | 2019-07-19 | 中国人民解放军军事医学科学院毒物药物研究所 | Loropetalum wood extract and its medical usage containing chinic acid class and glucoside compound |
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CN101153303A (en) * | 2007-09-18 | 2008-04-02 | 江西德宇集团 | Method for producing Baihuajimu flavone |
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CN101153303A (en) * | 2007-09-18 | 2008-04-02 | 江西德宇集团 | Method for producing Baihuajimu flavone |
Non-Patent Citations (2)
Title |
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周国海等.《红檵木叶中抑菌活性成分的初步研究.《食品科学》.2007,第28卷(第6期),74-75. * |
陈乃富等.红花檵木红色素的提取及其稳定性研究.《中国林副特产》.2004,(第70期),38-39. * |
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