CN101966212A - Preparation method and use of Syringa pubescens bark extract - Google Patents
Preparation method and use of Syringa pubescens bark extract Download PDFInfo
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- CN101966212A CN101966212A CN 201010505093 CN201010505093A CN101966212A CN 101966212 A CN101966212 A CN 101966212A CN 201010505093 CN201010505093 CN 201010505093 CN 201010505093 A CN201010505093 A CN 201010505093A CN 101966212 A CN101966212 A CN 101966212A
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- ethyl acetate
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Abstract
The invention belongs to the technical field of medicinal product research and development. The invention relates to a preparation method and use of Syringa pubescens bark extract. The method comprises: leaching 40-mesh Syringa pubescens bark powder with 70-percent ethanol in an amount which is 6 to 8 times that of the Syringa pubescens bark powder at room temperature for 8 to 10 hours, standing and filtering; leaching the filter residue with 70-percent ethanol in an amount which is 8 times that of the filter residue, leaching the filter residue with 70-percent ethanol in an amount which is 6 times that of the filter residue, performing ultrasonic treatment for 30 minutes, combining filtrate, recovering solvent and obtaining total extract; extracting the total extract with petroleum ether, ethyl acetate, water saturated n-butyl alcohol respectively at three times; and combining the petroleum ether layer extract solution, the ethyl acetate extract solution and the n-butyl alcohol extract solution, concentrating under vacuum, performing freeze drying, and obtaining the petroleum ether layer extract, ethyl acetate extract and n-butyl alcohol extract of the Syringa pubescens bark. The product of the invention has a remarkable removing effect on hydroxyl radicals, can be developed into a natural antioxidant medicament to be used as a substitute for synthetic antioxidant in treating diseases caused by an overlarge amount of radicals in the body.
Description
Technical field
Medical product research and development technical field under the present invention.The present invention relates to a kind of preparation method and its usage of Sytingamicrophylla bark extract.
Background technology
Sytingamicrophylla (Syringa Pubescens Turcz.) has another name called Syringa pubescens, tongue of sparrow flower, Syringa pubescens, be Oleaceae (Oleaceae) Genus Syringa (Syringa) plant, be distributed in ground such as China Henan, Hebei, Shaanxi, Shanxi, Gansu, be grown in the mountain region, ditch of height above sea level 800～2400m or on the cliffstone.Among the people early have understanding to its medical value, and Ceng Caiqi flower, fruit are made tea and drunk, and the curative effect of antiinflammatory, antitussive, treatment hepatitis and liver cirrhosis is arranged, but do not included by pharmacopeia so far.At present, both at home and abroad to the rare report of this Study on plants of Sytingamicrophylla, more belong to rare to the research of bark.
Free radical is the active chemical group that a class has unpaired electronics.Think at present, human diseases such as various inflammation, atherosclerosis, presenile dementia, parkinson, acute cerebrovascular disease, cancer, aging etc., all the oxidation with free radical stimulates closely related.Because the mechanism of oxidative damage plays an important role in the developing of disease, therefore, the antioxidation of Chinese medicine is its key factor that reaches therapeutic effect.Discover that the antioxidant of current main use mostly is the synthetic antioxidant, there are many negative effects in its health to the people.Therefore, in recent years, academia grows with each passing day to the research interest of the Natural antioxidant that exists in the plant.In order to seek antioxidant efficiently, the research of the Natural antioxidant is seemed extremely important.The focus of antioxidative research having become at present, but the antioxidant activity research of Sytingamicrophylla bark be yet there are no report.
Summary of the invention
The present invention is intended to inquire into the preparation method and its usage of Sytingamicrophylla bark extract, for the exploitation Natural antioxidant of fields such as medical science, Food Science provides new resources.
1, a kind of preparation method of Sytingamicrophylla bark extract is characterized in that may further comprise the steps:
(1) gets Sytingamicrophylla bark 40 order powder, doubly measure lixiviate 8-10h under the 70% ethanol room temperature, leave standstill filtration with 6-8;
(2) filtering residue is repeated above step respectively once, ultrasonic 30min with the ethanol of 8 times of amounts and 6 times of amounts 70% respectively again;
(3) merging filtrate reclaims solvent and promptly gets total extract;
(4) extract total extract respectively 3 times with petroleum ether, ethyl acetate and water-saturated n-butanol;
(5) merge petroleum ether layer, ethyl acetate layer and n-butanol layer extract respectively;
(6) with (five) petroleum ether layer, ethyl acetate layer and n-butanol layer extract difference concentrating under reduced pressure, lyophilization obtains Sytingamicrophylla bark petroleum ether layer extract, ethyl acetate layer extract, n-butanol layer extract.
2, the preparation method of the described Sytingamicrophylla bark extract of claim 1 is characterised in that its raw material is the bark of Sytingamicrophylla Syringa Pubescens Turcz..
3, a kind of purposes of Sytingamicrophylla bark extract is characterized in that this bark extract has very strong scavenging action to hydroxy radical.
4, a kind of purposes of Sytingamicrophylla bark extract is characterized in that this bark extract can be developed as the natural anti-oxidation medicine, the disease that the antioxidant therapy of replacement synthetic too much produces because of free radical in the human body.
5, the purposes of claim 3,4 each described Sytingamicrophylla bark extracts is characterised in that its preparation raw material is the bark of Sytingamicrophylla Syringa Pubescens Turcz..
According to the present invention, " % " among the present invention is percentage by weight.
The specific embodiment
The preparation method and its usage that relates to a kind of Sytingamicrophylla bark extract of the present invention comprises following examples, and the following examples can further specify the present invention, but do not limit the present invention in any way.
Embodiment 1:
(1) gets Sytingamicrophylla bark 40 order powder 100g,, leave standstill filtration with lixiviate 8h under 6 times of amount 70% ethanol room temperatures;
(2) filtering residue is repeated above step respectively once, ultrasonic 30min with the ethanol of 8 times of amounts and 6 times of amounts 70% respectively again;
(3) merging filtrate reclaims solvent and promptly gets total extract;
(4) extract total extract respectively 3 times with petroleum ether, ethyl acetate and water-saturated n-butanol;
(5) merge petroleum ether layer, ethyl acetate layer and n-butanol layer extract respectively;
(6) with (five) petroleum ether layer, ethyl acetate layer and n-butanol layer extract difference concentrating under reduced pressure, lyophilization obtains Sytingamicrophylla bark petroleum ether layer extract, ethyl acetate layer extract, n-butanol layer extract.
(7) with (six) petroleum ether layer extract, ethyl acetate layer extract, n-butanol layer extract carry out the antioxidation test, and this extract has very strong scavenging action to hydroxy radical.
Embodiment 2:
(1) gets Sytingamicrophylla bark 40 order powder 200g,, leave standstill filtration with lixiviate 10h under 8 times of amount 70% ethanol room temperatures;
(2) filtering residue is repeated above step respectively once, ultrasonic 30min with the ethanol of 8 times of amounts and 6 times of amounts 70% respectively again;
(3) merging filtrate reclaims solvent and promptly gets total extract;
(4) extract total extract respectively 3 times with petroleum ether, ethyl acetate and water-saturated n-butanol;
(5) merge petroleum ether layer, ethyl acetate layer and n-butanol layer extract respectively;
(6) with (five) petroleum ether layer, ethyl acetate layer and n-butanol layer extract difference concentrating under reduced pressure, lyophilization obtains Sytingamicrophylla bark petroleum ether layer extract, ethyl acetate layer extract, n-butanol layer extract.
(7) with (six) petroleum ether layer extract, ethyl acetate layer extract, n-butanol layer extract carry out the antioxidation test, and this extract has very strong scavenging action to hydroxy radical.
Pharmacological test example: the antioxidant activity of Sytingamicrophylla bark extract
1 materials and methods
1.1 laboratory sample source
Medical material picks up from the Jilin Agriculture University campus, is accredited as the bark of Oleaceae genus syringa Sytingamicrophylla Syringa Pubescens Turcz. by professor Hu Quande of gardening institute of Jilin Agriculture University.
1.2 instrument
76 new century ultraviolet-uisible spectrophotometers (Beijing Puxi General Instrument Co., Ltd); Lark LA114 type electronic balance (110g/0.0001g) (Bailing Balance Instrument Co., Ltd., Changshu); Electronic counting balance (500g/0.001g) (golden Yang Tianpingyiqichang); KQ-250DB type ultrasonic cleaner (Kunshan Ultrasonic Instruments Co., Ltd.); 101-2A type digital display electric heating is advertised drying baker (silk screen instrument and meter company limited Tongzhou, Shanghai branch company); Rotary Evaporators (Shanghai Yarong Biochemical Instrument Plant); Liquid-transfering gun (20ul); Water-bath.
1.3 reagent
DPPH solution, distilled water, dehydrated alcohol, methanol, ABTS, potassium peroxydisulfate, the potassium ferricyanide, phosphate buffer (PH=6.6), trichloroacetic acid, ferric chloride, Vc (vitamin C)
2 experimental techniques and step
2.1 the extraction of medical material component
Get Sytingamicrophylla bark sample powder 100g, after shredding, add 10 times respectively, 8 times, after 75% soak with ethanol of 6 times of amounts is spent the night, ultrasonic 30min leaves standstill filtration, merges 3 filtrates behind sucking filtration, place Rotary Evaporators to reclaim filtrate, be screwed into the liquid thickness to do not have the alcohol flavor approximately behind 150～300mL solution, pour in the evaporating dish, with water-bath (60 ℃ of temperature) with the solution evaporate to dryness, promptly get total extract, extraction ratio is 18.32%.Take out part water suspendible and become the 30mL suspension, once extract respectively 3 times with 3 times of amount petroleum ether, ethyl acetate and water-saturated n-butanols, merge petroleum ether layer, ethyl acetate layer and n-butanol layer extract, concentrating under reduced pressure, lyophilization obtains petroleum ether layer extract 5g respectively, ethyl acetate layer extract 8g, n-butanol layer extract 12g, standby.
2.2ABTS method is measured antioxidant activity
2.2.1 the preparation of sample solution
Accurately take by weighing the total extract, petroleum ether layer, ethyl acetate layer and the n-butanol layer extract 30mg that are dried to constant weight respectively, the water standardize solution is in the 10mL volumetric flask, being made into concentration is the sample mother solution of 3mg/mL, it is 0.018mg/mL that sample mother solution water stepwise dilution is become concentration, 0.037mg/mL, 0.075mg/mL, 0.15mg/mL, 0.31mg/mL, 0.62mg/mL, the sample solution of 1.25mg/mL is stand-by.
2.2.2ABTS
-+The preparation of solution
5mL, the ABTS of 14mM and 5mL, 4.9mMk2S2O8 mix generation ABTS+, static 16h in the dark, with using the ethanol dilution working solution before, requiring its absorbance under the 734nm wavelength is 0.70 ± 0.02.
2.2.3 sample determination
Get the 3ml sample solution and add 158 μ LABTS
+(A
Sample), do blank with ethanol, 158 μ LABTS
+With 3ml water be titer (A
Control), under the 734nm wavelength, measure absorbance behind the 6min, compare with VC.
Clearance rate (%)=[(AControl-ASample)/AControl] * 100%
2.3DPPH method is measured antioxidant activity
2.3.1 the preparation of sample solution
Accurately take by weighing the total extract, petroleum ether layer, ethyl acetate layer and the n-butanol layer extract 30mg that are dried to constant weight respectively, with the dehydrated alcohol standardize solution in the 10mL volumetric flask, being made into concentration is the sample mother solution of 3mg/mL, it is 0.018mg/mL that the sample mother solution is become concentration with the dehydrated alcohol stepwise dilution, 0.037mg/mL, 0.075mg/mL, 0.15mg/mL, 0.31mg/mL, 0.62mg/mL, the sample solution of 1.25mg/mL is stand-by.
2.3.2DPPH the preparation of solution
Precision takes by weighing DPPH sample 0.01g, adds dehydrated alcohol and is settled in the 50ml volumetric flask, obtains DPPH mother solution (concentration 0.2mg/mL).From mother solution, pipette 10mL, put in the 50mL volumetric flask, obtain DPPH solution, concentration 0.04mg/mL (whole process all needs lucifuge) with the dehydrated alcohol standardize solution.
2.3.3 sample determination
Total extract, petroleum ether layer, ethyl acetate layer and n-butanol layer extract sample solution are pressed table 1 and are added reactant liquor, shake up the back and leave standstill 30min in the room temperature lucifuge, measure absorbance at the 515nm place.Compare with VC.
Table 1 total extract, petroleum ether layer, ethyl acetate layer and n-butanol layer extract sample solution application of sample table
DPPH clearance rate %=(A-B+C)/A*100
3 results and discussion
3.1 result
3.1.1ABTS remove the free radical effect
See Table 2.
The different extract A BTS methods of Sytingamicrophylla bark are removed free radical activity under table 2 variable concentrations
3.1.2DPPH remove the free radical effect
See Table 3.
The different extract DPPH methods of Sytingamicrophylla bark are removed free radical activity under table 3. variable concentrations
3.2 discuss
3.2.1 the Sytingamicrophylla bark extract has stronger oxidation resistance, can remove ABTS, DPPH free radical very significantly.This research adopts in vitro method to investigate the antioxidant activity of its Sytingamicrophylla bark extract.Along with the increase of concentration, the oxidation resistance of Sytingamicrophylla bark extract strengthens thereupon, presents good dose-effect relationship.
3.2.2 Sytingamicrophylla bark extract ABTS method removing free radical ability size is under the variable concentrations: n-butanol layer＞ethyl acetate layer＞total extract＞petroleum ether layer, the n-butanol layer clearance rate approaches with concentration Vc.
3.2.3 Sytingamicrophylla bark extract DPPH method removing free radical ability size is under the variable concentrations: Vc＞n-butanol layer＞ethyl acetate layer＞total extract＞petroleum ether layer, the DPPH Faxian shows that Sytingamicrophylla bark extract oxidation resistance is remarkable.
This experiment has determined that Sytingamicrophylla is a Natural antioxidant resource preferably, for its Application and Development at aspects such as food, medical treatment and health cares provides foundation by to Sytingamicrophylla bark extract Study on Antioxidant Activities.
Claims (5)
1. the preparation method of a Sytingamicrophylla bark extract is characterized in that may further comprise the steps:
(1) gets Sytingamicrophylla bark 40 order powder, doubly measure lixiviate 8-10h under the 70% ethanol room temperature, leave standstill filtration with 6-8;
(2) filtering residue is repeated above step respectively once, ultrasonic 30min with the ethanol of 8 times of amounts and 6 times of amounts 70% respectively again;
(3) merging filtrate reclaims solvent and promptly gets total extract;
(4) extract total extract respectively 3 times with petroleum ether, ethyl acetate and water-saturated n-butanol;
(5) merge petroleum ether layer, ethyl acetate layer and n-butanol layer extract respectively;
(6) with (five) petroleum ether layer, ethyl acetate layer and n-butanol layer extract difference concentrating under reduced pressure, lyophilization obtains Sytingamicrophylla bark petroleum ether layer extract, ethyl acetate layer extract, n-butanol layer extract.
2. the preparation method of the described Sytingamicrophylla bark extract of claim 1 is characterised in that its raw material is the bark of Sytingamicrophylla Syringa Pubescens Turcz..
3. the purposes of a Sytingamicrophylla bark extract is characterized in that this bark extract has very strong scavenging action to hydroxy radical.
4. the purposes of a Sytingamicrophylla bark extract is characterized in that this bark extract can be developed as the natural anti-oxidation medicine, the disease that the antioxidant therapy of replacement synthetic too much produces because of free radical in the human body.
5. the purposes of claim 3,4 each described Sytingamicrophylla bark extracts is characterised in that its preparation raw material is the bark of Sytingamicrophylla Syringa Pubescens Turcz..
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102246829A (en) * | 2011-07-28 | 2011-11-23 | 北京农学院 | Clove extract for killing nematode and preparation method thereof |
| CN102579592A (en) * | 2012-02-20 | 2012-07-18 | 山东大学威海分校 | Syringa pubescens Turcz. bark extracts with protective effect on alcoholic liver injury |
| CN103405484A (en) * | 2013-08-26 | 2013-11-27 | 重庆工商大学 | Preparation method of patrinia villosa root anti-oxidization preparation |
| CN108976866A (en) * | 2018-08-06 | 2018-12-11 | 安徽三和工艺品有限公司 | A kind of bamboo rattan material wide spectrum mildew resistant paint |
| CN112245472A (en) * | 2020-11-25 | 2021-01-22 | 陕西科技大学 | Syringa microphylla seed extract and preparation method and application thereof |
-
2010
- 2010-09-28 CN CN 201010505093 patent/CN101966212A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 《中草药》 20030725 吴鸣建等 小叶丁香化学成分的研究(Ⅱ) 594页第2项 1、2 第34卷, 第07期 2 * |
| 《食品科学》 20100430 邓瑞雪等 小叶丁香中橄榄苦苷的纯化工艺研究 56页第一段、57页1.4项 1-5 第31卷, 第08期 2 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102246829A (en) * | 2011-07-28 | 2011-11-23 | 北京农学院 | Clove extract for killing nematode and preparation method thereof |
| CN102246829B (en) * | 2011-07-28 | 2013-05-01 | 北京农学院 | Clove extract for killing nematode and preparation method thereof |
| CN102579592A (en) * | 2012-02-20 | 2012-07-18 | 山东大学威海分校 | Syringa pubescens Turcz. bark extracts with protective effect on alcoholic liver injury |
| CN103405484A (en) * | 2013-08-26 | 2013-11-27 | 重庆工商大学 | Preparation method of patrinia villosa root anti-oxidization preparation |
| CN108976866A (en) * | 2018-08-06 | 2018-12-11 | 安徽三和工艺品有限公司 | A kind of bamboo rattan material wide spectrum mildew resistant paint |
| CN112245472A (en) * | 2020-11-25 | 2021-01-22 | 陕西科技大学 | Syringa microphylla seed extract and preparation method and application thereof |
| CN112245472B (en) * | 2020-11-25 | 2022-02-08 | 陕西帕尼尔生物科技有限公司 | Syringa microphylla seed extract and preparation method and application thereof |
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Open date: 20110209 |