CN103893216A - Method for extracting and separating antioxidant components from crude wood vinegar liquid - Google Patents
Method for extracting and separating antioxidant components from crude wood vinegar liquid Download PDFInfo
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- CN103893216A CN103893216A CN201410093045.8A CN201410093045A CN103893216A CN 103893216 A CN103893216 A CN 103893216A CN 201410093045 A CN201410093045 A CN 201410093045A CN 103893216 A CN103893216 A CN 103893216A
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Abstract
The invention discloses a method for extracting and separating antioxidant components from a crude wood vinegar liquid and relates to a method for extracting and separating components of the wood vinegar liquid. The method takes the crude wood vinegar liquid as a raw material and selects dichloromethane as an extraction agent. The method comprises the following extracting and separating processes: taking 100-200 ml of the crude wood vinegar liquid to extract with the dichloromethane for 1-3 times according to a volume ratio of (1:1)-(1:5), drying an extraction liquid to obtain extractum, and tracking antioxidant activity; and calculating removal rates and IC50 (50% Inhibiting Concentration) values of corresponding fraction samples and screening the samples to obtain an activity component with an optimum antioxidant activity. Through the method, a normal refining process of the crude wood vinegar liquid is reduced; the dichloromethane is high in extraction rate and simple in extraction process; macroporous resin fraction is high in separation rate; and meanwhile, the fraction is strong in capability of removing DPPH (Diphenyl Picrylhydrazyl) free radicals and good in antioxidant activity being higher than that of two reference substances.
Description
Technical field
The present invention relates to the extraction of wood vinegar component, separation method, particularly relate to extraction, the separation method of antioxidant composition in a kind of rough wood vinegar.
Background technology
Wood residue has source widely, from forest harvesting residue, log producing material residue to wood machining residues, comprises various forms of waste wood goods and wood fibre goods.According to statistics, various garbages can account for 50% of log scale.Producing Linesless charcoal is the effective way of deep exploitation wood residue, can obtain the Linesless charcoal having compared with high added value, and can collect wood vinegar, makes wood residue obtain utilizing the most completely.
As a kind of by-product of wildwood product, wood vinegar originates from the dry distilling industry of timber, is the product of cellulose, hemicellulose and lignin thermal decomposition in timber.In broad terms, wood vinegar refers to a trees carbonization, by its power conversion become gas again natural cooling become concentrated liquid.Also same and different along with different dry distilling raw materials and process for purification of the component of wood vinegar and character.Its main component relates to the compound of multiple types, contains hundreds of organic principles such as acid, ester, phenol, alcohol, furans and hydroxy kind in most of wood vinegar, is a kind of component complexity, diverse in function and metastable system material.
At present, from natural plants and marine resources, extraction, separating effective ingredient have become study hotspot as the product development of various uses.Wood vinegar does as a kind of natural plant resource and natural industrial chemicals, contains a considerable number of Organic substance, and its function is excavated by people gradually, can be widely used in all trades and professions.In agricultural, wood vinegar can subtract pesticide, simplify fertilizer amount, sterilization anthelmintic, preserve the ecological environment.In rice field, use wood vinegar, because wood vinegar can improve the activity of water and soil microorganism, can prevent and treat damping-off.In animal husbandry, wood vinegar can be eliminated the stink in the chicken farm of raising pigs, and can improve meat as feed additive.Pharmaceutically, wood vinegar is effective to vitamin B1 deficiency, dermatosis, hepatopathy and diabetes.In light industry, because wood vinegar has the effects such as anticorrosion, antioxidation, for the additive of makeup, bath foam and food and drink etc.(Doran W.L., 1932; This hero of palace one, 1962; Rodolfo, et al., 1975; Ohta, et al., 1994; Piao Zhe etc., 2003; Ma Jianyi, 2013).
Summary of the invention
The object of the present invention is to provide extraction, the separation method of antioxidant composition in a kind of rough wood vinegar.The method is taking the logging residues such as branch bar, leftover pieces of seeds as raw material, through the flue gas producing in charcoal kiln smoldering, its natural air cooling is condensed and become liquid, after ageing, be rough wood vinegar (color pitchy), then quantitative rough wood vinegar is extracted with dichloromethane, obtain extractum, then filter out best antioxidant activity component.The subtractive process that has reduced crude pyroligneous acid routine, dichloromethane extraction rate is high, and extraction process is easy.
The present invention can be achieved through the following technical solutions:
Extraction, the separation method of antioxidant content in a kind of rough wood vinegar, the method is taking rough wood vinegar as raw material, select dichloromethane as extractant, it extracts, separation process comprises: measure the rough wood vinegar of 100～200 ml, extract 1～3 time in the ratio of 1:1～1:5 volume ratio with dichloromethane, extract is dry, obtain extractum, take 1～3 g extractum, use alcohol 95 %, percent by volume, dissolves; Adopt wet method dress post method to carry out macroporous resin loading, choose methanol-water system 10%～100 %; Volume ratio, carries out eluting as eluent, and the sample liquid point silica gel plate eluting, dark box type uv analyzer are detected to analysis, obtains macroporous resin various flows duplicate samples; Simultaneously, configuration concentration vitamin E and vitamin C 0.2～10.0 μ g/ml and the rough wood vinegar of concentration, dichloromethane extraction liquid, macroporous resin flow point sample, be the DPPH(1 of 0.5～30.0 μ g/ml and 0.1～0.5 mmol, 1-diphenyl-2-trinitrophenyl-hydrazine) solution; Pipette the DPPH solution of 50 ~ 100 μ l and the rough wood vinegar of 50 ~ 100 μ l concentration, dichloromethane extraction liquid, macroporous resin flow point sample, be placed in respectively 96 orifice plates, lucifuge reaction 20～40 min, under 500 ~ 520 nm, survey its absorbance, the antioxidant activity of above-mentioned sample is followed the tracks of; Calculate clearance rate and the IC of corresponding flow point sample
50value, 503nhibiting concentration, screening obtains the active component of antioxidant activity the best.
Extraction, the separation method of antioxidant content in described a kind of rough wood vinegar, the IC of the method macroporous resin stream 2
50value is lower than 8.0 μ g/ml, lower than vitamin E and ascorbic IC
50value.
Advantage of the present invention and effect are:
1. the present invention, taking rough wood vinegar as raw material, can make full use of wood vinegar resource.Meanwhile, select dichloromethane as extractant, extract color is limpid, and golden yellow has reduced the subtractive process of crude pyroligneous acid routine; Dichloromethane extraction rate is high, and extraction process is easy.
2. in extraction of the present invention, separation process, adopt active means of tracking, to rough wood vinegar, dichloromethane extraction liquid with separate the different flow point samples that obtain through macroporous resin and carry out Real-Time Monitoring, screening active ingredients and separating technology are easy, and macroporous resin flow point 2 separation rates are high.And this fraction scavenging ability of DPPH free radical is more intense, antioxidant activity, higher than two reference substances, has good antioxidant activity.
Brief description of the drawings
Fig. 1 is the active testing figure of crude pyroligneous acid, dichloromethane extraction liquid, macroporous resin flow point 2 and two kind of antioxidant activity reference substance (VE, VC).
Detailed description of the invention
Embodiment 1:
Extraction, the separation method of antioxidant composition in a kind of rough wood vinegar of the present invention.Mainly realize by following steps: measure the rough wood vinegar of approximately 100～200 ml, with dichloromethane in 1:1～1:5(volume ratio) ratio extraction 1～3 time, extract is dry, obtain extractum, take approximately 1～3 g extractum, use ethanol (95%, percent by volume) to dissolve; Adopt respectively wet method dress post method to carry out macroporous resin loading, choose methanol-water system (10%～100 %; Volume ratio) carry out eluting as eluent, the sample liquid point silica gel plate eluting, dark box type uv analyzer are detected to analysis, obtain macroporous resin various flows part and divide sample.Simultaneously, adopt active tracking means, configure the vitamin E of variable concentrations and the DPPH(1 of vitamin C (0.2～10.0 μ g/ml) and the rough wood vinegar of variable concentrations, dichloromethane extraction liquid, macroporous resin flow point sample (being 0.5～30.0 μ g/ml) and 0.1～0.5 mmol, 1-diphenyl-2-trinitrophenyl-hydrazine) solution.Pipette the DPPH solution of 50 ~ 100 μ l and the rough wood vinegar of 50 ~ 100 μ l variable concentrations, dichloromethane extraction liquid, macroporous resin flow point sample, be placed in respectively 96 orifice plates, lucifuge reaction 20～40 min, under 500 ~ 520 nm, survey its absorbance, the antioxidant activity of above-mentioned sample is followed the tracks of.Calculate clearance rate and the IC of corresponding flow point sample
50value, screening obtains the active component of antioxidant activity the best.
The present invention, taking rough wood vinegar as raw material, selects dichloromethane as extractant, and extract color is limpid, and golden yellow has reduced the subtractive process of crude pyroligneous acid routine; Every 1000 mL crude pyroligneous acid evaporates to dryness can obtain the approximately dry cream of 20 ~ 30g crude pyroligneous acid, can obtain 10 ~ 15g dichloromethane extract through extracting to be dried.Dichloromethane extraction rate is greater than 50 %, and extraction process is easy.In the extraction of this method, separation process, adopt active means of tracking, to rough wood vinegar, dichloromethane extraction liquid with separate the different flow point samples that obtain through macroporous resin and carry out Real-Time Monitoring, screening active ingredients and separating technology are easy.Every 1000 mL crude pyroligneous acids are through evaporate to dryness, and extraction is dry, and mistake macroporous resin column obtains flow point 2 and is about 0.5 ~ 1.0 g, and macroporous resin flow point 2 separation rates are greater than 20 %.And this flow point scavenging ability of DPPH free radical is more intense, by the clearance rate of accompanying drawing 1, the IC of macroporous resin stream 2 as calculated
50value is lower than 8.0 μ g/ml, lower than vitamin E and ascorbic IC
50value, illustrates that it has good antioxidant activity.
Claims (2)
1. extraction, the separation method of antioxidant content in a rough wood vinegar, it is characterized in that, the method, taking rough wood vinegar as raw material, selects dichloromethane as extractant, it extracts, separation process comprises: measure the rough wood vinegar of 100～200 ml, in the ratio extraction of 1:1～1:5 volume ratio 1～3 time, extract is dry with dichloromethane, obtain extractum, take 1～3 g extractum, use alcohol 95 %, percent by volume, dissolves; Adopt wet method dress post method to carry out macroporous resin loading, choose methanol-water system 10%～100 %; Volume ratio, carries out eluting as eluent, and the sample liquid point silica gel plate eluting, dark box type uv analyzer are detected to analysis, obtains macroporous resin various flows duplicate samples; Simultaneously, configuration concentration vitamin E and vitamin C 0.2～10.0 μ g/ml and the rough wood vinegar of concentration, dichloromethane extraction liquid, macroporous resin flow point sample, be the DPPH(1 of 0.5～30.0 μ g/ml and 0.1～0.5 mmol, 1-diphenyl-2-trinitrophenyl-hydrazine) solution; Pipette the DPPH solution of 50 ~ 100 μ l and the rough wood vinegar of 50 ~ 100 μ l concentration, dichloromethane extraction liquid, macroporous resin flow point sample, be placed in respectively 96 orifice plates, lucifuge reaction 20～40 min, under 500 ~ 520 nm, survey its absorbance, the antioxidant activity of above-mentioned sample is followed the tracks of; Calculate clearance rate and the IC of corresponding flow point sample
50value, 503nhibiting concentration, screening obtains the active component of antioxidant activity the best.
2. extraction, the separation method of antioxidant content in a kind of rough wood vinegar according to claim 1, is characterized in that, the IC of the method macroporous resin stream 2
50value is lower than 8.0 μ g/ml, lower than vitamin E and ascorbic IC
50value.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104164248A (en) * | 2014-08-28 | 2014-11-26 | 桂林市艾康科技有限公司 | Preparation method of refined bamboo vinegar |
| CN108813275A (en) * | 2018-05-02 | 2018-11-16 | 黑龙江八农垦大学 | A kind of corn stover wood vinegar antioxidant and application |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001012178A1 (en) * | 1999-08-16 | 2001-02-22 | Microplants Co., Ltd | Method for isolating chlorogenic acid and 1,4-di-o-caffeoyl-d-(+)-quinic acid |
| CN1931960A (en) * | 2006-10-11 | 2007-03-21 | 涂志龙 | Prepn process of refined bamboo vinegar liquid |
| CN101185527A (en) * | 2007-08-03 | 2008-05-28 | 浙江省林业科学研究院 | Anti-oxidant containing wood and bamboo vinegar liquid extract and preparing method and application thereof |
| CN101697738A (en) * | 2009-10-27 | 2010-04-28 | 西北农林科技大学 | Method for continuously extracting antibactial substances and antioxidant substances from pyrolignucs acid |
| CN102899069A (en) * | 2012-10-30 | 2013-01-30 | 复旦大学 | Separating and upgrading method of bio-oil by column chromatography |
-
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2001012178A1 (en) * | 1999-08-16 | 2001-02-22 | Microplants Co., Ltd | Method for isolating chlorogenic acid and 1,4-di-o-caffeoyl-d-(+)-quinic acid |
| CN1931960A (en) * | 2006-10-11 | 2007-03-21 | 涂志龙 | Prepn process of refined bamboo vinegar liquid |
| CN101185527A (en) * | 2007-08-03 | 2008-05-28 | 浙江省林业科学研究院 | Anti-oxidant containing wood and bamboo vinegar liquid extract and preparing method and application thereof |
| CN101697738A (en) * | 2009-10-27 | 2010-04-28 | 西北农林科技大学 | Method for continuously extracting antibactial substances and antioxidant substances from pyrolignucs acid |
| CN102899069A (en) * | 2012-10-30 | 2013-01-30 | 复旦大学 | Separating and upgrading method of bio-oil by column chromatography |
Non-Patent Citations (1)
| Title |
|---|
| 邹勇: "木屑快速热解生物油中酚类提取物的抗氧化及抑真菌活性研究", 《西北林学院学报》, vol. 29, no. 1, 15 January 2014 (2014-01-15), pages 117 - 118 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104164248A (en) * | 2014-08-28 | 2014-11-26 | 桂林市艾康科技有限公司 | Preparation method of refined bamboo vinegar |
| CN108813275A (en) * | 2018-05-02 | 2018-11-16 | 黑龙江八农垦大学 | A kind of corn stover wood vinegar antioxidant and application |
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Inventor after: Gao Pinyi Inventor after: Liu Xuegui Inventor after: Zhang Zhenxue Inventor before: Liu Xuegui Inventor before: Gao Pinyi Inventor before: Wang Jilin Inventor before: Jin Mei Inventor before: Nian Zhongfeng Inventor before: Yang Di Inventor before: Zhang Zhenxue |