CN103893216B - A kind of extracting and developing method of antioxidant composition in rough wood vinegar - Google Patents
A kind of extracting and developing method of antioxidant composition in rough wood vinegar Download PDFInfo
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- CN103893216B CN103893216B CN201410093045.8A CN201410093045A CN103893216B CN 103893216 B CN103893216 B CN 103893216B CN 201410093045 A CN201410093045 A CN 201410093045A CN 103893216 B CN103893216 B CN 103893216B
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Abstract
A kind of extracting and developing method of antioxidant composition in rough wood vinegar, relate to wood vinegar component extracting and developing method, the method is with rough wood vinegar as raw material, select dichloromethane as extractant, its extracting and developing process includes: measure the 100～200 rough wood vinegar of ml, extracts 1～3 time in the ratio of 1:1～1:5 volume ratio with dichloromethane, is dried by extract, obtain extractum, antioxidant activity is tracked；Calculate clearance rate and the IC of respective streams part sample50Value, screening obtains the active component that antioxidant activity is optimal.The present invention reduces the subtractive process that crude pyroligneous acid is conventional；Dichloromethane extraction yield is high, and extraction process is easy.Antioxidant activity optimum activity Component seperation rate is high.And this stream part scavenging ability of DPPH free radical is stronger, antioxidant activity is higher than two reference substances, has preferable antioxidant activity.
Description
Technical field
The present invention relates to wood vinegar component extracting and developing method, particularly relate to a kind of extracting and developing method of antioxidant composition in rough wood vinegar.
Background technology
Wood residue has originates widely, from forest harvesting residue, log producing material residue to wood machining residues, comprises various forms of waste wood goods and lignocellulosic articles.According to statistics, various garbages can account for the 50% of log scale.Produce the effective way that Linesless charcoal is deep exploitation wood residue, the Linesless charcoal with relatively high added value can be obtained, and wood vinegar can be collected, make wood residue obtain most complete utilization.
As the by-product of a kind of wildwood product, wood vinegar originates from the dry distilling industry of timber, is the cellulose in timber, hemicellulose and the product of lignin thermal decomposition.In broad terms, wood vinegar refers to a trees carbonization, its energy is converted into gas natural cooling again and becomes concentrated liquid.The component of wood vinegar and character are same and different also with different dry distilling raw materials and process for purification.Its main component relates to the compound of multiple types, containing hundreds of organic principles such as acid, ester, phenol, alcohol, furans and hydroxy kinds in major part wood vinegar, is a kind of component complexity, diverse in function and metastable system material.
At present, from natural plants and marine resources, extracting and developing effective ingredient has become as study hotspot as the product development of various uses.Wood vinegar does as a kind of natural plant resource and natural industrial chemicals, and containing a considerable number of Organic substance, its function is gradually excavated by people, can be widely used in all trades and professions.Agriculturally, wood vinegar can subtract pesticide, simplify fertilizer amount, sterilization anthelmintic, preserve the ecological environment.In rice field, use wood vinegar, owing to wood vinegar can improve the activity of water and soil earth microorganism, damping-off can be prevented and treated.In animal husbandry, wood vinegar can eliminate the stink in chicken farm of raising pigs, can improve meat as feed additive.Pharmaceutically, wood vinegar is effective to vitamin B1 deficiency, dermatosis, hepatopathy and diabetes.In light industry, owing to wood vinegar has the effect 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
It is an object of the invention to provide a kind of extracting and developing method of antioxidant composition in rough wood vinegar.The method is with logging residues such as the branch bar of seeds, leftover pieces as raw material, flue gas through producing in charcoal kiln smoldering makes its natural air cooling condense becomes liquid, it is rough wood vinegar (color pitchy) after ageing, then quantitative rough wood vinegar dichloromethane is extracted, obtain extractum, then filter out optimal antioxidant activity component.Decreasing the subtractive process that crude pyroligneous acid is conventional, dichloromethane extraction yield is high, and extraction process is easy.
The present invention can be achieved through the following technical solutions:
A kind of extracting and developing method of antioxidant content in rough wood vinegar, the method is with rough wood vinegar as raw material, selecting dichloromethane as extractant, its extracting and developing process includes: measure the 100～200 rough wood vinegar of ml, extracts 1～3 time in the ratio of 1:1～1:5 volume ratio with dichloromethane, extract is dried, obtain extractum, weigh 1～3 g extractum, use alcohol 95 %, percent by volume, dissolves；Use wet method dress post method to carry out macroporous resin loading, choose methanol-water solution 10%～100 %；Volume ratio, carries out eluting as eluent, the sample liquid point silica gel plate eluted, dark box type uv analyzer is carried out detection and is analyzed, obtains macroporous resin various flows part sample；Simultaneously, compound concentration vitamin E and vitamin C 0.2～10.0 μ g/ml and the rough wood vinegar of concentration, dichloromethane extract, macroporous resin stream part sample, it is DPPH(1, the 1-diphenyl-2-trinitrophenyl-hydrazine of 0.5～30.0 μ g/ml and 0.1～0.5 mmol) solution；Pipette DPPH solution and the rough wood vinegar of 50 ~ 100 μ l concentration, dichloromethane extract, macroporous resin stream part sample of 50 ~ 100 μ l, it is respectively placed in 96 orifice plates, lucifuge reaction 20～40 min, under 500 ~ 520 nm, survey its absorbance, the antioxidant activity of above-mentioned sample is tracked；Calculate clearance rate and the IC of respective streams part sample50Value, screening obtains the active component that antioxidant activity is optimal.
The extracting and developing method of antioxidant content in described a kind of rough wood vinegar, the IC of this antioxidant activity optimum activity component50Value is less than 8.0 μ g/ml, less than vitamin E and ascorbic IC50Value.
Advantages of the present invention with effect is:
1. the present invention is with rough wood vinegar as raw material, can make full use of wood vinegar resource.Meanwhile, selecting dichloromethane as extractant, extract color is limpid, golden yellow, decreases the subtractive process that crude pyroligneous acid is conventional；Dichloromethane extraction yield is high, and extraction process is easy.
Activity means of tracking is used during extracting and developing the most of the present invention, rough wood vinegar, dichloromethane extract and the various flows part sample through macroporous resin isolated are monitored in real time, screening active ingredients and separating technology are easy, and antioxidant activity optimum activity Component seperation rate is high.And this stream part scavenging ability of DPPH free radical is stronger, antioxidant activity is higher than two reference substances, has preferable antioxidant activity.
Accompanying drawing explanation
Fig. 1 is crude pyroligneous acid, dichloromethane extract, antioxidant activity optimum activity component and the active testing figure of two kinds of antioxidant activity reference substances (VE, VC).
Detailed description of the invention
Embodiment 1:
The extracting and developing method of antioxidant composition in a kind of rough wood vinegar of the present invention.Mainly realized by following steps: measure the about 100～200 rough wood vinegar of ml, with dichloromethane in 1:1～1:5(volume ratio) ratio extract 1～3 time, extract is dried, obtain extractum, weigh about 1～3 g extractum, dissolve with ethanol (95%, percent by volume)；It is respectively adopted wet method dress post method and carries out macroporous resin loading, choose methanol-water solution (10%～100 %；Volume ratio) carry out eluting as eluent, the sample liquid point silica gel plate eluted, dark box type uv analyzer are carried out detection and analyze, obtains macroporous resin various flows part and divide sample.Simultaneously, use tracking activity means, i.e. prepare the vitamin E of variable concentrations and vitamin C (0.2～10.0 μ g/ml) and the rough wood vinegar of variable concentrations, dichloromethane extract, macroporous resin stream part sample (being 0.5～30.0 μ g/ml) and DPPH(1, the 1-diphenyl-2-trinitrophenyl-hydrazine of 0.1～0.5 mmol) solution.Pipette DPPH solution and the rough wood vinegar of 50 ~ 100 μ l variable concentrations, dichloromethane extract, macroporous resin stream part sample of 50 ~ 100 μ l, it is respectively placed in 96 orifice plates, lucifuge reaction 20～40 min, under 500 ~ 520 nm, survey its absorbance, the antioxidant activity of above-mentioned sample is tracked.Calculate clearance rate and the IC of respective streams part sample50Value, screening obtains the active component that antioxidant activity is optimal.
The present invention, with rough wood vinegar as raw material, selects dichloromethane as extractant, and extract color is limpid, golden yellow, decreases the subtractive process that crude pyroligneous acid is conventional；Every 1000 mL crude pyroligneous acids are evaporated and can obtain about 20 ~ 30g dry cream of crude pyroligneous acid, are dried available 10 ~ 15g dichloromethane extract through extraction.Dichloromethane extraction yield is more than 50 %, and extraction process is easy.Using activity means of tracking during the extracting and developing of this method, monitor rough wood vinegar, dichloromethane extract and the various flows part sample through macroporous resin isolated in real time, screening active ingredients and separating technology are easy.Every 1000 mL crude pyroligneous acids are through being evaporated, and extraction is dried, and cross macroporous resin column and obtain flowing part 2 about 0.5 ~ 1.0 g, and this antioxidant activity optimum activity Component seperation rate is more than 20 %.And this stream part scavenging ability of DPPH free radical is stronger, by the clearance rate of accompanying drawing 1, is computed the IC of antioxidant activity optimum activity component50Value is less than 8.0 μ g/ml, less than vitamin E and ascorbic IC50Value, illustrates that it has preferable antioxidant activity.
Claims (1)
1. the extracting and developing method of antioxidant content in a rough wood vinegar, it is characterized in that, the method is with rough wood vinegar as raw material, selecting dichloromethane as extractant, its extracting and developing process includes: measure the 100～200 rough wood vinegar of ml, is that the ratio of 1:1～1:5 extracts 1～3 time by volume with dichloromethane, extract is dried, obtain extractum, weigh 1～3 g extractum, dissolve with the ethanol that percent by volume is 95%；Wet method dress post method is used to carry out macroporous resin loading, choose volume ratio percentage ratio be 10%～100 the methanol-water solution of % carry out eluting as eluent, the sample liquid point silica gel plate eluted, dark box type uv analyzer are carried out detection and analyze, obtains macroporous resin various flows part sample；Meanwhile, compound concentration is the vitamin E of 0.2～10.0 μ g/ml and vitamin C and concentration is the rough wood vinegar of 0.5～30.0 μ g/ml, dichloromethane extract, macroporous resin stream part sample and DPPH solution that concentration is 0.1～0.5 mmol；The DPPH solution and the volume that pipette 50 ~ 100 μ l are the rough wood vinegar of 50 ~ 100 μ l, dichloromethane extract, macroporous resin stream part sample, it is respectively placed in 96 orifice plates, lucifuge reaction 20～40 min, under 500 ~ 520 nm, survey its absorbance, the antioxidant activity of above-mentioned sample is tracked；Calculate clearance rate and the IC of respective streams part sample50Value, screening obtains the active component that antioxidant activity is optimal, the IC of this antioxidant activity optimum activity component50Value is less than 8.0 μ g/ml, less than vitamin E and ascorbic IC50Value.
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| 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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| 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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| 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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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 |
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