CN102551170A - High efficiency preparation method of burdock leaf natural antioxidant - Google Patents
High efficiency preparation method of burdock leaf natural antioxidant Download PDFInfo
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- CN102551170A CN102551170A CN2010105796279A CN201010579627A CN102551170A CN 102551170 A CN102551170 A CN 102551170A CN 2010105796279 A CN2010105796279 A CN 2010105796279A CN 201010579627 A CN201010579627 A CN 201010579627A CN 102551170 A CN102551170 A CN 102551170A
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Abstract
The invention relates to a high efficiency preparation method of a burdock leaf natural antioxidant. The preparation method comprises the following characteristic steps: 1, crushing dry burdock leaves, adding water, carrying out composite enzyme process extraction to obtain an aqueous extract of the antioxidant, and concentrating to obtain a concentrate 1; 2, adding an ethanol solution to burdock leaf residues subjected to enzymatic hydrolysis, carrying out ultrasonic microwave synergistic extraction, and filtering to obtain an ethanol extract; 3, carrying out reduced pressure concentration on the ethanol extract until no solvent exists to obtain a concentrate a; 4, dispersing the concentrate a in water, adding the concentrate 1, extracting by solvents of hexane, ether, petroleum ether and the like, removing impurities of pigments and the like, and reserving the obtained water phase; and 5, adding n-butanol, ethyl acetate and the like to the water phase, extracting to obtain an extract, concentrating, and drying to obtain the burdock leaf natural antioxidant. According to the invention, the ultrasonic microwave synergistic extraction technology and the biological enzyme technology are utilized to extract, so the extraction time is substantially shortened, and the extraction rate is improved. The antioxidant activity of the antioxidant prepared in the invention is stronger than the antioxidant activity of TBHQ (tertiary butylhydroquinone).
Description
Technical field
The present invention relates to the method for extraction, separating natural anti-oxidant from the burdock leaf, particularly utilize ultrasonic-microwave synergic solvent extraction technology and complex enzyme technology to extract the method for natural.
Background technology
According to statistics, China's burdock output is big, reaches 1500Kg like radix bardanae in the per mu yield of Xuzhou Area, and leaf is about every mu of 1000Kg.This all discards the burdock phyllopodium, has caused the serious wasting of resources, and easy contaminated environment.And the active ingredient that contains in the burdock leaf has oxidation resistance.Therefore the polyphenol component in the burdock leaf is developed and utilized, both can fully utilize waste resource, can prepare a large amount of oxidation-resistant active ingredients again, have important economy, social effect.
At present, the anti-oxidant that food service industry is used, the overwhelming majority all is artificial synthetic, can cause many problems that are detrimental to health when edible too much.The quick raising of Along with people's living standard, people more and more distrust for synthetic additive, and show increasing interest for green, natural additive, people increase for the increasing demand of natural.Meanwhile, more and more many scholars begin to pay close attention to and the research natural component, comprise the preparation of various natural components and the evaluation of antioxidation activity.Research shows that the burdock leaf is rich in polyphenol component, is a kind of good source that can suppress Food Oxidation.
Extraction is to utilize plant material to prepare the committed step of natural.Ultrasonic wave leaching method is a kind of physical strengthening extractive technique.Ultrasonic wave is a kind of mechanical wave in the elastic fluid, utilizes institutional framework, state, the function of ultrasonic vibrational energy change material or quickens its change process.Extraction by Ultrasound is widely used aspect natural product extraction as a kind of novel extractive technique, have extraction time short, extraction efficiency is high, be extracted advantages such as active material is not destroyed.
Microwave technology is applied to the extraction of effective ingredients in plant, and the fuel factor of microwave can make the inner moisture of host material heat up and vaporization on the one hand, and heating up rapidly causes the host material structure to change, and it is loose that material becomes, and reduced resistance to mass tranfer; The non-thermal effect of microwave can make the reaction force attenuation between each component in the host material on the other hand, and desorption strengthens, and solubility improves, thereby reaches the purpose that significantly improves extraction effect.Big quantity research shows that the microwave assisted extraction has shortened extraction time greatly, extracts yield and also significantly improves.
Ultrasonic-microwave synergic solvent extraction is as a kind of brand-new isolation technics (principle is seen accompanying drawing); In conjunction with advantages ultrasonic, two kinds of technology of microwave; Produced better extraction separating effect; Adopting ultrasonic-microwave synergic solvent extraction technology preparation (burdock leaf) natural is a kind of new trial, and extraction time shortens dramatically, and extraction efficiency improves greatly.Ultrasonic-microwave synergic solvent extraction technology is combined with biological enzyme technology, and the preparation natural possibly have greater advantages, and this method is not appeared in the newspapers.
Summary of the invention
Technical scheme of the present invention is in order to overcome the health hazard that synthetized oxidation preventive agent causes; And a kind of production method of natural burdock leaf anti-oxidant is provided; This method can the suitability for industrialized production natural, and the natural oxidation resistance of being produced is strong, and practicality is good.And this method employing ultrasonic-microwave synergic solvent extraction technology and complex enzyme extractive technique, speed is fast, and production efficiency improves greatly.In addition, raw material-burdock leaf that the present invention is used is a kind of discarded object, and cost is very low, is another advantage of the present invention.
Technical scheme of the present invention is:
1, the high efficiency preparation method of burdock leaf natural.Its characterization step is:
(1) dried burdock leaf is pulverized, sieved; Burdock leaf powder is mixed with water, and the mass ratio of burdock leaf powder and water is 1: 5-1: 30.Add complex enzyme and carry out enzymolysis, filter then, obtain anti-oxidant water extract, concentrate, be concentrate 1.Gained burdock leaf residue is for use.Used complex enzyme is made up of cellulase and pectase, and the ratio of cellulase and pectase is 1: 1-1: 3.The complex enzyme addition is 2-80mg/g (a burdock leaf).
(2) in burdock leaf residue, add ethanolic solution as solvent, carry out ultrasonic-microwave synergic solvent extraction.Filter.Supernatant concentration to solvent-free, is obtained concentrate a.Wherein, the mass fraction of ethanolic solution is 15-70%, and the mass ratio of used burdock leaf powder was 5 when ethanolic solution began with experiment: 1-30: 1.Ultrasonic power is 0.05-1Kw, and microwave power is 0.1-2.5Kw, and extraction time is 0.5-50min.
(3) concentrate a is scattered in the water, adds concentrate 1, adopt organic solvents such as n-hexane, ether, benzinum repeatedly to extract earlier, remove impurity; Keep water.
(4) aqueous phase after extraction last time adds n-butanol, ethyl acetate etc., repeatedly extracts, and keeps the organic facies on upper strata, promptly obtains extract A.
(5) extract A decompression is concentrated, drying promptly obtains natural.
The invention has the beneficial effects as follows:
1, compare with other natural inhibitors preparation method, the present invention combines new ultrasonic-microwave synergic solvent extraction technology with the complex enzyme technology, extract natural, and this method is not appeared in the newspapers.
2, method of the present invention can realize suitability for industrialized production burdock leaf natural, provides the foundation for natural substitutes synthetized oxidation preventive agent.
3, the present invention has carried out the abstraction purification processing to extract, has prepared the very high natural of antioxidation activity, and the oxidation resistance of prepared anti-oxidant is better than TBHQ.
Oxidation resistance is measured:
The DPPH experiment: with burdock leaf anti-oxidant to be measured and TBHQ dissolving, and be diluted to serial solution, press table 2 application of sample, light absorption value is measured in the lucifuge reaction under the 517nm wavelength after 10 minutes.Replication 5 times, results averaged.Clearance rate (%)=(1-(A
i-A
j)/A
0) * 100%.
Table 2 DPPH experiment application of sample table and corresponding light absorption value
DPPH removes ability often with IC
50Represent.IC
50Be meant under experiment condition, remove 50% the required lowest drug concentration of DPPH free radical.5 times result of experiment shows: the IC of burdock leaf anti-oxidant and TBHQ
50Be respectively: 91.03 μ g/mL and 105.62 μ g/mL; It is thus clear that burdock leaf antioxidant has stronger oxidation resistance.
Description of drawings
Fig. 1 is a ultrasonic-microwave synergic solvent extraction principle of device sketch map
The specific embodiment
Below provide embodiment, the present invention is described further.
Embodiment 1
Get dried burdock leaf 5g, be crushed to below 100 orders, sieve; Add 50mL water as extracting solvent.Add the 250mg complex enzyme, carry out enzymolysis.Filter, obtain anti-oxidant water extract, concentrate, obtain concentrate 1.In burdock leaf residue, add the 30mL mass fraction and be 15% ethanolic solution as solvent, carry out ultrasonic-microwave synergic solvent extraction, ultrasonic power is 50w, and microwave power is 200w, and extraction time is 7min.Filter.Supernatant is evaporated to solvent-free, obtains concentrate a.Concentrate a is scattered in the water, adds concentrate 1, adopt n-hexane extraction 3 times earlier, remove impurity; Merge water.Add n-butanol to aqueous phase, extract 4 times, 40 ℃ of decompressions of extract are concentrated, 65 ℃ of vacuum drying make burdock leaf anti-oxidant, and final yield is a 45.55mg/g burdock leaf.
Through measuring, the main component of gained burdock leaf anti-oxidant is a polyphenol, and polyphenol content is 257.36mg/g.Measure the IC of burdock leaf anti-oxidant, Vc, TBHQ removing DPPH free radical according to foregoing method
50Value is tested 3 times, averages.The result shows, the IC of gained burdock leaf antioxidant for clearing DPPH free radical
50Value is 91.11 μ g/mL, and the IC of Vc, TBHQ removing DPPH free radical
50Value is respectively: 127.87 μ g/mL and 105.68 μ g/mL, therefore, to compare with Vc, TBHQ, and burdock leaf anti-oxidant has stronger antioxidation activity.
Embodiment 2
Get dried burdock leaf 1000g, pulverize, cross 50 mesh sieves, add 30L water, mixing.Add the 10g complex enzyme, carry out enzymolysis.Filter, obtain anti-oxidant water extract, concentrate, obtain concentrate 1.Adding 20L mass fraction is 30% ethanolic solution in the burdock leaf residue that first step extraction obtains, and fully mixes.Act on simultaneously at 200w ultrasonic wave, 900w microwave and to handle down 30min, filter, extract, 50 ℃ are evaporated to solvent-freely, obtain concentrate a.Concentrate a and concentrate 1 are merged, adopt petroleum ether extraction 8 times, merge remaining water, use the ethyl acetate extraction water again 3 times, 50 ℃ of decompressions of extract are concentrated, spray-drying makes burdock leaf anti-oxidant, and final yield is a 50.87mg/g burdock leaf.The polyphenol content of gained burdock leaf anti-oxidant is 238.20mg/g, the IC of gained burdock leaf antioxidant for clearing DPPH free radical
50Value is 91.02 μ g/mL.
Embodiment 3
Get dried burdock leaf 200g, pulverize, cross 50 mesh sieves, add 1.5L water, add the 1g complex enzyme successively and carry out enzymolysis.Filter then, obtain anti-oxidant water extract, concentrate, obtain concentrate 1.Adding 3L mass fraction is 50% ethanolic solution in the burdock leaf residue of gained, fully mixes.Act on simultaneously at 900w ultrasonic wave, 2000w microwave and to handle down 3min, filter, extract, 45 ℃ are evaporated to solvent-freely, obtain concentrate a.Concentrate a and concentrate 1 are merged, adopt n-hexane extraction 7 times, merge water.Aqueous phase to extraction last time adds n-butanol, extracts 9 times, and 55 ℃ of decompressions of extract are concentrated, and 700W microwave drying aid makes burdock leaf anti-oxidant, and its final yield is a 47.10mg/g burdock leaf.
Through measuring, the main component of gained burdock leaf anti-oxidant is a polyphenol, and polyphenol content is 261.43mg/g.Measure the IC of burdock leaf anti-oxidant, Vc, TBHQ removing DPPH free radical according to foregoing method
50Value is tested three times, averages.The result shows, the IC of gained burdock leaf antioxidant for clearing DPPH free radical
50Value is 91.18 μ g/mL, and the IC of Vc, TBHQ removing DPPH free radical
50Value is respectively: 127.76 μ g/mL and 105.57 μ g/mL, therefore, to compare with Vc, TBHQ, and burdock leaf anti-oxidant has stronger antioxidation activity.
Claims (6)
1. the high efficiency preparation method of burdock leaf natural.Its characterization step is:
(1) dried burdock leaf is pulverized, sieved; Burdock leaf powder is mixed with water.Add complex enzyme and carry out enzymolysis, filter then, obtain anti-oxidant water extract, concentrate, be concentrate 1.Gained burdock leaf residue is for use.
(2) in burdock leaf residue, add ethanolic solution as solvent, ultrasonic-microwave synergic solvent extraction is filtered.Supernatant concentration to solvent-free, is obtained concentrate a.
(3) concentrate a is scattered in the water, adds concentrate 1, adopt organic solvents such as n-hexane, ether, benzinum repeatedly to extract earlier, remove impurity; Keep water.
(4) aqueous phase after extraction last time adds n-butanol, ethyl acetate etc., repeatedly extracts, and keeps the organic facies on upper strata, promptly obtains extract A.
(5) extract A is concentrated, drying promptly obtains natural.
2. the high efficiency preparation method of burdock leaf natural according to claim 1, it is characterized in that step (1) condition is: dried burdock leaf is crushed to below the 20-100 order, and the mass ratio of burdock leaf powder and water is 1: 5-1: 30.Complex enzyme is made up of cellulase and pectase, and the ratio of cellulase and pectase is 1: 1-1: 3.The complex enzyme addition is 2-80mg/g (a burdock leaf).
3. the high efficiency preparation method of burdock leaf natural according to claim 1; It is characterized in that step (2) ultrasonic-microwave synergic solvent extraction; Its condition is: in the burdock leaf residue that step (1) obtains, add solvent; Solvent is that mass fraction is the ethanolic solution of 15-70%, and the mass ratio of used burdock leaf powder was 5 when ethanolic solution began with experiment: 1-30: 1, and carry out ultrasonic-microwave synergic solvent extraction.Ultrasonic power is 0.05-1Kw, and microwave power is 0.1-2.5Kw, and extraction time is 0.5-50min.
4. the high efficiency preparation method of burdock leaf natural according to claim 1 is characterized in that step (3) condition is: adopt organic solvents such as n-hexane, ether, benzinum, repeatedly extraction.
5. the high efficiency preparation method of burdock leaf natural according to claim 1 is characterized in that step (4) condition is: adopt organic solvents such as ethyl acetate, n-butanol, repeatedly extraction.
6. the high efficiency preparation method of burdock leaf natural according to claim 1 is characterized in that step (5) condition is: 40-70 ℃ of decompression concentrates, 50-70 ℃ of vacuum drying or 70-100 ℃ of spray-drying or 0.5-2Kw microwave drying aid.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103960300A (en) * | 2013-02-01 | 2014-08-06 | 江南大学 | Method for preparation of mould inhibitor from burdock leaves |
| CN103960299A (en) * | 2013-02-01 | 2014-08-06 | 江南大学 | Preparation method for bacterial biofilm inhibitor |
| CN105132118A (en) * | 2015-09-25 | 2015-12-09 | 海南大学 | Coconut oil extraction method |
| CN105533050A (en) * | 2015-12-31 | 2016-05-04 | 尹佳妮 | Radix millettiae speciosae tea and preparation method thereof |
| CN106805180A (en) * | 2017-01-13 | 2017-06-09 | 江南大学 | A kind of method that polyphenol substance is extracted in desmoenzyme and the ultrasonically treated endotesta walnut kernel by band |
| CN109329940A (en) * | 2018-12-14 | 2019-02-15 | 洛阳采方医药科技有限公司 | A kind of food grade antioxidants and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101602818A (en) * | 2009-07-07 | 2009-12-16 | 江南大学 | A kind of method of utilizing ultrasonic-microwave extraction to prepare edible burdock inulin |
-
2010
- 2010-12-09 CN CN2010105796279A patent/CN102551170A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101602818A (en) * | 2009-07-07 | 2009-12-16 | 江南大学 | A kind of method of utilizing ultrasonic-microwave extraction to prepare edible burdock inulin |
Non-Patent Citations (5)
| Title |
|---|
| 娄在祥等: "微波辅助提取牛蒡叶多酚及其抗氧化、抗菌活性研究", 《食品与发酵工业》 * |
| 娄在祥等: "牛蒡叶多酚的超声波辅助提取及抗氧化活性、成分分析研究", 《食品工业科技》 * |
| 滕道祥等: "牛蒡多酚的提取及清除DPPH自由基的研究", 《安徽农业科学》 * |
| 马利华等: "牛蒡提取物体外抗氧化性的研究", 《食品与机械》 * |
| 马利华等: "超声波-微波协同提取牛蒡叶中类胡萝卜素", 《食品研究与开发》 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103960300A (en) * | 2013-02-01 | 2014-08-06 | 江南大学 | Method for preparation of mould inhibitor from burdock leaves |
| CN103960299A (en) * | 2013-02-01 | 2014-08-06 | 江南大学 | Preparation method for bacterial biofilm inhibitor |
| CN103960299B (en) * | 2013-02-01 | 2016-09-28 | 江南大学 | A kind of method preparing bacterial biof iotalm inhibitor |
| CN103960300B (en) * | 2013-02-01 | 2016-12-28 | 江南大学 | A kind of method utilizing Herba Arctii leaf to prepare mould inhibitor |
| CN105132118A (en) * | 2015-09-25 | 2015-12-09 | 海南大学 | Coconut oil extraction method |
| CN105533050A (en) * | 2015-12-31 | 2016-05-04 | 尹佳妮 | Radix millettiae speciosae tea and preparation method thereof |
| CN106805180A (en) * | 2017-01-13 | 2017-06-09 | 江南大学 | A kind of method that polyphenol substance is extracted in desmoenzyme and the ultrasonically treated endotesta walnut kernel by band |
| CN109329940A (en) * | 2018-12-14 | 2019-02-15 | 洛阳采方医药科技有限公司 | A kind of food grade antioxidants and preparation method thereof |
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Application publication date: 20120711 |