CN103751317A - Method for extracting hovenia dulcis thunb total flavones by cooperation of surfactant and microwave-ultrasonic extraction process - Google Patents
Method for extracting hovenia dulcis thunb total flavones by cooperation of surfactant and microwave-ultrasonic extraction process Download PDFInfo
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Abstract
The invention particularly relates to a method for extracting hovenia dulcis thunb total flavones by cooperation of a surfactant and a microwave-ultrasonic extraction process. The method comprises the following steps: (1) grinding hovenia dulcis thunb, and performing Soxhlet extraction by petroleum ether to remove fat so as to obtain fully defatted ground hovenia dulcis thunb; (2) uniformly mixing the ground hovenia dulcis thunb, distilled water and the surfactant to obtain a mixed solution; (3) performing microwave-ultrasonic extraction on the mixed solution at the microwave power of 200-600 W and the ultrasonic power of 100-500 W for 5-20 minutes; (4) after the extraction, performing alcohol precipitation on the extracted filtrate to remove alcohol supernatant, and concentrating and drying to obtain a hovenia dulcis thunb total flavones extract. Due to the adoption of the method for extracting hovenia dulcis thunb total flavones, the extraction time is greatly shortened, the extraction efficiency is improved, the cost is reduced, and the energy consumption is low; meanwhile, a distilled water solution in which a small amount of the surfactant is dissolved is taken as an extraction solution, so that the problem of toxic organic solvent residues is solved.
Description
Technical field
The present invention relates to a kind of extracting method of natural active matter, be specifically related to a kind of method of utilizing the collaborative microwave-ultrasonic of surfactant to extract Semen Hoveniae (Fructus Hoveniae) total flavones.
Background technology
Semen Hoveniae (Fructus Hoveniae) be Rhamnaceae plant trifoliate orange chess (
hoveniadulcisThunb) dry seed.Traditional Chinese Medicine thinks, Semen Hoveniae (Fructus Hoveniae) has the relieving restlessness of quenching the thirst, clearing away damp-heat, deinebriating function.For dysphoria with smothery sensation, quench the thirst, difficulty in urination and defecation, the diseases such as alcoholism.Wherein the main active of Semen Hoveniae (Fructus Hoveniae) is flavonoid (comprising kaempferol, apiolin, myricetin, Quercetin, dihydromyricetin) and anthraquinone analog compound emodin etc.The method of extracting at present Semen Hoveniae (Fructus Hoveniae) flavone mainly contains traditional solid-liquid extractions such as merceration, percolation, soxhlet extraction, heat reflow method.But these methods inevitably exist energy consumption high, length consuming time, the shortcoming such as lower and organic solvent residual of productive rate.Modern disease pharmacological research shows, excessive free radical and the oxidation reaction of induction thereof are relevant with a lot of diseases, as atherosclerosis, aging, cancer etc.And there is certain toxicity more in current synthetic antioxidant BHT, BHA, TBHA.Along with the concept of environmental protection is rooted in the hearts of the people gradually, growing to the demand of natural anti-oxidation composition.Flavone in Semen Hoveniae (Fructus Hoveniae) has good antioxidant activity as the Natural antioxidant, in food, cosmetics, medicine, has a wide range of applications potential quality.
Summary of the invention
Goal of the invention of the present invention is to provide the method for the collaborative microwave-ultrasonic extraction of a kind of surfactant Semen Hoveniae (Fructus Hoveniae) total flavones, by the aqueous solution to be dissolved with surfactant, it is extracting solution, in conjunction with microwave extraction method and ultrasonic extraction, extract Semen Hoveniae (Fructus Hoveniae) total flavones, described method can improve extraction efficiency greatly, reduce extraction cost, and do not have the problem of poisonous organic solvent residual.
For achieving the above object, the technical solution adopted in the present invention is:
Surfactant assists microwave-ultrasonic to extract a method for Semen Hoveniae (Fructus Hoveniae) total flavones, and it comprises the steps:
(1) Semen Hoveniae (Fructus Hoveniae) is pulverized to final vacuum and be dried, then take petroleum ether as solvent, adopt soxhlet extraction to remove the fat in Semen Hoveniae (Fructus Hoveniae), obtain the Semen Hoveniae (Fructus Hoveniae) ground product of complete grease removal;
(2) by Semen Hoveniae (Fructus Hoveniae) ground product and distilled water in mass ratio 1:11 ~ 1:33 after fully mixing, obtain feed liquid;
(3) in the feed liquid of step (2), add surfactant, after mixing, obtain mixed solution, the quality of described surfactant is 0.2% ~ 2% of described distilled water quality;
(4) mixed solution of step (3) is carried out to microwave-ultrasonic extraction, microwave power is 200 ~ 600W, and ultrasonic power is 100 ~ 500W, and extraction time is 5 ~ 20min;
(5) microwave-ultrasonic extracts and finishes, and gets its filtrate after filtration;
(6) in filtrate, add ethanol to carry out precipitate with ethanol, discard alcohol supernatant after standing, reconcentration and dry after, obtain Semen Hoveniae (Fructus Hoveniae) total flavones.
In such scheme, described surfactant is polysorbas20, polysorbate40 or polysorbate60; Preferably polysorbas20.In such scheme, described microwave power is 300W, and ultrasonic power is 400W, and extraction time is
10min。
In such scheme, the volumetric concentration of described ethanol is 40% ~ 80%; Preferably 60%.
Principle of the present invention is: surfactant has hydrophilic and oleophilic double properties, can reduce the interfacial tension between Semen Hoveniae (Fructus Hoveniae) cell membrane and aqueous solution, make effective ingredient stripping easily, therefore using be dissolved with suitable dose surfactant water replace organic solvent as extract medium, effective ingredient is had to the effect of " solubilising "; In addition, thereby microwave is to produce heat effect by making polar molecule that resonance friction occur, microwave has again penetrance simultaneously, can make solvent and material inside heat simultaneously, so not only utilize heat effect, because cell interior is in heating, produced pressure simultaneously, cell more easily breaks, and effective ingredient can free stripping; Ultrasound wave is to utilize " cavitation " local high pressure that produces moment, makes cell produce hole and even breaks, and also can make effective ingredient further flow out; So triplicity is acted on to Semen Hoveniae (Fructus Hoveniae) extraction process simultaneously, can improve greatly extraction efficiency, reduce costs.
Beneficial effect of the present invention:
(1) adopt the method for the invention to extract Semen Hoveniae (Fructus Hoveniae) total flavones, extraction time shortens to 5 ~ 20min by traditional 2h ~ 4h, has greatly shortened extraction time, has improved extraction efficiency, and cost is low, power consumption few;
(2) using the distilled water solution that is dissolved with a small amount of surfactant as extracting solution, replaced traditional organic solvent, because surfactant is widely used in food, health product, cosmetics, nontoxic, there is not the problem of poisonous dissolvent residual in the Semen Hoveniae (Fructus Hoveniae) total flavones therefore extracting with the inventive method when being applied to above field.
(3) adopt the inventive method to extract the Semen Hoveniae (Fructus Hoveniae) total flavones obtaining, owing to having avoided long heat effect, reduced that flavone is hydrolyzed, thermal decomposition, oxidized degree, its antioxidation activity in vitro is obviously better than the total flavones that adopts traditional method for extracting to obtain.
(4) the method for the invention is simple to operate, and equipment needed thereby is simple, and solvent is easy to get and easily stores, and has potential application prospect.
The specific embodiment
In order to understand better the present invention, below in conjunction with embodiment, further illustrate content of the present invention, but content of the present invention is not only confined to the following examples.
embodiment 1
The collaborative microwave-ultrasonic of a kind of surfactant extracts the method for Semen Hoveniae (Fructus Hoveniae) total flavones, comprise the steps: that (1) accurately takes 5g Semen Hoveniae (Fructus Hoveniae) ground product, after vacuum drying, carry out petroleum ether Soxhlet and be extracted into complete grease removal, obtain the Semen Hoveniae (Fructus Hoveniae) ground product 4.59g of complete grease removal; (2) will after the Semen Hoveniae (Fructus Hoveniae) ground product 4.59g of complete grease removal, 50g distilled water and 0.4g surfactant polysorbas20 mix homogeneously, obtain mixed solution; (3) described mixed solution is carried out to microwave-ultrasonic extraction, microwave power is 300W, and ultrasonic power is 400W, and extraction time is 10min; (4) extract after to mixed solution filter after get filtrate; (5) in filtrate, add 60vt%(volumetric concentration) ethanol carries out precipitate with ethanol, abandons alcohol supernatant after standing, reconcentration and dry after, obtain Semen Hoveniae (Fructus Hoveniae) total flavones.
Adopt NaNO
2-Al (NO
3)
3the content of the Semen Hoveniae (Fructus Hoveniae) total flavones that-NaOH method mensuration said extracted obtains, result shows: general flavone content is 2.21wt%.
The Semen Hoveniae (Fructus Hoveniae) total flavones that adopts o-phenanthroline, pyrogallol Autoxidation Method, DPPH method to obtain said extracted carries out the test of antioxidation in vitro performance, and result shows: when total flavones concentration is 0.4mgml
-1time, its clearance rate OH is 79.1%, O
2 -be that 83.2%, DPPH is 96.7%; Known with comparative example contrast, method is extracted the total flavones obtaining described in the present embodiment, and its in vitro anti-oxidation is obviously better than adopting traditional heat reflow method to extract the flavone obtaining.
embodiment 2
The collaborative microwave-ultrasonic of a kind of surfactant extracts the method for Semen Hoveniae (Fructus Hoveniae) total flavones, comprise the steps: that (1) accurately takes 5g Semen Hoveniae (Fructus Hoveniae) ground product, after vacuum drying, carry out petroleum ether Soxhlet and be extracted into complete grease removal, obtain the Semen Hoveniae (Fructus Hoveniae) ground product 4.59g of complete grease removal; (2) will after the Semen Hoveniae (Fructus Hoveniae) ground product 4.59g of complete grease removal, 100g distilled water and 0.2g surfactant polysorbate40 mix homogeneously, obtain mixed solution; (3) described mixed solution is carried out to microwave-ultrasonic extraction, microwave power is 200W, and ultrasonic power is 100W, and extraction time is 5min; (4) extract after to mixed solution filter after get filtrate; (5) in filtrate, add 80vt% ethanol to carry out precipitate with ethanol, abandon alcohol supernatant after standing, reconcentration and dry after, obtain Semen Hoveniae (Fructus Hoveniae) total flavones.
Adopt NaNO
2-Al (NO
3)
3the content of the Semen Hoveniae (Fructus Hoveniae) total flavones that-NaOH method mensuration said extracted obtains, result shows: general flavone content is 1.31wt%.
The Semen Hoveniae (Fructus Hoveniae) total flavones that adopts o-phenanthroline, pyrogallol Autoxidation Method, DPPH method to obtain said extracted carries out the test of antioxidation in vitro performance, and result shows: when total flavones concentration is 0.4mgml
-1time, its clearance rate OH is 73.3%, O
2 -be that 79.9%, DPPH is 92.1%.Known with comparative example contrast, method is extracted the total flavones obtaining described in the present embodiment, and its in vitro anti-oxidation is obviously better than adopting traditional heat reflow method to extract the flavone obtaining.
embodiment 3
The collaborative microwave-ultrasonic of surfactant extracts a method for Semen Hoveniae (Fructus Hoveniae) total flavones, comprises the steps:
(1) accurately take 5g Semen Hoveniae (Fructus Hoveniae) ground product, after vacuum drying, carry out petroleum ether Soxhlet and be extracted into complete grease removal, obtain the Semen Hoveniae (Fructus Hoveniae) ground product 4.59g of complete grease removal; (2) will after the Semen Hoveniae (Fructus Hoveniae) ground product 4.59g of complete grease removal, 150g distilled water and 3g surfactant polysorbate60 mix homogeneously, obtain mixed solution; (3) described mixed solution is carried out to microwave-ultrasonic extraction, microwave power is 600W, and ultrasonic power is 500W, and extraction time is 20min; (4) extract after to mixed solution filter after get filtrate; (5) in filtrate, add 40vt% ethanol to carry out precipitate with ethanol, abandon alcohol supernatant after standing, reconcentration and dry after, obtain Semen Hoveniae (Fructus Hoveniae) total flavones.
Adopt NaNO
2-Al (NO
3)
3the content of the Semen Hoveniae (Fructus Hoveniae) total flavones that-NaOH method mensuration said extracted obtains, result shows: general flavone content is 1.98wt%.
The Semen Hoveniae (Fructus Hoveniae) total flavones that adopts o-phenanthroline, pyrogallol Autoxidation Method, DPPH method to obtain said extracted carries out the test of antioxidation in vitro performance, and result shows: when concentration is 0.4mgml
-1time, its clearance rate OH is 76.3.1%, O
2 -be that 80.0%, DPPH is 95.2%.Known with comparative example contrast, the present embodiment method is extracted the total flavones obtaining, and its in vitro anti-oxidation is obviously better than adopting traditional heat reflow method to extract the flavone obtaining.
comparative example
Adopt traditional heat reflow method to extract the method for Semen Hoveniae (Fructus Hoveniae) total flavones, comprise the steps:
(1) accurately take 5g Semen Hoveniae (Fructus Hoveniae) ground product, after vacuum drying, carry out petroleum ether Soxhlet and be extracted into complete grease removal, obtain the Semen Hoveniae (Fructus Hoveniae) ground product 4.59g of complete grease removal; (2) will after the Semen Hoveniae (Fructus Hoveniae) ground product 4.59g of complete grease removal, 50mL70vt% alcoholic solution mix homogeneously, obtain mixed solution; (3) described mixed solution is heated to micro-boiling, connects condensing unit and keep ethanol to continue to reflux on heating container, extraction time is 120min; (4) extract after to mixed solution filter after get filtrate; (5) in filtrate, add 60vt% ethanol to carry out precipitate with ethanol, abandon alcohol supernatant after standing, reconcentration and dry after, obtain Semen Hoveniae (Fructus Hoveniae) total flavones.
The total flavones that said extracted is obtained adopts o-phenanthroline, pyrogallol Autoxidation Method, DPPH method to carry out the test of antioxidation in vitro performance, and result is: when total flavones concentration is 0.4mgml
-1time, its clearance rate OH is 60.7%, O
2 -be that 70.2%, DPPH is 73.9%.Contrast knownly, utilize the method for the invention to extract the total flavones obtaining, its in vitro anti-oxidation is obviously better than adopting traditional heat reflow method to extract the total flavones obtaining.
Obviously, above-described embodiment is to be only the example that clearly explanation is done, and the not restriction to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here without also giving exhaustive to all embodiments.And the apparent variation therefore amplified or variation are still within the protection domain in the invention.
Claims (6)
1. a method for surfactant assisted microwave synthesis-ultrasonic extraction Semen Hoveniae (Fructus Hoveniae) total flavones, is characterized in that: it comprises the steps:
(1) Semen Hoveniae (Fructus Hoveniae) is pulverized to final vacuum and be dried, then take petroleum ether as solvent, adopt soxhlet extraction to remove the fat in Semen Hoveniae (Fructus Hoveniae), obtain the Semen Hoveniae (Fructus Hoveniae) ground product of complete grease removal;
(2) by Semen Hoveniae (Fructus Hoveniae) ground product and distilled water in mass ratio 1:11 ~ 1:33 after fully mixing, obtain feed liquid;
(3) in the feed liquid of step (2), add surfactant, after mixing, obtain mixed solution, the quality of described surfactant is 0.2% ~ 2% of described distilled water quality;
(4) mixed solution of step (3) is carried out to microwave-ultrasonic extraction, microwave power is 200 ~ 600W, and ultrasonic power is 100 ~ 500W, and extraction time is 5 ~ 20min;
(5) microwave-ultrasonic extracts and finishes, and gets its filtrate after filtration;
(6) in filtrate, add ethanol to carry out precipitate with ethanol, discard alcohol supernatant after standing, reconcentration and dry after, obtain Semen Hoveniae (Fructus Hoveniae) total flavones.
2. method according to claim 1, is characterized in that, described surfactant is polysorbas20, polysorbate40 or polysorbate60.
3. method according to claim 2, is characterized in that, described surfactant is polysorbas20.
4. method according to claim 1, is characterized in that, described microwave power is 300W, and ultrasonic power is 400W, and extraction time is 10min.
5. method according to claim 1, is characterized in that, the volumetric concentration of described ethanol is 40% ~ 80%.
6. method according to claim 5, is characterized in that, the volumetric concentration of described ethanol is 60%.
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| CN106975240A (en) * | 2017-05-09 | 2017-07-25 | 福建农林大学 | A kind of integrated approach that flavones is extracted from purple perilla |
| CN107115382A (en) * | 2017-06-14 | 2017-09-01 | 广东番石榴健康产业有限公司 | A kind of method that general flavone is extracted from Guava Leaf |
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| CN116440049A (en) * | 2023-05-31 | 2023-07-18 | 诺德溯源(广州)生物科技有限公司 | Whitening composition suitable for sensitive muscles and having skin barrier repairing effect and application thereof |
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| CN105231249A (en) * | 2015-09-17 | 2016-01-13 | 暨南大学 | Bamboo leaf flavone extracting method by synergy of ultrasonic and surface-active agent |
| CN106975240A (en) * | 2017-05-09 | 2017-07-25 | 福建农林大学 | A kind of integrated approach that flavones is extracted from purple perilla |
| CN107115382A (en) * | 2017-06-14 | 2017-09-01 | 广东番石榴健康产业有限公司 | A kind of method that general flavone is extracted from Guava Leaf |
| CN107213203A (en) * | 2017-06-14 | 2017-09-29 | 广东番石榴健康产业有限公司 | A kind of method that total polyphenols are extracted from Guava Leaf |
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| CN110467734A (en) * | 2019-08-29 | 2019-11-19 | 贵州大学 | A kind of method of the thick glue solution purifying preparation eucommia ulmoides refined glue of Cortex Eucommiae seed peel |
| CN110467734B (en) * | 2019-08-29 | 2022-07-29 | 贵州大学 | Method for preparing eucommia ulmoides refined gum by purifying eucommia ulmoides seed skin crude gum aqueous solution |
| CN116440049A (en) * | 2023-05-31 | 2023-07-18 | 诺德溯源(广州)生物科技有限公司 | Whitening composition suitable for sensitive muscles and having skin barrier repairing effect and application thereof |
| CN116440049B (en) * | 2023-05-31 | 2023-12-22 | 诺德溯源(广州)生物科技有限公司 | Whitening composition suitable for sensitive muscles and having skin barrier repairing effect and application thereof |
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