CN103239546A - Method for extracting general flavone from litchi shells - Google Patents
Method for extracting general flavone from litchi shells Download PDFInfo
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- CN103239546A CN103239546A CN2013101558627A CN201310155862A CN103239546A CN 103239546 A CN103239546 A CN 103239546A CN 2013101558627 A CN2013101558627 A CN 2013101558627A CN 201310155862 A CN201310155862 A CN 201310155862A CN 103239546 A CN103239546 A CN 103239546A
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- exocarpium litchi
- total flavones
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- litchi
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Abstract
The invention discloses a method for extracting general flavone from litchi shells. The extraction method comprises the following steps of: drying and crushing the waste litchi shells; performing ultrasonic extraction; filtering and concentrating; adsorbing by a resin column; eluting by elution solution; collecting the eluted solution; and drying to obtain the natural general flavone. With the adoption of the extraction process, the content of the general flavone is tested to be not less than 80%. The extraction method disclosed by the invention has the advantages of being simple in operation process, high in safety, extraction rate and extraction purity, and easy for industrialized production. With the adoption of the extraction method disclosed by the invention, recycling for the waste litchi shells is realized, and economic income is increased, so that the extraction method has a wide market prospect.
Description
Technical field
The present invention relates to material extractive technique field, be specifically related to a kind of method of from Exocarpium Litchi, extracting total flavones.
Background technology
Fructus Litchi is sapindaceous plant, is the torrid zone and semi-tropical famous-brand and high-quality fruit, and all there are a large amount of plantations in provinces such as the Guangdong of China, Guangxi, Fujian, Taiwan, Hainan, and output is very high.Fructus Litchi often is processed into products such as canned litchi, litchi spirit or litchi drink except directly eating, the Exocarpium Litchi of peelling off in the course of processing is fallen as garbage disposal usually, has caused very big waste.In fact, Exocarpium Litchi contains the various active composition, as flavonoid, phenols and polysaccharose substance, has very high medical value.Wherein, total flavones has bio-pharmacology activity such as antioxidation, antiinflammatory, antimutagenic, antitumor; Particularly the flavone of natural origin can be absorbed rapidly by human body because molecular weight is little, has allaying tiredness, protection blood vessel, functions such as preventing arteriosclerosis.Because hypotoxicity and the high efficiency of Flavonoid substances, the research at aspects such as cardiovascular and cerebrovascular disease and oncotherapys has received concern more and more widely about total flavones in recent years, becomes the focus of natural drug research and development.Development and use to Flavonoid substances in the Exocarpium Litchi not only make discarded Exocarpium Litchi be recycled, and can also increase orchard worker's income.
At present, the purification process of traditional flavones ingredient has extraction and polyamide column chromatography method etc., exist troublesome poeration, extraction time long, and solvent has shortcoming such as toxicity in various degree.Therefore improve extraction ratio, the dna purity that extracts Flavonoid substances in the Exocarpium Litchi, make extracting method safety again simple to operate, be easy to suitability for industrialized production and seem particularly important.
Summary of the invention
At above-mentioned deficiency, technical problem to be solved by this invention provides a kind of method of extracting total flavones from Exocarpium Litchi, and this method operating procedure is simple, safe, has extraction ratio height, advantage that dna purity is high.
For addressing the above problem, the present invention is achieved through the following technical solutions:
From Exocarpium Litchi, extract the method for total flavones, may further comprise the steps:
1) the fresh lichee shell is put into 35～50 ℃ baking oven, behind air cooking 10h, pulverized 60 mesh sieves, get the Exocarpium Litchi powder, put room temperature and preserve standby;
2) the Exocarpium Litchi powder adding concentration that makes to step 1) is 50～70% alcoholic solution, carries out supersound extraction 30～50min then, extracting solution is filtered and concentration again, obtains the Exocarpium Litchi concentrated solution;
3) described Exocarpium Litchi concentrated solution is carried out purification by pretreated macroporous adsorptive resins;
4) wash described macroporous adsorptive resins, use the eluent eluting then, collect the part elute soln, be concentrated into driedly, obtain described total flavones.Wherein, washing is to remove residual solution and other materials in the resin.
In the such scheme, preferably, step 2) addition of alcoholic solution can be 40～65 times of Exocarpium Litchi powder weight in.
Preferably, in step 2) in, when carrying out supersound extraction, ultrasonic power is preferably controlled at 95～120W.
Preferably, in step 2) in, the number of times of described supersound extraction is 2 times.Certainly the number of times that extracts is not limited to 2 times, it can be 3 times, 4 times or 5 times, generally speaking, number of times is more many, the total flavones that can extract is more many, but the total flavones that extracts of single can be fewer and feweri several times in the back, and it is bigger repeatedly to extract used energy consumption, cause the increase of cost, therefore preferred 2 times.
Preferably, in step 4), described eluent can be that concentration is 60～90% alcoholic solution.
Preferably, in step 4), the flow velocity of described washing is 2.5～6BV/h, and the flow velocity of described eluent is 2～5.5 BV/h.
Preferably, in step 4), solution is solution behind the eluting between 0.5～3BV/h BV/h behind the described part eluting.
Preferably, in step 4), described macroporous adsorptive resins is AB-8 macroporous resin or D101 macroporous resin.
Beneficial effect of the present invention is:
1, after the present invention carries out drying, pulverizing with discarded Exocarpium Litchi, carries out supersound extraction again, after the filtering and concentrating, resin column absorption, reuse eluent eluting, solution behind the collection eluting, drying obtains natural total flavones, under these process conditions, content of total flavone is not less than 80%, and it is simple to have an operating procedure, safe, the extraction ratio height, the advantage that dna purity is high, and be easy to suitability for industrialized production.
2, of the present invention realization increased income to the recycling of discarded Exocarpium Litchi, has vast market prospect.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that following examples only to be used for explanation the present invention and be not used in and limit the scope of the invention.
Embodiment 1:
From Exocarpium Litchi, extract the method for total flavones, get 1kg fresh lichee shell and put into 45 ℃ baking oven, behind air cooking 10h, pulverized 60 mesh sieves, get the Exocarpium Litchi powder, adding concentration is 60% alcoholic solution, and its addition is 50 times of Exocarpium Litchi powder weight, is under the condition of 100W at power then, supersound extraction 2 times, each 40min.Merge extracted twice liquid, carry out concentration after leaving standstill filtration, obtain 2100ml Exocarpium Litchi concentrated solution.
Get the good AB-8 macroporous resin of a certain amount of pretreatment, the internal diameter of packing into is in the glass column of 2.5cm, making its bed volume is 180ml, flow velocity with 2.5BV/h makes 2100ml Exocarpium Litchi concentrated solution slowly pass through resin bed, remove solution residual in the post with the washing of 4500ml then, the alcoholic solution of reuse 80% flows through resin column with the flow velocity of 4.5BV/h, solution behind the eluting between collection 0.5～3BV/h, be evaporated to driedly, namely obtain total flavones.After testing, content of total flavone is 79.5% in the 1kg Exocarpium Litchi.
Embodiment 2:
From Exocarpium Litchi, extract the method for total flavones, get 1kg fresh lichee shell and put into 45 ℃ baking oven, behind air cooking 10h, pulverized 60 mesh sieves, get the Exocarpium Litchi powder, adding concentration is 60% alcoholic solution, and its addition is 50 times of Exocarpium Litchi powder weight, is under the condition of 100W at power then, supersound extraction 2 times, each 40min.Merge extracted twice liquid, carry out concentration after leaving standstill filtration, obtain 2100ml Exocarpium Litchi concentrated solution.
Get the good D101 macroporous resin of a certain amount of pretreatment, the internal diameter of packing into is in the glass column of 2.5cm, making its bed volume is 180ml, flow velocity with 2.5BV/h makes 2100ml Exocarpium Litchi concentrated solution slowly pass through resin bed, remove solution residual in the post with the washing of 4500ml then, the alcoholic solution of reuse 80% flows through resin column with the flow velocity of 4.5BV/h, solution behind the eluting between collection 0.5～3BV/h, be evaporated to driedly, namely obtain total flavones.After testing, content of total flavone is 80.5% in the 1kg Exocarpium Litchi.
Embodiment 3:
From Exocarpium Litchi, extract the method for total flavones, get 3kg fresh lichee shell and put into 45 ℃ baking oven, behind air cooking 10h, pulverized 60 mesh sieves, get the Exocarpium Litchi powder, adding concentration is 70% alcoholic solution, and its addition is 55 times of Exocarpium Litchi powder weight, is under the condition of 110W at power then, supersound extraction 2 times, each 40min.Merge extracted twice liquid, carry out concentration after leaving standstill filtration, obtain 6300ml Exocarpium Litchi concentrated solution.
Get the good AB-8 macroporous resin of a certain amount of pretreatment, the internal diameter of packing into is in the glass column of 4.2cm, making its bed volume is 420ml, flow velocity with 2.5BV/h makes 6300ml Exocarpium Litchi concentrated solution slowly pass through resin bed, remove solution residual in the post with the washing of 13200ml then, the alcoholic solution of reuse 80% flows through resin column with the flow velocity of 4BV/h, solution behind the eluting between collection 0.5～3BV/h, be evaporated to driedly, namely obtain total flavones.After testing, content of total flavone is 81.5% in the 3kg Exocarpium Litchi.
Embodiment 4:
From Exocarpium Litchi, extract the method for total flavones, get 3kg fresh lichee shell and put into 45 ℃ baking oven, behind air cooking 10h, pulverized 60 mesh sieves, get the Exocarpium Litchi powder, adding concentration is 70% alcoholic solution, and its addition is 55 times of Exocarpium Litchi powder weight, is under the condition of 110W at power then, supersound extraction 2 times, each 40min.Merge extracted twice liquid, carry out concentration after leaving standstill filtration, obtain 6300ml Exocarpium Litchi concentrated solution.
Get the good D101 macroporous resin of a certain amount of pretreatment, the internal diameter of packing into is in the glass column of 4.2cm, making its bed volume is 420ml, flow velocity with 2.5BV/h makes 6300ml Exocarpium Litchi concentrated solution slowly pass through resin bed, remove solution residual in the post with the washing of 13200ml then, the alcoholic solution of reuse 80% flows through resin column with the flow velocity of 4BV/h, solution behind the eluting between collection 0.5～3BV/h, be evaporated to driedly, namely obtain total flavones.After testing, content of total flavone is 82.5% in the 3kg Exocarpium Litchi.
Claims (8)
1. from Exocarpium Litchi, extract the method for total flavones, it is characterized in that may further comprise the steps:
1) the fresh lichee shell is put into 35～50 ℃ baking oven, behind air cooking 10h, pulverized 60 mesh sieves, get the Exocarpium Litchi powder, put room temperature and preserve standby;
2) the Exocarpium Litchi powder adding concentration that makes to step 1) is 50～70% alcoholic solution, carries out supersound extraction 30～50min then, extracting solution is filtered and concentration again, obtains the Exocarpium Litchi concentrated solution;
3) described Exocarpium Litchi concentrated solution is carried out purification by pretreated macroporous adsorptive resins;
4) wash described macroporous adsorptive resins, use the eluent eluting then, collect the part elute soln, be concentrated into driedly, obtain described total flavones.
2. the method for extracting total flavones from Exocarpium Litchi according to claim 1 is characterized in that: step 2) in the addition of alcoholic solution be 40～65 times of Exocarpium Litchi powder weight.
3. the method for extracting total flavones from Exocarpium Litchi according to claim 1 is characterized in that: in step 2) in, when carrying out supersound extraction, ultrasonic power is controlled at 95～120W.
4. the method for extracting total flavones from Exocarpium Litchi according to claim 1 is characterized in that: in step 2) in, the number of times of described supersound extraction is 2 times.
5. the method for extracting total flavones from Exocarpium Litchi according to claim 1, it is characterized in that: in step 4), described eluent is that concentration is 60～90% alcoholic solution.
6. the method for extracting total flavones from Exocarpium Litchi according to claim 1, it is characterized in that: in step 4), the flow velocity of described washing is 2.5～6BV/h, and the flow velocity of described eluent is 2～5.5BV/h.
7. the method for extracting total flavones from Exocarpium Litchi according to claim 1 is characterized in that: in step 4), solution is solution behind the eluting between 0.5～6BV/h behind the described part eluting.
8. the method for extracting total flavones from Exocarpium Litchi according to claim 1, it is characterized in that: in step 4), described macroporous adsorptive resins is AB-8 macroporous resin or D101 macroporous resin.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015078396A1 (en) * | 2013-11-28 | 2015-06-04 | 上海家化联合股份有限公司 | 5α-reductase inhibitor and use thereof |
| CN105232731A (en) * | 2015-11-13 | 2016-01-13 | 谢镜国 | Method for extracting total flavonoids from litchi shells |
| CN105663197A (en) * | 2016-03-09 | 2016-06-15 | 贵州师范大学 | Method for extracting total flavonoids of gnaphalium japonicum |
| CN106214774A (en) * | 2016-08-30 | 2016-12-14 | 新疆医科大学 | A kind of extraction method of cassie card Pu's Fructus Jujubae total flavones |
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| JP2012036128A (en) * | 2010-08-06 | 2012-02-23 | Oriza Yuka Kk | Collagen production promoter and skin-beautifying composition comprising the same |
| TW201244729A (en) * | 2011-05-06 | 2012-11-16 | Univ Yuanpei | Production method and application of litchi polyphenol |
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2013
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015078396A1 (en) * | 2013-11-28 | 2015-06-04 | 上海家化联合股份有限公司 | 5α-reductase inhibitor and use thereof |
| CN105232731A (en) * | 2015-11-13 | 2016-01-13 | 谢镜国 | Method for extracting total flavonoids from litchi shells |
| CN105663197A (en) * | 2016-03-09 | 2016-06-15 | 贵州师范大学 | Method for extracting total flavonoids of gnaphalium japonicum |
| CN106214774A (en) * | 2016-08-30 | 2016-12-14 | 新疆医科大学 | A kind of extraction method of cassie card Pu's Fructus Jujubae total flavones |
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Application publication date: 20130814 |