CN103211926A - Method for extracting total flavonoids in grape seeds in double-aqueous phase system - Google Patents
Method for extracting total flavonoids in grape seeds in double-aqueous phase system Download PDFInfo
- Publication number
- CN103211926A CN103211926A CN2013101579021A CN201310157902A CN103211926A CN 103211926 A CN103211926 A CN 103211926A CN 2013101579021 A CN2013101579021 A CN 2013101579021A CN 201310157902 A CN201310157902 A CN 201310157902A CN 103211926 A CN103211926 A CN 103211926A
- Authority
- CN
- China
- Prior art keywords
- vitis viniferae
- semen vitis
- double
- aqueous phase
- phase system
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Abstract
The invention discloses a method for extracting total flavonoids in grape seeds in a double-aqueous phase system, belonging to the field of separation and extraction methods of natural product active ingredients. The method comprises the following steps of: firstly preparing grape seed rough extract from grape seeds with ethanol; then adding absolute ethyl alcohol, ammonia sulfate, inorganic salt and water in the grape seed rough extract to form the double-aqueous phase system, mixing uniformly, standing for 5-30 minutes at room temperature for delamination to obtain an upper phase and a lower phase, concentrating the upper phase through pressure reduction and drying so as to obtain total flavonoids of grape seed. In the double-aqueous phase system, the mass percents of grape seed rough extract, absolute ethyl alcohol, ammonia sulfate and inorganic salt are respectively 5% to 30%, 10% to 30%, 16% to 30%, and 0 to 5%, the balance is supplemented to be 100% with water, and the pH of the double-aqueous phase system is 3.0 to 11.0. Flavonoids are extracted by utilizing double aqueous phases in the method; the method is simple, the operation is convenient, the production cost is low and the treating capacity is large, small test data can be directly amplified, and the yield of flavonoids in the grape seeds reaches up to 98.2%; and the method can be operated continuously, and is suitable for industrialized production of flavonoids in the grape seeds.
Description
Technical field
The invention belongs to a kind of separating and extracting process field of active ingredient of natural product, the method for total flavones in particularly a kind of double-aqueous phase system extraction Semen Vitis viniferae.
Technical background
The Hexi Corridor is located in north latitude 36 to be spent between 40 degree, has the resources such as optimal light, heat, water, soil of production high-quality vinifera, is one of best place of production of China and even whole world organic wine.In the wine course of processing, the annual a large amount of skin slag garbages that account for Fructus Vitis viniferae processing capacity 20-30% that produce wherein mainly are Pericarpium Vitis viniferae, Semen Vitis viniferae and carpopodium etc.Semen Vitis viniferae contains plurality of active ingredients, mainly contains flavone, protein, polysaccharide, procyanidin.Flavones ingredient in the Semen Vitis viniferae has blood vessel dilating, increase peripheral blood circulation and blood flow rate, the cholesterol level in the reduction blood, improve effects such as cholesterol and phospholipid ratio; The formation of thrombosis can be effectively suppressed,, and symptom can be greatly improved coronary heart disease, hypertension and cardiovascular and cerebrovascular disease; Can promote big cerebral circulation metabolism, improve memory function, the recovery and the alzheimer disease of brain injury all had positive therapeutic and health-care effect; Have anti-inflammation, suppress the effect that cancer starts the factor, can improve immune function of human body and anti-senescence function; Have strong anti-oxidation, antitumaous effect.The bioflavonoids that extracts from Semen Vitis viniferae is compared with most of flavone, and structure is special, good water solubility, and the effectiveness height, bioavailability very easily is absorbed by the body more than 90%.Therefore the extraction separation research to flavones ingredient in the Semen Vitis viniferae is a heat subject of the world of medicine.
In the existing report,, mainly contain solvent extraction method, resin adsorption method, ultrafiltration and aqueous two-phase extraction method are also arranged the extraction separation method of flavone compound in the plant.Double-aqueous phase system (ATPE) is during with the aqueous solution of two kinds of different water-soluble polymers, polymer concentration reaches certain value, system is divided into mutual exclusive biphase naturally, mainly comprises high polymer/high polymer double-aqueous phase system and high polymer/inorganic salt double-aqueous phase system.
Known in the artly be, double-aqueous phase system is not to be fit to all to contain the extraction of total flavonoid plant, even be fit to the extraction of total flavones in the certain plants, the variation of conditions such as the concrete consumption of the reagent in the described double-aqueous phase system, concentration, pH all has considerable influence to the yield of total flavones, time etc.Therefore a spot of report that the Flavonoid substances in the Folium toonae sinensis is carried out separation and Extraction as Chinese invention patent CN101396432A employing ethanol-ammonium sulfate double-aqueous phase system is only arranged.In addition, the extraction to total flavones in the Semen Vitis viniferae in the prior art generally all is to use solvent extraction method, and the someone does not adopt double-aqueous phase system that total flavones in the Semen Vitis viniferae is extracted.Although Chinese invention patent CN101125841A discloses a kind of extracting method of seed of Fructus Vitis viniferae flavone, adopt solvent extraction method to carry out multiple extraction to it, can finish in 3-5 days once and extract, yield is 64%, but extract total flavones in the Semen Vitis viniferae with solvent extraction method, process cycle is long, and extraction ratio is undesirable, is unfavorable for suitability for industrialized production.
Summary of the invention
The purpose of this invention is to provide the method that a kind of cost is low, mass transfer rate fast, the lab scale data can directly be amplified, treating capacity is big, but the high double-aqueous phase system that reaches continued operation of yield extracts total flavones in the Semen Vitis viniferae.
The method of total flavones comprises the steps: earlier Semen Vitis viniferae to be prepared the Semen Vitis viniferae crude extract with ethanol extraction in the double-aqueous phase system extraction Semen Vitis viniferae of the present invention; Again dehydrated alcohol, ammonium sulfate, inorganic salt, water are joined in the described Semen Vitis viniferae crude extract and form double-aqueous phase system, mixing, room temperature leave standstill the 5-30min layering, obtain phase (being the ethanol phase) and descend mutually, get through concentrating under reduced pressure and dry, obtain total flavone from grap seeds; In double-aqueous phase system, Semen Vitis viniferae crude extract shared mass ratio in system is 5%-30%, described dehydrated alcohol shared mass ratio in system is 10%-30%, described ammonium sulfate shared mass ratio in system is 16%-30%, described inorganic salt shared mass ratio in system is 0-5%, the surplus water complements to 100%, and the pH of described double-aqueous phase system is 3.0-11.0.
" mass ratio " of the present invention is meant the ratio of the quality and the whole constituent mass sum of each component.
" mass transfer rate " of the present invention is meant the amount kmol/s of unit interval transmitter substance.
Semen Vitis viniferae crude extract of the present invention is preferably to make as follows; but should not be construed as restriction to Semen Vitis viniferae crude extract of the present invention; select other extracting method similar or well known in the art for use, the Semen Vitis viniferae crude extract that makes is all within protection scope of the present invention:
With the Semen Vitis viniferae powder of described Semen Vitis viniferae through obtaining after roguing, washing, oven dry, the pulverizing, add then and be equivalent to the alcoholic solution that Semen Vitis viniferae powder volume 6-10 doubly measures, the volume fraction of described alcoholic solution is 30-70%, supersound process 5-15min, ultrasonic power is 200-400W, with the mixed liquor filtering and impurity removing after the supersound process.
" volume fraction " of the present invention is meant the ethanol volume in the alcoholic solution and the ratio of whole liquor capacity.
The method for making of preferred Semen Vitis viniferae crude extract is, is to add the alcoholic solution that is equivalent to 8 times of amounts of Semen Vitis viniferae powder volume, and the volume fraction of described alcoholic solution is 50%.
The method for making of further preferred Semen Vitis viniferae crude extract is that in supersound process, used ultrasonic power is that 325W, processing time are 10min.
Double-aqueous phase system of the present invention, when dehydrated alcohol shared mass ratio in system is that 19%-23%, ammonium sulfate shared mass ratio in system is that 17%-24%, inorganic salt shared mass ratio in system is 0-2.5%, when the surplus water complements to 100%, can obtains effect more.
In the double-aqueous phase system of the present invention, pH value has important function for the yield of final total flavones, the time of extraction, and as previously mentioned, the present invention finds that unexpectedly the pH value scope of double-aqueous phase system of the present invention is 3.0-11.0.When pH is 5.0-9.0, can obtain effect more, about 10 minutes of mass transfer rate.
The method of total flavones in the double-aqueous phase system extraction Semen Vitis viniferae of the present invention, described inorganic salt includes but not limited to sodium chloride, potassium chloride etc., particularly preferably is sodium chloride.
The method of total flavones in the double-aqueous phase system of the present invention extraction Semen Vitis viniferae, the described standing demix time is 10-20min, promptly total flavone from grap seeds can be realized quick transmission at two in mutually, and has higher mass transfer rate.
Described concentrating under reduced pressure is also dry, is that described going up 60-80 ℃ of distilling under reduced pressure concentrated and vacuum drying.Wherein the temperature of distilling under reduced pressure preferably is 75-79 ℃.
Specifically, the method for total flavones in a kind of double-aqueous phase system extraction Semen Vitis viniferae of the present invention, described method comprises the steps:
A. with the Semen Vitis viniferae powder of described Semen Vitis viniferae through obtaining after roguing, washing, oven dry, the pulverizing, be to add that to be equivalent to Semen Vitis viniferae powder volume 8 times of amounts, volume fractions be 50% alcoholic solution, at used ultrasonic power supersound process 10min under the situation of 325W, with the mixed liquor filtering and impurity removing after the supersound process, get the Semen Vitis viniferae crude extract;
B. again dehydrated alcohol, ammonium sulfate, inorganic salt, water are joined in the described Semen Vitis viniferae crude extract and form double-aqueous phase system, mixing, room temperature leave standstill the 10-20min layering, obtain upper and lower phase, get, vacuum drying concentrated, obtain total flavone from grap seeds in 75 ℃ of distilling under reduced pressure;
In described double-aqueous phase system, described Semen Vitis viniferae crude extract shared mass ratio in system is 17.5%, described dehydrated alcohol shared mass ratio in system is 23%, described ammonium sulfate shared mass ratio in system is 17%, described sodium chloride shared mass ratio in system is 2.5%, the surplus water complements to 100%, and the pH of described double-aqueous phase system is 7.0.
Beneficial effect of the present invention is that ⑴ is a raw material with Hexi Corridor aboundresources Semen Vitis viniferae, turns waste into wealth, and has improved its added value, and product cost is low; ⑵ extract in the system near physiological environment, aqueous two-phase water content height, and the steric configuration of the composition of remaining valid can not cause bioactive substance inactivation or degeneration; ⑶ the phase-splitting time is short, and mass transfer rate is fast, but just phase-splitting in the fastest 5 minutes, and response rate height, average out to is more than 98.2%; ⑷ adopted nontoxic dehydrated alcohol, with low cost, and do not have the organic solvent residual problem; ⑸ a large amount of impurity can together be removed with solid matter; ⑹ partition coefficient repeatability is good, and the lab scale data can directly be amplified, and can directly be connected with follow-up purifying technique, need not to carry out special handling; ⑺ operating condition gentleness, the whole operation process is carried out at normal temperatures and pressures; ⑻ can improve the selectivity of partition coefficient and extraction.
The invention will be further described below in conjunction with embodiment, and according to mensuration and the calculated yield of UV-VIS spectrophotometry to total flavone from grap seeds:
The specific embodiment
Algoscopy 1
Flavone in the Semen Vitis viniferae:
Use NaNO
2-Al (NO
3)
3-NaOH system complexation chemistry light absorption method is got control substance of Rutin and is made into standard solution, adds NaNO
2-Al (NO
3)
3-NaOH measures light absorption value with spectrophotometer at 510nm after developing the color, and gets the standard curve equation to be: y=1.245x-0.0024, and wherein y is a light absorption value, and x is flavones content (mg), and correlation coefficient is R==0.9992; Through the sample liquid of double-aqueous phase system extraction, get it up and down through NaNO
2-Al (NO
3)
3After-NaOH the colour developing, measure light absorption value y' with spectrophotometer at 510nm, substitution standard curve equation gets flavones content x'.
The yield of flavone in the Semen Vitis viniferae:
System compares R=V
On/ V
DownV wherein
On, V
DownIt is respectively the volume (mL) of upper and lower phase;
The aqueous two-phase partition coefficient K=C of target substance
On/ C
DownWherein, C
On, C
DownIt is respectively the mass concentration (mg/mL) of upper and lower target substance;
Yield is calculated as follows:
Embodiment 1 lab scale
Supersound extraction: precision weighing Semen Vitis viniferae, through roguing, washing, it is in 50% the alcoholic solution that the 10g Semen Vitis viniferae powder that obtains after pulverizing adds the 80ml volume fraction, at power supersound process 10min under the condition of 325W, mixed liquor filtering and impurity removing with after the supersound process obtains the Semen Vitis viniferae crude extract;
Aqueous two-phase extraction: will form double-aqueous phase system in 2.3g dehydrated alcohol, 1.7g ammonium sulfate, 0.25g sodium chloride, the 4.0g water adding 1.75g Semen Vitis viniferae crude extract, with each material mixing in the system, regulating pH is 7.0, leaves standstill 5min under room temperature, layering obtains upper and lower phase, on be the ethanol phase mutually;
Concentrating under reduced pressure: get above-mentioned ethanol phase, 75 ℃ of concentrated, vacuum dryings of distilling under reduced pressure obtain total flavone from grap seeds.
Experimental result: get 0.2mL and add NaNO
2-Al (NO
3)
3After-NaOH the colour developing, total flavone from grap seeds is 0.276 at last phase light absorption value, gets 1mL and adds NaNO
2-Al (NO
3)
3After-NaOH the colour developing, following phase light absorption value is 0.03, brings the total flavones regression equation calculation into and obtains concentration C
OnBe 1.118mg/mL, C
DownBe 0.026mg/mL, so partition coefficient K is 42.96.This moment system to compare R be 1.3, the yield of then going up the phase total flavones is 99.2%.
Embodiment 2 lab scales
Supersound extraction: precision weighing Semen Vitis viniferae, adding the 60ml volume fraction through the 10g Semen Vitis viniferae powder that obtains after the roguing, washing, oven dry, pulverizing is in 30% the alcoholic solution, at power supersound process 5min under the condition of 325W, mixed liquor filtering and impurity removing with after the supersound process obtains the Semen Vitis viniferae crude extract;
Aqueous two-phase extraction: will form double-aqueous phase system in 3.0g dehydrated alcohol, 1.6g ammonium sulfate and the 3.4g water adding 2.0g Semen Vitis viniferae crude extract.Wherein the pH of double-aqueous phase system is 5.0.With each material mixing in the system, and room temperature (25 ℃) leaves standstill 20min, and layering obtains upper and lower phase, on be the ethanol phase mutually;
Concentrating under reduced pressure: get above-mentioned ethanol phase, 60 ℃ of concentrated, vacuum dryings of distilling under reduced pressure obtain total flavone from grap seeds.
Experimental result: partition coefficient K is 46.55, and total flavones is 98.3% at the yield of ethanol in mutually.
Embodiment 3 lab scales
Supersound extraction: precision weighing Semen Vitis viniferae, through roguing, washing, it is in 70% the alcoholic solution that the 10g Semen Vitis viniferae powder that obtains after pulverizing adds the 100ml volume fraction, and supersound process 15min, used ultrasonic power is 300W, mixed liquor filtering and impurity removing with after the supersound process obtains the Semen Vitis viniferae crude extract;
Aqueous two-phase extraction: will form double-aqueous phase system in 1.0g dehydrated alcohol, 2.1g ammonium sulfate, 0.1g sodium chloride and the described Semen Vitis viniferae crude extract of 3.8g water adding 3.0g.Wherein the pH of double-aqueous phase system is 9.0.With each material mixing in the system, and room temperature (25 ℃) leaves standstill 30min, and layering obtains upper and lower phase, on be the ethanol phase mutually;
Concentrating under reduced pressure: get above-mentioned ethanol phase, 80 ℃ of concentrated, vacuum dryings of distilling under reduced pressure obtain total flavone from grap seeds.
Experimental result: partition coefficient K is 41.96, and total flavones is 98.4% at the yield of ethanol in mutually.
Embodiment 4 lab scales
Supersound extraction: precision weighing is through roguing, washing, it is in 70% the alcoholic solution that the 10g Semen Vitis viniferae powder that obtains after pulverizing adds the 100ml volume fraction, and supersound process 15min, and used ultrasonic power is 325W, mixed liquor filtering and impurity removing with after the supersound process obtains the Semen Vitis viniferae crude extract;
Aqueous two-phase extraction: will form double-aqueous phase system in 2.1g dehydrated alcohol, 1.5g ammonium sulfate, 0.05g potassium chloride and the described Semen Vitis viniferae crude extract of 4.85g water adding 1.5g.Wherein the pH of double-aqueous phase system is 3.0.With each material mixing in the system, and room temperature (25 ℃) leaves standstill 30min, and layering obtains upper and lower phase, on be the ethanol phase mutually;
Concentrating under reduced pressure: get above-mentioned ethanol phase, 79 ℃ of concentrated, vacuum dryings of distilling under reduced pressure obtain total flavone from grap seeds.
Experimental result: partition coefficient K is 21.96, and total flavones is 98.8% at the yield of ethanol in mutually.
Embodiment 5 lab scales
Supersound extraction: precision weighing is through roguing, washing, it is in 70% the alcoholic solution that the 10g Semen Vitis viniferae powder that obtains after pulverizing adds the 100ml volume fraction, and supersound process 15min, and used ultrasonic power is 350W, mixed liquor filtering and impurity removing with after the supersound process obtains the Semen Vitis viniferae crude extract;
Aqueous two-phase extraction: will form double-aqueous phase system in 1.9g dehydrated alcohol, 2.3g ammonium sulfate, 0.15g potassium chloride and the described Semen Vitis viniferae crude extract of 3.15g water adding 2.5g.Wherein the pH of double-aqueous phase system is 11.0.With each material mixing in the system, and room temperature (25 ℃) leaves standstill 30min, and layering obtains upper and lower phase, on be the ethanol phase mutually;
Concentrating under reduced pressure: get above-mentioned ethanol phase, 80 ℃ of concentrated, vacuum dryings of distilling under reduced pressure obtain total flavone from grap seeds.
Experimental result: partition coefficient K is 25.96, and total flavones is 98.7% at the yield of ethanol in mutually.
Embodiment 6 pilot scales
Supersound extraction: precision weighing is through roguing, washing, it is in 70% the alcoholic solution that the 10kg Semen Vitis viniferae powder that obtains after pulverizing adds the 50L volume fraction, and supersound process 15min, and used ultrasonic power is 390W, mixed liquor filtering and impurity removing with after the supersound process obtains the Semen Vitis viniferae crude extract;
Aqueous two-phase extraction: will form double-aqueous phase system in 1.9kg dehydrated alcohol, 2.1kg ammonium sulfate, 0.20kg sodium chloride and the described Semen Vitis viniferae crude extract of 3.55kg water adding 2.25kg.Wherein the pH of double-aqueous phase system is 7.0.With each material mixing in the system, and room temperature (25 ℃) leaves standstill 30min, and layering obtains upper and lower phase, on be the ethanol phase mutually;
Concentrating under reduced pressure: get above-mentioned ethanol phase, 76 ℃ of concentrated, vacuum dryings of distilling under reduced pressure obtain total flavone from grap seeds.
Experimental result: partition coefficient K is 31.56, and total flavones is 99.0% at the yield of ethanol in mutually.
Embodiment 7 pilot scales
Supersound extraction: precision weighing is through roguing, washing, it is in 70% the alcoholic solution that the Semen Vitis viniferae powder that obtains 10kg after pulverizing adds the 100L volume fraction, and supersound process 15min, and used ultrasonic power is 210W, mixed liquor filtering and impurity removing with after the supersound process obtains the Semen Vitis viniferae crude extract;
Aqueous two-phase extraction: will form double-aqueous phase system in 23kg dehydrated alcohol, 17kg ammonium sulfate, 2.5kg sodium chloride and the described Semen Vitis viniferae crude extract of 40kg water adding 17.5kg.Wherein the pH of double-aqueous phase system is 7.0.With each material mixing in the system, and room temperature (25 ℃) leaves standstill 5min, and layering obtains upper and lower phase, on be the ethanol phase mutually;
Concentrating under reduced pressure: get above-mentioned ethanol phase, 75 ℃ of concentrated, vacuum dryings of distilling under reduced pressure obtain total flavone from grap seeds.
Experimental result: partition coefficient K is 41.96, and total flavones is 98.6% at the yield of ethanol in mutually.
Embodiment 8 tries greatly
Supersound extraction: precision weighing is through roguing, washing, it is in 70% the alcoholic solution that the 20kg Semen Vitis viniferae powder that obtains after pulverizing adds the 200L volume fraction, and supersound process 15min, and used ultrasonic power is 280W, mixed liquor filtering and impurity removing with after the supersound process obtains the Semen Vitis viniferae crude extract;
Aqueous two-phase extraction: will form double-aqueous phase system in 37.5Kg dehydrated alcohol, 34Kg ammonium sulfate, 1Kg sodium chloride and the described Semen Vitis viniferae crude extract of 90Kg water adding 37.5Kg.Wherein the pH of double-aqueous phase system is 7.0.With each material mixing in the system, and room temperature (25 ℃) leaves standstill 30min, and layering obtains upper and lower phase, on be the ethanol phase mutually;
Concentrating under reduced pressure: get above-mentioned ethanol phase, 78 ℃ of concentrated, vacuum dryings of distilling under reduced pressure obtain total flavone from grap seeds.
Experimental result: partition coefficient K is 28.89, and total flavones is 98.2% at the yield of ethanol in mutually.
The above embodiment only is that preferred implementation of the present invention is described; be not that scope of the present invention is limited; design under the prerequisite of spirit not breaking away from the present invention; various distortion and improvement that those of ordinary skills make technical scheme of the present invention all should fall in the definite protection domain of claims of the present invention.
Claims (10)
1. the method for total flavones in the double-aqueous phase system extraction Semen Vitis viniferae is characterized in that described method comprises the steps: earlier Semen Vitis viniferae to be prepared the Semen Vitis viniferae crude extract with ethanol extraction; Again dehydrated alcohol, ammonium sulfate, inorganic salt, water are joined in the described Semen Vitis viniferae crude extract and form double-aqueous phase system, mixing, room temperature leaves standstill the 5-30min layering, obtains upper and lower phase, gets through concentrating under reduced pressure and dry, obtains total flavone from grap seeds;
In described double-aqueous phase system, described Semen Vitis viniferae crude extract shared mass ratio in system is 5%-30%, described dehydrated alcohol shared mass ratio in system is 10%-30%, described ammonium sulfate shared mass ratio in system is 16%-30%, described inorganic salt shared mass ratio in system is 0-5%, the surplus water complements to 100%, and the pH of described double-aqueous phase system is 3.0-11.0.
2. the method for total flavones in the double-aqueous phase system extraction Semen Vitis viniferae according to claim 1 is characterized in that described Semen Vitis viniferae crude extract is to make as follows:
With the Semen Vitis viniferae powder of described Semen Vitis viniferae through obtaining after roguing, washing, oven dry, the pulverizing, add then and be equivalent to the alcoholic solution that Semen Vitis viniferae powder volume 6-10 doubly measures, the volume fraction of described alcoholic solution is 30-70%, supersound process 5-15min, ultrasonic power is 200-400W, with the mixed liquor filtering and impurity removing after the supersound process.
3. the method for total flavones in the double-aqueous phase system extraction Semen Vitis viniferae according to claim 2, it is characterized in that, in the preparation of described Semen Vitis viniferae crude extract, be to add the alcoholic solution that is equivalent to 8 times of amounts of Semen Vitis viniferae powder volume, the volume fraction of described alcoholic solution is 50%.
4. the method for total flavones is characterized in that in the described supersound process, used ultrasonic power is that 325W, processing time are 10min in the double-aqueous phase system extraction Semen Vitis viniferae according to claim 2.
5. the method for total flavones in the double-aqueous phase system extraction Semen Vitis viniferae according to claim 1, it is characterized in that, in the described double-aqueous phase system, described dehydrated alcohol shared mass ratio in system is 19%-23%, described ammonium sulfate shared mass ratio in system is 17%-24%, described inorganic salt shared mass ratio in system is 0-2.5%, and the surplus water complements to 100%.
6. the method for total flavones is characterized in that the pH of described double-aqueous phase system is 5.0-9.0 in the double-aqueous phase system extraction Semen Vitis viniferae according to claim 1.
7. the method for total flavones is characterized in that described inorganic salt includes but not limited to one or more in sodium chloride, the potassium chloride in the double-aqueous phase system extraction Semen Vitis viniferae according to claim 1.
8. the method for total flavones is characterized in that the described standing demix time is 10-20min in the double-aqueous phase system extraction Semen Vitis viniferae according to claim 1, and described concentrating under reduced pressure is also dry, is that described going up 60-80 ℃ of distilling under reduced pressure concentrated and vacuum drying.
9. the method for total flavones is characterized in that the temperature of described distilling under reduced pressure is 75-79 ℃ in the double-aqueous phase system extraction Semen Vitis viniferae according to claim 8.
10. the method for total flavones in the double-aqueous phase system extraction Semen Vitis viniferae is characterized in that described method comprises the steps:
A. with the Semen Vitis viniferae powder of described Semen Vitis viniferae through obtaining after roguing, washing, oven dry, the pulverizing, be to add that to be equivalent to Semen Vitis viniferae powder volume 8 times of amounts, volume fractions be 50% alcoholic solution, at used ultrasonic power supersound process 10min under the situation of 325W, with the mixed liquor filtering and impurity removing after the supersound process, get the Semen Vitis viniferae crude extract;
B. again dehydrated alcohol, ammonium sulfate, inorganic salt, water are joined in the described Semen Vitis viniferae crude extract and form double-aqueous phase system, mixing, room temperature leave standstill the 10-20min layering, obtain upper and lower phase, get, vacuum drying concentrated, obtain total flavone from grap seeds in 75 ℃ of distilling under reduced pressure;
In described double-aqueous phase system, described Semen Vitis viniferae crude extract shared mass ratio in system is 17.5%, described dehydrated alcohol shared mass ratio in system is 23%, described ammonium sulfate shared mass ratio in system is 17%, described sodium chloride shared mass ratio in system is 2.5%, the surplus water complements to 100%, and the pH of described double-aqueous phase system is 7.0.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101579021A CN103211926A (en) | 2013-05-02 | 2013-05-02 | Method for extracting total flavonoids in grape seeds in double-aqueous phase system |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013101579021A CN103211926A (en) | 2013-05-02 | 2013-05-02 | Method for extracting total flavonoids in grape seeds in double-aqueous phase system |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103211926A true CN103211926A (en) | 2013-07-24 |
Family
ID=48810312
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2013101579021A Pending CN103211926A (en) | 2013-05-02 | 2013-05-02 | Method for extracting total flavonoids in grape seeds in double-aqueous phase system |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103211926A (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103690577A (en) * | 2013-12-19 | 2014-04-02 | 甘肃凯源生物技术开发中心 | Method for ionic liquid aqueous two-phase extraction of flavones and saponins in songaria cynomorium herb |
| CN104435060A (en) * | 2014-11-05 | 2015-03-25 | 桂林三宝生物科技有限公司 | Method for extracting gynostemma pentaphyllum saponins from gynostemma pentaphyllum |
| CN104644815A (en) * | 2015-03-17 | 2015-05-27 | 柳州师范高等专科学校 | Method for extracting total flavonoids of Chinese wampee leaves employing two-phase aqueous system and ultrasonic integration |
| CN105748547A (en) * | 2014-12-16 | 2016-07-13 | 中国科学院大连化学物理研究所 | Method for separating active components from saussurea involucrata cell culture through extraction |
| CN107739359A (en) * | 2017-11-30 | 2018-02-27 | 天津农学院 | A kind of method using double-aqueous phase system extracting procyanidins |
| CN108003127A (en) * | 2017-11-30 | 2018-05-08 | 天津农学院 | A kind of method using aqueous two-phase system extraction longan skin procyanidins |
| CN109805051A (en) * | 2019-01-21 | 2019-05-28 | 杭州洲际食品有限公司 | Composite frozen dough characters modifying agent and preparation method thereof |
| CN112239710A (en) * | 2019-07-19 | 2021-01-19 | 四川酩创酒科技有限公司 | Total flavone extract and preparation method and application thereof |
| CN112826835A (en) * | 2021-02-05 | 2021-05-25 | 许昌学院 | Method for extracting active substances in honey |
-
2013
- 2013-05-02 CN CN2013101579021A patent/CN103211926A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 李羚, 杨雪滢, 高云涛: "<酿酒科技>", <双水相分离与超声提取耦合法从葡萄籽中提取抗氧化活性物质研究> * |
Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103690577A (en) * | 2013-12-19 | 2014-04-02 | 甘肃凯源生物技术开发中心 | Method for ionic liquid aqueous two-phase extraction of flavones and saponins in songaria cynomorium herb |
| CN103690577B (en) * | 2013-12-19 | 2016-02-24 | 甘肃凯源生物技术开发中心 | A kind of method of flavone and saponin in ionic liquid aqueous two-phase extraction Herba Cynomorii |
| CN104435060B (en) * | 2014-11-05 | 2018-03-20 | 桂林三宝生物科技有限公司 | A kind of method that gynosaponin is extracted from gynostemma pentaphylla |
| CN104435060A (en) * | 2014-11-05 | 2015-03-25 | 桂林三宝生物科技有限公司 | Method for extracting gynostemma pentaphyllum saponins from gynostemma pentaphyllum |
| CN105748547B (en) * | 2014-12-16 | 2019-03-01 | 中国科学院大连化学物理研究所 | A method of extracting isolating active component from saussurea involucrata cell culture |
| CN105748547A (en) * | 2014-12-16 | 2016-07-13 | 中国科学院大连化学物理研究所 | Method for separating active components from saussurea involucrata cell culture through extraction |
| CN104644815B (en) * | 2015-03-17 | 2017-11-07 | 柳州师范高等专科学校 | A kind of method of utilization double-aqueous phase system and ultrasonic integrated extraction Calusena lansium leaf flavonoids |
| CN104644815A (en) * | 2015-03-17 | 2015-05-27 | 柳州师范高等专科学校 | Method for extracting total flavonoids of Chinese wampee leaves employing two-phase aqueous system and ultrasonic integration |
| CN107739359A (en) * | 2017-11-30 | 2018-02-27 | 天津农学院 | A kind of method using double-aqueous phase system extracting procyanidins |
| CN108003127A (en) * | 2017-11-30 | 2018-05-08 | 天津农学院 | A kind of method using aqueous two-phase system extraction longan skin procyanidins |
| CN108003127B (en) * | 2017-11-30 | 2022-05-27 | 天津农学院 | Method for extracting procyanidine in longan skin by using aqueous two-phase system |
| CN109805051A (en) * | 2019-01-21 | 2019-05-28 | 杭州洲际食品有限公司 | Composite frozen dough characters modifying agent and preparation method thereof |
| CN112239710A (en) * | 2019-07-19 | 2021-01-19 | 四川酩创酒科技有限公司 | Total flavone extract and preparation method and application thereof |
| CN112826835A (en) * | 2021-02-05 | 2021-05-25 | 许昌学院 | Method for extracting active substances in honey |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103211926A (en) | Method for extracting total flavonoids in grape seeds in double-aqueous phase system | |
| CN103655928B (en) | A kind of combined-enzyme method extracts the method for tea polyphenols in tealeaf residue | |
| CN103980242B (en) | The method of Moringa flavones is extracted from leaf of Moringa | |
| CN104710391B (en) | Method for extracting luteolin and beta-sitosterol from peanut shells | |
| CN103172685B (en) | Method for extracting hesperidin and synephrine from immature bitter oranges | |
| CN102302592B (en) | Preparation technology and purpose of citrus grandis peel flavones | |
| CN101463027B (en) | Method for extracting and separating flavone and anthocyanidin from elder fruit | |
| CN104523836A (en) | Method for comprehensively extracting protein, polysaccharide and polyphenol from avocado kernels | |
| CN103815103B (en) | A kind of method extracting low-caffeine high content tea polyphenol from fresh tea leaf in its | |
| CN105061529A (en) | Extraction process of mulberry anthocyanin | |
| CN102746362A (en) | Method for extracting refined astragaloside from astragaliradix | |
| CN105311075A (en) | Preparation method of manyprickle acanthopanax root extract | |
| CN102633900A (en) | Method for extracting and purifying polysaccharide from Cordyceps militaris | |
| CN110496179A (en) | A kind of method and application for rapidly and efficiently extracting antioxidant in Areca | |
| CN103709014B (en) | High and the Hydroxytyrosol extracting method that the rate of recovery is high of a kind of transformation efficiency | |
| CN104940280A (en) | Method for extracting total flavones from radix puerariae employing enzyme preparation | |
| CN102070411A (en) | Method for refining honokiol | |
| CN104211690B (en) | Method for separating and purifying mangiferin from aquilaria sinensis leaves | |
| CN101474350B (en) | Method for extracting total saponin in asparagus and use thereof | |
| CN105153253A (en) | Purple sweet potato anthocyanin extraction process | |
| CN105085224B (en) | A kind of method that hypericin is extracted from hypericum perforatum | |
| CN106565422A (en) | Extraction process for hydroxytyrosol from olive leaf | |
| CN104586904B (en) | A kind of separated in synchronization prepares cynomorium songaricum polysaccharide and the method for cynomorium songaricum flavones | |
| CN105920089A (en) | Method for preparing plant total polyphenol from walnut green peel through efficient separation | |
| CN115252489A (en) | Preparation method and application of camellia japonica flower and leaf extract |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C12 | Rejection of a patent application after its publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20130724 |