CN101288468B - Method of sequential extraction of biological activity component from jujube - Google Patents
Method of sequential extraction of biological activity component from jujube Download PDFInfo
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- CN101288468B CN101288468B CN200810055155XA CN200810055155A CN101288468B CN 101288468 B CN101288468 B CN 101288468B CN 200810055155X A CN200810055155X A CN 200810055155XA CN 200810055155 A CN200810055155 A CN 200810055155A CN 101288468 B CN101288468 B CN 101288468B
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Abstract
The invention discloses a fractional method for extracting bioactive components from dates; the dates are selected, enucleated, washed with water, dried, ground into particles, added with 65-75% of ethanol to be extracted for 2-3 times, and separated into date slag and filtrate; the filtrate is concentrated to obtain total flavonol soluble extract, the date slag is added with deionized water, the weight of which is 10-15 times that of the date slag, to be extracted for 2-3 times and separated into water extract and residue; the water extract is concentrated to 1/8-1/6 of the original volume, the concentrated solution is added with 95% of ethanol which is 4-6 times that of the volume of the concentrated solution to carry out alcohol precipitation separation for 10-18 hours, so as to obtain precipitate and filtrate; the precipitate is washed by the ethanol with the concentration of over 98% for 2-3 times, and is dried to obtain date crude polysaccharide, the filtrate is concentrated to obtain ribonucleotide water soluble extract; the residue is dried and ground into dietary fiber powder. The method realizes one-step fractional extraction of a plurality of active components from the dates, has simple operation, and does not adopt any organic solvent except ethanol, thus having safety, no toxicity and residue; the active components in dates can be completely extracted, thus achieving the purpose of making best use of dates.
Description
Technical field
The invention belongs to the natural product extracting technique field, be specifically related to a kind of method of from jujube, extracting multiple bioactive ingredients.The present invention adopts grading extraction technology simultaneously, extracts the molten medicinal extract of general flavone alcohol, the thick polysaccharide of jujube, nucleotides medicinal extract and dietary fiber from jujube.
Background technology
Jujube is the ripening fruits of the perennial deciduous plant jujube tree of Rhamnaceae, just is listed in one of " five fruits " (peach, Lee, plum, apricot, jujube) from ancient times, and is with a long history.Contain various bioactive ingredients (comprising mono-and di-saccharides class, compound sugar, polysaccharide, protein, fat, organic acid, mineral matter, nucleotides, triterpene compound, flavonoids etc.) in the date fruit, have multiple nutritive value and health care, be rated as the natural treasure-house of a nutriment.Jujube is traditional medicinal and edible plant, also is the distinctive living resources of China.The traditional Chinese medical science is thought that jujube has tonifying middle-Jiao and Qi, nourishing blood to promote the production of body fluid, the town of calming the nerves is painful and is regulated function such as drug effect.Jujube is not only nutritious, and delicious taste, and the laudatory title of " kings of all kinds of fruits " is arranged.
Jujube deep processed product on the domestic market is a lot of at present, as dried jujube, candied date, jujube sheet, jujube sauce, jujube wine etc., these products are adding color, shape and the quality that has changed the jujube fruit man-hour, and characteristic nutrition and bioactive ingredients in the jujube fruit are not fully utilized.
Deep day by day along with jujube research and development, about extracting polysaccharide, nucleotides, flavonoids in the jujube fruit, and it is also more and more to extract the relevant report document of polysaccharide, triterpenic acid technology from the jujube slag.CN1175758C disclose a kind of from jujube the method for separation and Extraction cyclic nucleotide syrup, dietary fiber and jujube wax, this method adopts alcohol extract, make the jujube food fibre powder behind the alcohol extracting residue evaporate to dryness, alcohol extract is through organic solvent extraction, isolate jujube wax, raffinate concentrates and makes cyclic nucleotide syrup, has realized the purpose by the active component and the physicochemical property exploitation multiple product of jujube.CN101139402A discloses a kind of method of extracting polysaccharide from date, and this technology is extracted the date water, adds fining agent in the water extract, obtains the jujube polysaccharide after alcohol precipitation, separation, drying.
More than the general character defective that exists of two technology be: one, all used a large amount of organic solution and compound in jujube extraction of active ingredients process, not only environment has been caused pollution, residual in the final products also can bring food-safety problem; Two, be rich in the various active composition in the jujube, and above-mentioned technology has just been extracted a part wherein separately, does not accomplish comprehensive extraction, makes the best use of everything.
Summary of the invention
The invention provides a kind of method of from jujube, extracting the molten medicinal extract of general flavone alcohol, the thick polysaccharide of jujube, nucleotides medicinal extract and dietary fiber, its objective is the problem that organic solution is polluted and the jujube resource can not get making the best use of everything that prior art exists that solves, extract by hierarchical synthesis, realized the effect that contained bioactive ingredients is extracted to the greatest extent in the jujube.
Fractional extraction method of the present invention comprises the steps:
(1) jujube cleaned, after the stoning, washing, drying, is ground into 10～40 purpose particles;
(2) add 65～75% alcohol extract 2～3 times in jujube granule, be separated into jujube slag and filtrate, filtrate concentrates to such an extent that contain the pure dissolubility medicinal extract of general flavone;
(3) add the deionized water that accounts for 10～15 times of jujube slag weight in the jujube slag, under the condition of pH=4～12, extract, repeat to extract 2～3 times, be separated into water extract and residue;
(4) merge the water extract, regulate the pH value to neutrality, be concentrated into 1/8～1/6 of original volume, 95% ethanol that adds 4～6 times of concentrate volumes slowly stirs, and alcohol precipitation separates 10～18h, get sediment and filtrate, sediment cleans 2～3 times with the ethanol more than 98%, the dry thick polysaccharide of jujube that gets, and concentrating filter liquor obtains containing the water-soluble medicinal extract of nucleotides;
(5) after the residue drying, be ground into 60～300 purpose food fibre powders.
Wherein, the drying of material can be the vacuum drying under forced air drying or the vacuum 0.06～0.095MPa in the technology, at 50～80 ℃ of drying 5～20h, to the water content of material be 5～20%.
Material extracting method in the technology can adopt one or several the complex method in conventional immersion method, supercritical ultrasonics technology, the microwave method to carry out.Conventional immersion method wherein is to extract 0.5～5h under 40～80 ℃ of conditions; Supercritical ultrasonics technology is that the ultrasonic wave with frequency 25～80KHz, power 50～1000W extracts 10～60min under 40～80 ℃ of conditions; Microwave method is with Microwave Extraction 10～60min of frequency 30～100MHz, power 50～1200W under 40～80 ℃ of conditions.
The concentrated employing decompression of material concentrates in the technology, carries out under the condition of 40～90 ℃ of temperature, pressure 0.04～0.095MPa.
The main component of the pure dissolubility medicinal extract that the present invention obtains is the jujube Flavonoid substances.
The main component of the thick polysaccharide of date that the present invention obtains has water-soluble polysaccharide, crude protein and mineral matter etc. multiple, can be ground into 60～100 purpose fine powders, in incapsulating, is prepared into the thick polyoses extract product of jujube fruit.
The water-soluble medicinal extract that the present invention obtains mainly contains water soluble ingredients such as nucleotides, monose, disaccharide, compound sugar, can be used as foodstuff base material or with the composite processing health beverages of other food.
Last residue mechanical crushing to 60～100 purpose fine powders, perhaps mechanical coarse crushing earlier, further ultra tiny pulverizing makes fineness reach 100～300 orders, and the main component of this powder is a dietary fiber.
Major advantage of the present invention is: (1) has realized the separation and Extraction of various active composition in the jujube by simple extraction process flow process, compared with prior art, has advantage simple to operate, that cost is low; (2) the ethanol of using always except that the use food processing in the extraction process, do not use other any organic solvents, have the advantage of safety non-toxic, noresidue; (3) several active components of separation and Extraction physiological function of having nothing in common with each other can be segmented as the raw material of health food or the intermediate of medicine, accomplishes to make the best use of everything.
Description of drawings
Fig. 1 is the process flow diagram of the present invention's sequential extraction of biological activity component from jujube.
The specific embodiment
Embodiment 1
Ripe jujube is really rejected non-edible parts such as disease and pest corrosion, clean up manual stoning with mobile running water.Take by weighing the 1Kg jujube and really place air dry oven, in 60～65 ℃ of dry 10h, to water content about 10%.The jujube of drying is really taken out, and after the cooling, mechanical crushing becomes 10 purpose particles.
Add 65% ethanol 10L in the jujube fruit granule, the ultrasonic echography with frequency 25KHz, power 200W under 50 ℃ extracts 40min, repeats to extract standing separation 2 times.Merging filtrate, in 60 ℃, 0.08MPa down decompression concentrate and reclaim ethanol, obtain pure dissolubility medicinal extract 460g, its main component is the jujube Flavonoid substances.
Add the 10L deionized water in the jujube slag that obtains after the alcohol extracting, regulator solution pH=7 adopts conventional immersion method to extract, and extracts 50 ℃ of temperature, time 1.5h, and centrifugation is water extract and jujube slag.The jujube slag repeats to extract 2 times, obtains water extract 18.8L altogether, jujube slag 1970g.
The water extract is evaporated to 3.2L under 70 ℃, 0.09MPa, add 95% ethanol of 16L again, slowly stirs, and alcohol precipitation separates more than the 10h, and suction filtration obtains sediment 32.5g, filtrate 18.3L.
Sediment is cleaned 2 times with the ethanol more than 98%, each 300mL, 40 ℃ of forced air dryings obtain the thick polyoses extract 29.5g of jujube fruit after the pulverizing.Wherein polyoses content 30.6%, moisture 12.1%.
Filtrate in 50 ℃, 0.09MPa down decompression concentrate and reclaim ethanol, be concentrated into soluble solid content and account for 65%, obtain medicinal extract 750g.Contain multiple water soluble ingredients such as nucleotides, monose, disaccharide, compound sugar in the medicinal extract, wherein nucleotide content 176mg.
Residue after the alcohol extracting places air dry oven, and in 60～65 ℃ of following dry 10h, to water content below 10%, cooling, mechanical crushing becomes 80 purpose fine powder 120g, and wherein dietary fiber content 62.3%.
Embodiment 2
Ripe jujube is really rejected non-edible parts such as disease and pest corrosion, clean up manual stoning with mobile running water.Take by weighing the 500g jujube and really place air dry oven, in 60～65 ℃ of dry 10h, to water content about 10%.The jujube of drying is really taken out, and after the cooling, mechanical crushing becomes 20 purpose particles.
Add 70% ethanol 6L in the jujube fruit granule, with the Microwave Extraction 30min of frequency 40MHz, power 500W, repeat to extract standing separation 2 times under 60 ℃.Merging filtrate, in 63 ℃, 0.09MPa down decompression concentrate and reclaim ethanol, obtain pure dissolubility medicinal extract 238g, its main component is the jujube Flavonoid substances.
Add the 4.5L deionized water in the jujube slag that obtains after the alcohol extracting, regulator solution pH=5 adopts conventional immersion method to extract, and extracts 50 ℃ of temperature, time 1h, and regulator solution pH value is neutral, centrifugation is water extract and jujube slag.The jujube slag repeats to extract 3 times, obtains water extract 12.8L altogether, jujube slag 970g.
The water extract is evaporated to 1.6L under 75 ℃, 0.09MPa, add 95% ethanol of 9.6L, slowly stirs, and alcohol precipitation separates more than the 10h, and suction filtration obtains sediment 15.5g, filtrate 10.7L.
Sediment is cleaned 2 times with the ethanol more than 98%, each 120mL, 45 ℃ of forced air dryings obtain the thick polyoses extract 13.8g of jujube fruit after the pulverizing.Wherein polyoses content 38.4%, moisture 11.7%.
Filtrate in 60 ℃, 0.08MPa down decompression concentrate and reclaim ethanol, be concentrated into soluble solid content and account for 63%, obtain medicinal extract 362g.Contain multiple water soluble ingredients such as nucleotides, monose, disaccharide, compound sugar in the medicinal extract, wherein nucleotide content 86mg.
Residue after the alcohol extracting places air dry oven, in 60～65 ℃ of following dry 10h, and to water content below 10%, cooling, mechanical coarse crushing, further micropowders is broken into 250 purpose fine powder 97g, and wherein dietary fiber content 64.4%.
Embodiment 3
Ripe jujube is really rejected non-edible parts such as disease and pest corrosion, clean up, stoner stoning automatically with mobile running water.Take by weighing the 1kg jujube and really place air dry oven, in 60～65 ℃ of dry 12h, to water content about 8%.The jujube of drying is really taken out, and after the cooling, mechanical crushing becomes 40 purpose particles.
Add 70% ethanol 10L in the jujube fruit granule, extract 2h in 60 ℃ of water-baths.Repeat to extract standing separation 3 times.Merging filtrate, in 58 ℃, 0.07MPa down decompression concentrate and reclaim ethanol, obtain pure dissolubility medicinal extract 505g, its main component is the jujube Flavonoid substances.
Add the 9.2L deionized water in the jujube slag that obtains after the alcohol extracting, regulator solution pH=11 adopts microwave method to extract, frequency 50MHz, and power 800W, 50 ℃ of temperature, time 30min, it is neutral transferring pH, centrifugation is water extract and jujube slag.The jujube slag repeats to extract 2 times, obtains water extract 17.3L altogether, jujube slag 1710g.
The water extract is evaporated to 2.5L under 75 ℃, 0.09MPa, add 95% ethanol of 10L again, slowly stirs, and alcohol precipitation separates more than the 14h, and suction filtration obtains sediment 35.4g, filtrate 11.6L.
Sediment is cleaned 2 times with the ethanol more than 98%, each 350mL, 45 ℃ of forced air dryings obtain the thick polyoses extract 32.9g of jujube fruit after the pulverizing.Wherein polyoses content 35.4%, moisture 12.6%.
Filtrate in 60 ℃, 0.08MPa down decompression concentrate and reclaim ethanol, be concentrated into soluble solid content and account for 73%, obtain medicinal extract 722g.Contain multiple water soluble ingredients such as nucleotides, monose, disaccharide, compound sugar in the medicinal extract, wherein nucleotide content 168mg.
Residue after the alcohol extracting places air dry oven, in 60～65 ℃ of following dry 10h, and to water content below 10%, cooling, mechanical coarse crushing, further micropowders is broken into 180 purpose fine powder 106g, and wherein dietary fiber content 63.6%.
Claims (8)
1. the method for a sequential extraction of biological activity component from jujube comprises the steps:
(1) jujube cleaned, after the stoning, washing, drying, is ground into 10～40 purpose particles;
(2) add 65～75% alcohol extract 2～3 times in jujube granule, be separated into jujube slag and filtrate, filtrate concentrates to such an extent that contain the pure dissolubility medicinal extract of general flavone;
(3) add the deionized water that accounts for 10～15 times of jujube slag weight in the jujube slag, under the condition of pH=4～12, extract, repeat to extract 2～3 times, be separated into water extract and residue;
(4) merge the water extract, regulate the pH value to neutrality, be concentrated into 1/8～1/6 of original volume, 95% ethanol that adds 4～6 times of concentrate volumes slowly stirs, and alcohol precipitation separates 10～18h, get sediment and filtrate, sediment cleans 2～3 times with the ethanol more than 98%, the dry thick polysaccharide of jujube that gets, and concentrating filter liquor obtains containing the water-soluble medicinal extract of nucleotides;
(5) after the residue drying, be ground into 60～300 purpose food fibre powders.
2. according to claim 1 from jujube the method for sequential extraction of biological activity component, it is characterized in that the drying in the described technology is at 50～80 ℃ of drying 5～20h, to the water content of material be 5～20%.
3. according to claim 2 from jujube the method for sequential extraction of biological activity component, it is characterized in that described drying is the vacuum drying under forced air drying or the vacuum 0.06～0.095MPa.
4. according to claim 1 from jujube the method for sequential extraction of biological activity component, it is characterized in that material extracting method in the described technology adopts one or several the complex method in conventional immersion method, supercritical ultrasonics technology, the microwave method to carry out.
5. according to claim 4 from jujube the method for sequential extraction of biological activity component, it is characterized in that described conventional immersion method is to extract 0.5～5h under 40～80 ℃ of conditions.
6. according to claim 4 from jujube the method for sequential extraction of biological activity component, it is characterized in that described supercritical ultrasonics technology is that the ultrasonic wave with frequency 25～80KHz, power 50～1000W extracts 10～60min under 40～80 ℃ of conditions.
7. according to claim 4 from jujube the method for sequential extraction of biological activity component, it is characterized in that described microwave method is with Microwave Extraction 10～60min of frequency 30～100MHz, power 50～1200W under 40～80 ℃ of conditions.
8. according to claim 1 from jujube the method for sequential extraction of biological activity component, it is characterized in that material in the described technology concentrates to adopt decompression to concentrate, under the condition of 40～90 ℃ of temperature, pressure 0.04～0.095MPa, carry out.
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| CN108354146A (en) * | 2018-01-22 | 2018-08-03 | 中山大学 | The integrated extraction technique of active material in a kind of ginger |
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| CN101942213A (en) * | 2010-09-30 | 2011-01-12 | 福建农林大学 | Method for extracting red date pigment |
| CN102461898A (en) * | 2010-11-12 | 2012-05-23 | 天津市食品研究所有限公司 | Technological process for extracting flavone from jujube fruits |
| CN102061322B (en) * | 2010-11-12 | 2013-10-09 | 盐城工学院 | Method for preparing polysaccharide, flavone and dietary fiber of peanut hulls in united manner |
| CN103421125A (en) * | 2012-05-15 | 2013-12-04 | 周鑫 | Comprehensive utilization method of jujube residue |
| CN103330157A (en) * | 2013-04-23 | 2013-10-02 | 申琳 | Red date extract extraction method and red date extracts |
| CN107212314A (en) * | 2017-03-13 | 2017-09-29 | 浙江大学 | The method of active principle in serialization grading extraction jujube |
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| CN1408257A (en) * | 2002-09-25 | 2003-04-09 | 河北农业大学 | Separating and extracting method for date cyclic nucleotide syrup, dietary fibre and date wax |
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