CN1876685B - Method for extracting apple polysaccharide from concentrated apple juice production - Google Patents
Method for extracting apple polysaccharide from concentrated apple juice production Download PDFInfo
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- CN1876685B CN1876685B CN2005100176654A CN200510017665A CN1876685B CN 1876685 B CN1876685 B CN 1876685B CN 2005100176654 A CN2005100176654 A CN 2005100176654A CN 200510017665 A CN200510017665 A CN 200510017665A CN 1876685 B CN1876685 B CN 1876685B
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Abstract
The invention relates the preparing method of extracting apple polysaccharide, belonging to extracting polysaccharide technology field. The method extracts apple polysaccharide from filter thickening liquid of enriching apple process. The method comprises the following steps: extracting film filter thickening liquid, rouging, and extracting again; or salifying the film filter thickening liquid with caustic soda, neutralizing with alcaine, and extracting; or treating film filter thickening liquid with trichloroacetic acid, extracting, and extracting again. The method has the advantages of improving availability ratio and reducing environmental influence.
Description
Technical field
The invention belongs to apple polysaccharide extractive technique field, particularly a kind of production method of in the apple juice production process, utilizing the dense poly-liquid of membrane filtration to extract polysaccharose substance.
Background technology
The concentrated Succus Mali pumilae production process is as follows: (1) raw material is really purchased: before producing the arriving in season every year apple purchase zone is generally investigated, to determine the purchase zone of safety.The apple of acceptance(check) is deposited in the fruit storehouse.(2) broken squeezing: choose apple after qualified and enter that grinding machine is broken to be squeezed.(3) pre-crust kills: fruit juice groove fruit juice is squeezed into turbid juice jar through the fruit juice pump and is carried out pre-sterilizing through interchanger again.(4) enzymolysis: the fruit juice after pre-crust kills enters enzymatic vessel through the plate-type heat exchanger cooling and carries out enzymolysis.(5) membrane filtration: the abundant fruit juice of enzymolysis, be pumped to respectively membrane filter appts filter clear juice.(6) decolouring: clear juice pumps into decolorizing column by clear juice jar and handles.(7) concentrate: the fruit juice after the decolouring pumps into vaporizer and concentrates.(8) crust kills: the fruit juice after concentrating carries out final pasteurising.(9) can: the fruit juice after crust kills cools off through interchanger, carries out sterile filling by filling machine.(10) packing: finished product be packaged as sterile bag, steel drum, plastic lining bag, liquid bag.(11) store: the finished product concentrated apple clear juice leaves in the freezer in batches.
In present production technique, behind the membrane filter appts operation certain hour, insoluble solid content increases in the circulation fluid, and the filtered solution flow descends, at this moment can be dense poly-liquid discharging in the circulation tank, in case influence filtering membrane.In this technology, all to drain a large amount of dense poly-liquid before each the cleaning.And in this dense poly-liquid, contain profuse polysaccharose substance, and therefore it is fully utilized, it is extremely important to turn waste into wealth.
Summary of the invention
The object of the invention is to provide a kind of method of extracting apple polysaccharide from the fruit juice concentrate production process.
For reaching above-mentioned purpose, the present invention adopts following technical scheme: extract the method for apple polysaccharide from the concentrated Succus Mali pumilae production process, extract apple polysaccharide from the dense poly-liquid of membrane filtration.
The aperture of filtering with film is 0.001-10 μ m.
The dense poly-liquid of membrane filtration through alcohol analyse, water-soluble impurity elimination, alcohol is analysed and is obtained again.
Get the dense poly-liquid of membrane filtration and be heated to 60-100 ℃, add 1-3 times of volume of ethanol, get the polysaccharide precipitate; Boiling water dissolving, filtration, filtrate that the polysaccharide precipitate adds 1 times of polysaccharide volume are concentrated into 1/2 volume, add 2 times of volume ethanol of concentrated solution, get the polysaccharide precipitate.
The dense poly-liquid of membrane filtration is analysed and is obtained through highly basic salinization, acid neutralization, alcohol.
Get the dense poly-liquid of membrane filtration and add equal-volume 0.1-0.8mol/l sodium hydroxide solution, 60-100 ℃ of heating 10-90min, hydrochloric acid is neutralized to neutrality, filters gained filtrate and adds its 1-5 times volume ethanol, gets the polysaccharide precipitate.
Adding equal-volume ethanol leaves standstill behind the dense poly-liquid deproteinated of membrane filtration, filters gained filtrate and concentrates 2-5 times of volume ethanol of back adding, and stand at low temperature gets the polysaccharide precipitate.
The present invention improves the membrane filter appts cleaning step, and the dense poly-liquid of discharging is collected, and heats then, a series of processing such as alkali or trichoroacetic acid(TCA) are handled, the extraction of alcohol precipitation, drying, extracts polysaccharose substance wherein.The apple polysaccharide that obtains by above method extraction is removed small molecules → vacuum-drying with 95% ethanol, acetone, ether, absolute ethanol washing → decolouring → Deproteinization → dialysis successively can obtain highly purified apple polysaccharide.
Embodiment
Embodiment 1, extract the method for apple polysaccharide from the fruit juice concentrate production process, get dense poly-liquid 200ml, be heated to 80 ℃, kept 1.5 hours, add the dehydrated alcohol of 3 times of volumes, leave standstill, 5 ℃ refrigerate 3 hours polysaccharide and separate out.Take out the polysaccharide precipitate, add 1 times of volume boiling water, after the polysaccharide dissolving, filtered while hot impurity, evaporation concentration to 1/3 volume adds 2 times of volume ethanol, takes out the polysaccharide precipitate, and 50 ℃ of constant pressure and dries get apple polysaccharide.
Embodiment 2, from the fruit juice concentrate production process, extract the method for apple polysaccharide, get dense poly-liquid 200ml, be heated to 100 ℃, kept 1 hour, the dehydrated alcohol of 1 times of volume of adding, normal temperature leaves standstill 5 hours polysaccharide and separates out.Filter, take out the polysaccharide precipitate, add 1.5 times of volume boiling water, after the dissolving, filtered while hot impurity, evaporation concentration to 1/2 volume adds 3 times of volume ethanol, takes out the polysaccharide precipitate, and 40 ℃ of vacuum-dryings get apple polysaccharide.
Embodiment 3, from the fruit juice concentrate production process, extract the method for apple polysaccharide, get dense poly-liquid 200ml, be heated to 90 ℃, kept 3.5 hours, the dehydrated alcohol of 2 times of volumes of adding, polysaccharide is separated out.Take out the polysaccharide precipitate, add 2 times of volume boiling water, after the dissolving, filtered while hot impurity, evaporation concentration to 1/2 volume adds 2 times of volume ethanol, takes out the polysaccharide precipitate, and vacuum-drying gets apple polysaccharide.
Embodiment 4, from the fruit juice concentrate production process, extract the method for apple polysaccharide, get dense poly-liquid 300ml and place beaker, add 50ml 0.8mol/LNaOH solution, 80 ℃ of water-bath 20min, with the hydrochloric acid neutrality that neutralizes, the centrifugal 30min of 5000r/min gets supernatant liquor again, add 3 times of volume ethanol of supernatant liquor, centrifugal 5000r/min, 30min gets precipitation, 50 vacuum-dryings get apple polysaccharide.
Embodiment 5, from the fruit juice concentrate production process, extract the method for apple polysaccharide, get dense poly-liquid 300ml and place beaker, add 100 ℃ of water-bath 90min of 100ml 0.1mol/LNaOH solution, again with the hydrochloric acid neutrality that neutralizes, the centrifugal 90min of 5000r/min, get supernatant liquor, add 5 times of volume ethanol of supernatant liquor, the centrifugal 50min of centrifugal 5000r/min gets precipitation, 40 ℃ of dryings get apple polysaccharide.
Embodiment 6, from the fruit juice concentrate production process, extract the method for apple polysaccharide, get dense poly-liquid 300ml and place beaker, add 250ml0.4mol/LNaOH solution, 100 ℃ of water-bath 60min, again with the hydrochloric acid neutrality that neutralizes, the centrifugal 90min of 5000r/min gets supernatant liquor, adds 3 times of volume ethanol of supernatant liquor, the centrifugal 60min of centrifugal 5000r/min, get precipitation, vacuum-drying gets apple polysaccharide.
Embodiment 7, from the fruit juice concentrate production process, extract the method for apple polysaccharide, get the dense poly-liquid of 300ml centrifugal → supernatant liquor adds behind the 10% trichoroacetic acid(TCA) mixing of 10ml 10 ℃ and leaves standstill 24h, centrifugal, get supernatant liquor and add the long-pending ethanol of monoploid, leave standstill 60min, the centrifugal 60min of 8000r/min → collection supernatant liquor rotary evaporation concentrates → adds the long-pending ethanol of tetraploid → 4 ℃ of centrifugal 15min → collecting precipitations of standing over night → 8000r/min, and 60 ℃ of vacuum-dryings get polysaccharide.
Embodiment 8, from the fruit juice concentrate production process, extract the method for apple polysaccharide, get the dense poly-liquid of 300ml centrifugal → supernatant liquor adds behind the 8% trichoroacetic acid(TCA) mixing of 20ml 10 ℃ and leaves standstill 10h, centrifugal, get supernatant liquor and add 3 times of volume ethanol → leave standstill 15min, the centrifugal 30min of 8000r/min → collection supernatant liquor rotary evaporation concentrates → adds the long-pending ethanol of tetraploid → 4 ℃ of centrifugal 15min → collecting precipitations of standing over night → 8000r/min, and 40 ℃ of vacuum-dryings get polysaccharide.
Embodiment 9, from the fruit juice concentrate production process, extract the method for apple polysaccharide, get the dense poly-liquid of 300ml centrifugal → supernatant liquor adds behind the 15% trichoroacetic acid(TCA) mixing of 10ml 5 ℃ and leaves standstill 24h, centrifugal, get supernatant liquor and add 3 times of volume ethanol → leave standstill 30min, the centrifugal 60min of 8000r/min → collection supernatant liquor rotary evaporation concentrates → adds the long-pending ethanol of tetraploid → 4 ℃ of centrifugal 15min → collecting precipitations of standing over night → 8000r/min, and 60 ℃ of vacuum-dryings get polysaccharide.
Embodiment 10, from the fruit juice concentrate production process, extract the method for apple polysaccharide, get dense poly-liquid 2000L, place double boiler, 10kg sodium hydroxide elder generation chemical solution, slowly add dense poly-liquid again, double boiler is heated to 90 degree keeps 30min, cooling back is with the hydrochloric acid neutrality that neutralizes, the centrifugal 30min of 5000r/min gets supernatant liquor, adds 3 times of volume ethanol of supernatant liquor, centrifugal, get precipitation, 40 ℃ of vacuum-dryings get apple polysaccharide.
Embodiment 11, from the fruit juice concentrate production process, extract the method for apple polysaccharide, get dense poly-liquid 2000L, place double boiler, 16kg sodium hydroxide elder generation chemical solution, slowly add dense poly-liquid again, double boiler is heated to 90 degree keeps 30min, cooling back is with the hydrochloric acid neutrality that neutralizes, the centrifugal 30min of 5000r/min gets supernatant liquor, adds 3 times of volume ethanol of supernatant liquor, centrifugal, get precipitation, 40 ℃ of vacuum-dryings get apple polysaccharide.
Embodiment 12, from the fruit juice concentrate production process, extract the method for apple polysaccharide, get dense poly-liquid 2000L, place double boiler, 30kg sodium hydroxide elder generation chemical solution, slowly add dense poly-liquid again, double boiler is heated to 90 degree keeps 30min, cooling back is with the hydrochloric acid neutrality that neutralizes, the centrifugal 30min of 5000r/min gets supernatant liquor, adds 3 times of volume ethanol of supernatant liquor, centrifugal, get precipitation, 40 ℃ of vacuum-dryings get apple polysaccharide.
Claims (7)
1. from the concentrated Succus Mali pumilae production process, extract the method for apple polysaccharide, it is characterized in that, from the dense poly-liquid of membrane filtration, extract apple polysaccharide, get the dense poly-liquid of membrane filtration and be heated to 60-100 ℃, add 1-3 times of volume of ethanol, get the polysaccharide precipitate; Boiling water dissolving, filtration, filtrate that the polysaccharide precipitate adds 1 times of polysaccharide volume are concentrated into 1/2 volume, add 2 times of volume ethanol of concentrated solution, get the polysaccharide precipitate.
2. the method for claim 1 is characterized in that, the aperture of filtering with film is 0.001-10 μ m.
3. from the concentrated Succus Mali pumilae production process, extract the method for apple polysaccharide, it is characterized in that, from the dense poly-liquid of membrane filtration, extract apple polysaccharide, get the dense poly-liquid of membrane filtration and add equal-volume 0.1-0.8mol/l sodium hydroxide solution, 60-100 ℃ of heating 10-90min, hydrochloric acid is neutralized to neutrality, filters gained filtrate and adds its 1-5 times volume ethanol, gets the polysaccharide precipitate.
4. method as claimed in claim 3 is characterized in that, the aperture of filtering with film is 0.001-10 μ m.
5. from the concentrated Succus Mali pumilae production process, extract the method for apple polysaccharide, it is characterized in that, from the dense poly-liquid of membrane filtration, extract apple polysaccharide, it is centrifugal to get the dense poly-liquid of 300ml, 10 ℃ leave standstill 24h behind the 10% trichoroacetic acid(TCA) mixing of supernatant liquor adding 10ml, centrifugal, get supernatant liquor and add the long-pending ethanol of monoploid, leave standstill 60min, the centrifugal 60min of 8000r/min, collecting the supernatant liquor rotary evaporation concentrates, add the long-pending ethanol of tetraploid, 4 ℃ of standing over night, the centrifugal 15min of 8000r/min, collecting precipitation, 60 ℃ of vacuum-dryings get polysaccharide.
6. from the concentrated Succus Mali pumilae production process, extract the method for apple polysaccharide, it is characterized in that, from the dense poly-liquid of membrane filtration, extract apple polysaccharide, it is centrifugal to get the dense poly-liquid of 300ml, 10 ℃ leave standstill 10h behind the 8% trichoroacetic acid(TCA) mixing of supernatant liquor adding 20ml, centrifugal, get supernatant liquor and add 3 times of volume ethanol, leave standstill 15min, the centrifugal 30min of 8000r/min, collecting the supernatant liquor rotary evaporation concentrates, add the long-pending ethanol of tetraploid, 4 ℃ of standing over night, the centrifugal 15min of 8000r/min, collecting precipitation, 40 ℃ of vacuum-dryings get polysaccharide.
7. from the concentrated Succus Mali pumilae production process, extract the method for apple polysaccharide, it is characterized in that, from the dense poly-liquid of membrane filtration, extract apple polysaccharide, it is centrifugal to get the dense poly-liquid of 300ml, 5 ℃ leave standstill 24h behind the 15% trichoroacetic acid(TCA) mixing of supernatant liquor adding 10ml, centrifugal, get supernatant liquor and add 3 times of volume ethanol, leave standstill 30min, the centrifugal 60min of 8000r/min, collecting the supernatant liquor rotary evaporation concentrates, add the long-pending ethanol of tetraploid, 4 ℃ of standing over night, the centrifugal 15min of 8000r/min, collecting precipitation, 60 ℃ of vacuum-dryings get polysaccharide.
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| CN2005100176654A CN1876685B (en) | 2005-06-09 | 2005-06-09 | Method for extracting apple polysaccharide from concentrated apple juice production |
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| CN2005100176654A CN1876685B (en) | 2005-06-09 | 2005-06-09 | Method for extracting apple polysaccharide from concentrated apple juice production |
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| CN1876685B true CN1876685B (en) | 2010-12-15 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101167831B (en) * | 2007-10-29 | 2011-12-21 | 刘莉 | Apple polysaccharide, its preparation method and application in preventing and treating tumor metastasis medicine |
| CN103462140B (en) * | 2013-09-25 | 2014-07-23 | 江南大学 | Low frequency ultrasonic-assisted desugaring and deacidification method for concentrated waxberry juice |
| CN108606210A (en) * | 2018-03-08 | 2018-10-02 | 南昌大学 | A kind of composite juice beverage and preparation method thereof of high Vc contents |
| CN109045151A (en) * | 2018-09-29 | 2018-12-21 | 昆明医科大学第附属医院 | A kind of composition and preparation method thereof of regulation intestinal flora |
| DE102020208914A1 (en) * | 2020-07-16 | 2022-01-20 | Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung eingetragener Verein | PROCESS FOR OBTAINING GLYCAN EXTRACTS FROM APPLE POCKET, PROCESS FOR PRODUCING FUNCTIONALIZED GLYCANS, AND FUNCTIONALIZED GLYCAN PRODUCABLE BY THE PROCESS AND ITS USE |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1337410A (en) * | 2001-09-03 | 2002-02-27 | 王维新 | Production process of extracting fruit polysaccharide from fruits |
| CN1418892A (en) * | 2002-12-03 | 2003-05-21 | 南京大学 | Extraction refining method for aloe-polysaccharide |
| CN1473822A (en) * | 2003-08-05 | 2004-02-11 | 西安翠宝首饰集团公司 | Extracting process of flavone and poly saccharide in duckweed |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1337410A (en) * | 2001-09-03 | 2002-02-27 | 王维新 | Production process of extracting fruit polysaccharide from fruits |
| CN1418892A (en) * | 2002-12-03 | 2003-05-21 | 南京大学 | Extraction refining method for aloe-polysaccharide |
| CN1473822A (en) * | 2003-08-05 | 2004-02-11 | 西安翠宝首饰集团公司 | Extracting process of flavone and poly saccharide in duckweed |
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