CN106046195A - Purification method for treating araban in alkali treatment water for orange and tangerine tin can processing - Google Patents
Purification method for treating araban in alkali treatment water for orange and tangerine tin can processing Download PDFInfo
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- CN106046195A CN106046195A CN201610367571.8A CN201610367571A CN106046195A CN 106046195 A CN106046195 A CN 106046195A CN 201610367571 A CN201610367571 A CN 201610367571A CN 106046195 A CN106046195 A CN 106046195A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0006—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid
- C08B37/0045—Homoglycans, i.e. polysaccharides having a main chain consisting of one single sugar, e.g. colominic acid alpha-D-Galacturonans, e.g. methyl ester of (alpha-1,4)-linked D-galacturonic acid units, i.e. pectin, or hydrolysis product of methyl ester of alpha-1,4-linked D-galacturonic acid units, i.e. pectinic acid; Derivatives thereof
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Abstract
The invention discloses a purification method for treating araban in alkali treatment water for orange and tangerine tin can processing. The purification method comprises the steps that the pH of the alkali treatment water is regulated to be neutral; then, the neutral liquid is subjected to vacuum concentration at the temperature of 50 DEG C till the mass fraction of the total solids is 1.5%-1.9%; after the pH of concentrate qualified in content of the total solids is regulated to be 1.0-3.5, even heating is performed at the temperature of 83-95 DEG C for more than 10 minutes to produce floccules, floccule-containing mixed liquid is filtered through filter cloth, and filtrate is collected; the filtrate is subjected to one-time ultra-filtration to remove small molecule impurities, and araban concentrate is obtained; the concentrate is subjected to spray drying to obtain araban powder. The raw materials are cheap and rich in source, and the araban belongs to an orange and tangerine tin can processing by-product. The purification method is simple in process operation and short in purification time and is suitable for industrial application, and the production process is green and environmentally friendly. In addition, waste discharge during orange and tangerine tin can processing s reduced, and the purification method has the positive significance on the orange and tangerine tin can processing.
Description
Technical field
The invention belongs to Polyose extraction purification art, particularly relate to a kind of Citrus can processing alkali process in water purification I
The method of primary polysaccharide.
Technical background
Arabinan is widely present in plant tissue, including the position such as seed, fruit, is the composition of plant cell wall
One of composition.Here arabinan refers to a class polysaccharide, except finding, in the insides such as Semen Brassicae campestris, the Ah that sugar composition is more single
Drawing outside primary polysaccharide, arabinose (Ara) can also be formed containing a large amount of Arabic combined with xylose (Xyl), galactose (Gal) etc.
The araboxylan (arabinoxylan, AX) of sugar and arabinogalactan (arabinogaIactan, AG) etc. are functional
Polysaccharide, is widely present in the corn such as Semen Tritici aestivi and the vegetable such as Radix Raphani, Rhizoma Solani tuber osi, and additionally arabinan is the most often classified as pectin
A kind of component of class material, structurally, it is predominantly due to the RGI region (rhamnogalacturonan I) of pectin.Therefore
The purification of target of arabinan is the arabinan chain (being not necessarily made up of completely) stayed based on Ara Ara, to obtain
Obtain the functional activity components such as highly purified AX, AG or RGI.
Arabinan has a lot of physiologically active, and it is a kind of natural plant edible fiber, can significantly reduce gallbladder
Sterin and blood lipid level, improve intestinal microecology, increases lactic acid bacteria and the quantity of bacillus bifidus, it is proposed that adult daily intakes 30
～about 40g；Additionally also play an important role in terms of blood glucose regulation, glucose and insulin level can be regulated and controled；At antiviral
Antiinflammatory aspect also has outstanding contributions, can be activated NK cell etc. played a role by regulation immunocompetence；It addition, it is Arabic poly-
Sugar is also recognized further in terms of active anticancer and is paid attention to.
Except the most concerned physiologically active, arabinan can also serve as thickening agent etc. in food production, has
Water-retaining property, can significantly improve the sense organ of food, especially be widely used in bakery, is that a kind of wholesome food adds
Agent.
Therefore the market demand of following arabinan will grow at top speed, and the new source excavating arabinan is also many
Many benefits are kind.And need to develop the arabinan of higher degree, the efficient performance of the above function could be ensured, in economy
Upper just have more preferable commodity value.
Citrus skin lesion of the scrotum clothing operation in Citrus can processing, need to be with dipping by lye Fructus Citri tangerinae lobe with thoroughly removing capsule clothing, Fructus Citri tangerinae lobe
Middle part vegetable polysaccharides is just dissolved in alkali liquor.It has been investigated that the polysaccharide in alkali liquor is in addition to containing galacturonic acid, also have
More arabinose, therefore it is in addition to utilizing as pectin polysaccharide, is also the good source purifying arabinan, and has
May be in purification process, it is achieved the classified utilization of polysaccharide and make resource efficiency maximize.
At present the method for purification of crude polysaccharide is mainly column chromatography, it is common to use include ion exchange column method, molecular sieve
Method etc..Ion exchange can be divided into anion exchange and cation exchange, to the crude polysaccharides containing acid polysaccharide moiety conventional cloudy from
Sub-exchange process carries out isolated and purified, and such as DEAE-52 cellulose column, its end N, with a positive charge, belongs to weakly-basic anion
Exchange；Also commonly use now strong anion and exchange quick post, Q sephrose fast flow as quaternized in end.Sieve method
Also being the one of column chromatography, the filler simply used often is accompanied with the effect of molecular sieve, can be according to the size of molecular weight analyte
Crude polysaccharides is carried out grading purification.Isolated and purified (the Qin of arabinan in Fructus Lycii is carried out if any using DEAE-cellulose column
Xiao Ming, Lin Huajuan. the purification & isolation of Fructus Lycii arabinan and structural feature research [J] thereof. Food Science, 2003,24
(2): 52-56.), but its purification is intended merely to the information such as analytical structure is used, and its target is not as last using purification sugar
Products application.Because being below no matter quick post or conventional post, it is directed to clean filler, dress post, balance etc. a series of loaded down with trivial details
Time-consuming pre-treatment, and also applied sample amount is little, and low grade of yield in unit time limits, and is not suitable for large-scale production.Additionally I
The purification of primary polysaccharide also has use ethanol or ammonium sulfate graded precipitation, but needs additionally to use precipitant, and step is cumbersome, becomes
This is bigger.
Summary of the invention
Present invention aims to the deficiencies in the prior art, it is provided that a kind of Citrus can processing alkali process in water Ah
Drawing the purification process of primary polysaccharide, the method uses equipment few, separates sample size big, and whole separation process is the biggest compared with traditional method
Big shortening, easy and simple to handle, can be used for factory and separate on a large scale.Simultaneously as the by-product of Citrus can processing, decrease canned food
Waste discharge in processing, too increases the added value of Citrus procession.
It is an object of the invention to be achieved through the following technical solutions: a kind of Citrus can processing alkali processes in water Arabic
The purification process of polysaccharide, the method comprises the following steps:
(1) take in Citrus can processing alkali process water, with HCl solution regulation pH to neutral；
(2) mass fraction that neutral liquid is concentrated in vacuo at 50 DEG C total solid is 1.5%～1.9%；
(3) concentrated solution qualified for above-mentioned total solids content is pumped in acid resistant heater, and use 3mol/L hydrochloric acid solution
Adjust pH to 1.0～3.5；
(4) at 83～95 DEG C, uniformly heat more than 10min, produce flocculate, filter-cloth filtering mixed liquor Han flocculate, receive
Collection filtrate；
(5) filtrate is through a ultrafiltration, removes small molecular weight impurity, obtains arabinan concentrated solution；
(6) above-mentioned concentrated solution is spray-dried to obtain arabinan powder.
Further, the mass fraction being concentrated in vacuo to solid content described in is 1.7～1.8%.
Further, in described step (3), concentrated solution pH regulator to 2.5.
Further, in described step (4), heating-up temperature is 92 DEG C；Heat time heating time 15min.It is then used by 350 mesh filter clothes
Filter and collect filtrate.
Further, in described step (5), ultrafilter membrane uses molecular cut off to be 5kDa.
Further, in described step (6), be spray-dried and use inlet temperature 170～180 DEG C, sample introduction speed 600～
900ml/h.Suction power 100%.
Advantages of the present invention is as follows:
(1) raw material sources are cheap, belong to the garbage recycling in Citrus can processing, increase Citrus Industry added value,
Also promote the greenization of Citrus procession, greatly reduce the waste of resource and the discharge of harmful substance.
(2) purifying process is simple, and equipment requirements is low, and unit processing ease realizes industrialization, worker training's low cost.
(3) purification time is short, and efficiency is high, and isolated and purified compared to traditional column packing, this technique does not exist the sample of loading
Quality restricted problem.
(4) purge process green safety, does not use poisonous and harmful reagent, is not required to use eluent etc. yet, alleviates follow-up product
The desalination burden of product.
Detailed description of the invention
The present invention a kind of Citrus can processing alkali processes the method for purification of arabinan in water, comprises the steps:
(1) take in Citrus can processing alkali process water, with HCl solution regulation pH to neutral；
(2) mass fraction that neutral liquid is concentrated in vacuo at 50 DEG C total solid is 1.5%～1.9%；Total solid
The mass fraction of shape thing is unsuitable excessive or too small, and too small flocculation can not effectively form thus affect purification effect, excessive, wads a quilt with cotton
Condensate filter efficiency is low, easily blocks up filter cloth.Cryogenic vacuum concentrates the shadow reducing heat to polysaccharide chain form of can trying one's best in concentration process
Ring so that it is add at subsequent high temperature and hanker having performance of preferably flocculating.Be concentrated in vacuo to the mass fraction of solid content be preferably 1.7～
1.8%.
(3) concentrated solution qualified for above-mentioned total solids content is pumped in acid resistant heater, and use 3mol/L hydrochloric acid solution
Adjust pH to 1.0～3.5；At this ph, acutely heating can promote the flocculation in solution between par-tial polysaccharide, precipitates with flocculate
Form removes, thus purified polysaccharide.Concentrated solution pH is preferably 2.5.
(4) at 83～95 DEG C, uniformly heat more than 10min, produce flocculate, filter-cloth filtering mixed liquor Han flocculate, receive
Collection filtrate；Heating flocculation needs higher heating-up temperature, and temperature is too low can not occur flocculation at short notice.The too high then wave of temperature
Take energy, also improve the requirement to equipment.Heating-up temperature is preferably 92 DEG C；Heat time heating time is preferably 15min.It is then used by
350 mesh filter-cloth filterings also collect filtrate.
(5) filtrate is through a ultrafiltration, removes small molecular weight impurity, obtains arabinan concentrated solution；Ultrafilter membrane uses and retains
Molecular weight is preferably 5kDa.The filtrate removing flocculate is the limpidest, is easier to filter, and available small-bore ultrafiltration mwco membrane enters
Row desalination, the process of de-small-molecule substance.
(6) above-mentioned concentrated solution is spray-dried to obtain arabinan powder；It is spray-dried and uses inlet temperature 170～180
DEG C, sample introduction speed 600～900ml/h.Suction power 100%.
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1
The concentrated solution of the different pH of the present embodiment carries out heating flocculation, to optimize the purification effect of arabinan, specifically
Step is as follows:
The alkali taking Citrus can processing skin lesion of the scrotum clothing operation processes water, and (HCl solution is dense to use HCl solution regulation pH to 5～7
Degree non-quantitative, uses bigger concentration can improve the efficiency adjusting pH, and big concentration HCl needs big stir speed (S.S.)).Re-use vacuum concentrator
At 50 DEG C, carry out concentrating under reduced pressure, and on-line checking total solids content (mass fraction), be concentrated into total solid mass fraction
Stop when being 1.7～1.8% concentrating, concentrated solution be pumped into acid resistant heater, use 3mol/L hydrochloric acid solution to adjust pH to 1,
1.5,2.5,3.5,4.At 92 DEG C, uniformly heat 15min, produce flocculate, somewhat use 350 mesh filter-cloth filterings after cooling, receive
Collection filtrate, filtrate is again through a ultrafiltration, and ultrafilter membrane molecular cut off is 5kDa, the macromolecular polysaccharide concentrated solution warp again under retaining
Crossing spray drying, obtain arabinan powder, drying parameter is inlet temperature 180 DEG C, charging rate 800ml/h, merit of bleeding
Rate 100%.Measure the sugar composition of dried polysaccharide, in mole percent.Result see table:
According to the total proportion (i.e. the purity of arabinan) shared by Ara+Xyl+Gal, preferably pH is 2.5.
Embodiment 2
The present embodiment uses different heating temperature, to optimize the purification effect of arabinan, specifically comprises the following steps that
The alkali taking Citrus can processing skin lesion of the scrotum clothing operation processes water, and (HCl solution is dense to use HCl solution regulation pH to 5～7
Degree non-quantitative, uses bigger concentration can improve the efficiency adjusting pH, and big concentration HCl needs big stir speed (S.S.)).Re-use vacuum concentrator
At 50 DEG C, carry out concentrating under reduced pressure, and on-line checking total solids content (mass fraction), be concentrated into total solid mass fraction
Stop when being 1.6～1.7% concentrating, concentrated solution is pumped into acid resistant heater, use 3mol/L hydrochloric acid solution to adjust pH to 2.5.
Respectively 80, at 83,88,92,95 DEG C, uniformly heat 15min, produce flocculate, somewhat use 350 mesh filter-cloth filterings after cooling,
Collecting filtrate, filtrate is again through a ultrafiltration, and ultrafilter membrane molecular cut off is 5kDa, and the macromolecular polysaccharide concentrated solution under retaining is again
Through being spray-dried, obtaining arabinan powder, drying parameter is inlet temperature 180 DEG C, and charging rate 900ml/h is bled
Power 100%.Measure the sugar composition of dried polysaccharide, in mole percent.Result see table:
According to the total proportion (i.e. the purity of arabinan) shared by Ara+Xyl+Gal, and energy economy using priciple,
Preferably flocculation heating-up temperature is 92 DEG C.
Embodiment 3
The present embodiment uses the different heating time, to optimize the purification effect of arabinan, specifically comprises the following steps that
The alkali taking Citrus can processing skin lesion of the scrotum clothing operation processes water, and (HCl solution is dense to use HCl solution regulation pH to 5～7
Degree non-quantitative, uses bigger concentration can improve the efficiency adjusting pH, and big concentration HCl needs big stir speed (S.S.)).Re-use vacuum concentrator
At 50 DEG C, carry out concentrating under reduced pressure, and on-line checking total solids content (mass fraction), be concentrated into total solid mass fraction
Stop when being 1.5～1.6% concentrating, concentrated solution is pumped into acid resistant heater, use 3mol/L hydrochloric acid solution to adjust pH to 2.5.
At 92 DEG C, the most uniformly heat 8min, 10min, 12min, 15min, 20min, produce flocculate, somewhat after cooling, use 350
Mesh filter-cloth filtering, collects filtrate, and filtrate is again through a ultrafiltration, and ultrafilter membrane molecular cut off is 5kDa, the macromole under retaining
Polysaccharide concentrated solution through being spray-dried, obtains arabinan powder again, and drying parameter is inlet temperature 170 DEG C, charging rate
600ml/h, suction power 100%.Measure the sugar composition of dried polysaccharide, in mole percent.Result see table:
According to the total proportion (i.e. the purity of arabinan) shared by Ara+Xyl+Gal, and energy economy using priciple,
Preferably flocculation heat time heating time be 15min.
Embodiment 4
The alkali taking Citrus can processing skin lesion of the scrotum clothing operation processes water, and (HCl solution is dense to use HCl solution regulation pH to 5～7
Degree non-quantitative, uses bigger concentration can improve the efficiency adjusting pH, and big concentration HCl needs big stir speed (S.S.)).Re-use vacuum concentrator
At 50 DEG C, carry out concentrating under reduced pressure, and on-line checking total solids content (mass fraction), be concentrated into total solid mass fraction
Stop when being 1.7～1.8% concentrating, concentrated solution is pumped into acid resistant heater, use 3mol/L hydrochloric acid solution to adjust pH to 2.5.
Uniformly heating 15min at 92 DEG C, produce flocculate, somewhat use 300 mesh filter-cloth filterings after cooling, collect filtrate, filtrate is again
Through a ultrafiltration, ultrafilter membrane molecular cut off is 10kDa, and the macromolecular polysaccharide concentrated solution under retaining passes through and is spray-dried,
Obtaining arabinan powder, drying parameter is inlet temperature 160 DEG C, charging rate 500ml/h, suction power 90%.Measure
The sugar composition of dried polysaccharide, in mole percent, the content of result display Ara+Xyl+Gal is 85%.
Embodiment 5
The alkali taking Citrus can processing skin lesion of the scrotum clothing operation processes water, and (HCl solution is dense to use HCl solution regulation pH to 5～7
Degree non-quantitative, uses bigger concentration can improve the efficiency adjusting pH, and big concentration HCl needs big stir speed (S.S.)).Re-use vacuum concentrator
At 50 DEG C, carry out concentrating under reduced pressure, and on-line checking total solids content (mass fraction), be concentrated into total solid mass fraction
Stop when being 1.8～1.9% concentrating, concentrated solution is pumped into acid resistant heater, use 3mol/L hydrochloric acid solution to adjust pH to 2.5.
Uniformly heating 15min at 92 DEG C, produce flocculate, somewhat use 400 mesh filter-cloth filterings after cooling, collect filtrate, filtrate is again
Through a ultrafiltration, ultrafilter membrane molecular cut off is 5kDa, and the macromolecular polysaccharide concentrated solution under retaining is again through being spray-dried, i.e.
Obtaining arabinan powder, drying parameter is inlet temperature 175 DEG C, charging rate 700ml/h, suction power 100%.Measure dry
The sugar composition of dry rear polysaccharide, in mole percent, the content of result display Ara+Xyl+Gal is 91%.
Claims (6)
1. the purification process of arabinan during a Citrus can processing alkali processes water, it is characterised in that the method include with
Lower step:
(1) take in Citrus can processing alkali process water, with HCl solution regulation pH to neutral；
(2) mass fraction that neutral liquid is concentrated in vacuo at 50 DEG C total solid is 1.5%～1.9%；
(3) concentrated solution qualified for above-mentioned total solids content is pumped in acid resistant heater, and adjust pH with 3mol/L hydrochloric acid solution
To 1.0～3.5；
(4) uniformly heating more than 10min, generation flocculate, filter-cloth filtering mixed liquor Han flocculate, collection filter at 83～95 DEG C
Liquid；
(5) filtrate is through a ultrafiltration, removes small molecular weight impurity, obtains arabinan concentrated solution；
(6) above-mentioned concentrated solution is spray-dried to obtain arabinan powder.
Purification process the most according to claim 1, it is characterised in that described in be concentrated in vacuo to the mass fraction of solid content and be
1.7～1.8%.
Purification process the most according to claim 1, it is characterised in that in described step (3), concentrated solution pH regulator to 2.5.
Purification process the most according to claim 1, it is characterised in that in described step (4), heating-up temperature is 92 DEG C；Add
Heat time 15min.It is then used by 350 mesh filter-cloth filterings and collects filtrate.
Purification process the most according to claim 1, it is characterised in that in described step (5), ultrafilter membrane uses and retains molecule
Amount is 5kDa.
Purification process the most according to claim 1, it is characterised in that in described step (6), is spray-dried and uses air intake temperature
Spend 170～180 DEG C, sample introduction speed 600～900ml/h.Suction power 100%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111040042A (en) * | 2019-12-13 | 2020-04-21 | 浙江大学 | Wolfberry polysaccharide, preparation method and application thereof |
| CN116508994A (en) * | 2023-05-06 | 2023-08-01 | 浙江大学 | Probiotics RG-I pectin microcapsule and preparation method thereof |
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| EA016871B1 (en) * | 2009-05-05 | 2012-08-30 | Зайниддин Камарович Мухидинов | Method for processing sun flower into pectin |
| CN102731681A (en) * | 2011-04-15 | 2012-10-17 | 吕维学 | Method for extracting pectin from orange peel and shaddock peel |
| CN103468761A (en) * | 2013-09-25 | 2013-12-25 | 重庆工商大学 | Method for preparing L-arabinose by using rape cake |
| CN104211835A (en) * | 2014-09-22 | 2014-12-17 | 山西大学 | Method for extracting araboxylan from astragalus medicine residues by using ionic liquid |
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| EA016871B1 (en) * | 2009-05-05 | 2012-08-30 | Зайниддин Камарович Мухидинов | Method for processing sun flower into pectin |
| CN102731681A (en) * | 2011-04-15 | 2012-10-17 | 吕维学 | Method for extracting pectin from orange peel and shaddock peel |
| CN102643883A (en) * | 2012-04-20 | 2012-08-22 | 上海应用技术学院 | Preparation method of low-ester pectin |
| CN103468761A (en) * | 2013-09-25 | 2013-12-25 | 重庆工商大学 | Method for preparing L-arabinose by using rape cake |
| CN104211835A (en) * | 2014-09-22 | 2014-12-17 | 山西大学 | Method for extracting araboxylan from astragalus medicine residues by using ionic liquid |
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| CN111040042A (en) * | 2019-12-13 | 2020-04-21 | 浙江大学 | Wolfberry polysaccharide, preparation method and application thereof |
| CN111040042B (en) * | 2019-12-13 | 2021-11-23 | 浙江大学 | Wolfberry polysaccharide, preparation method and application thereof |
| CN116508994A (en) * | 2023-05-06 | 2023-08-01 | 浙江大学 | Probiotics RG-I pectin microcapsule and preparation method thereof |
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