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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- arabinan
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- 238000000034 method Methods 0.000 title claims abstract description 33
- 238000000746 purification Methods 0.000 title claims abstract description 27
- 238000012545 processing Methods 0.000 title claims abstract description 24
- 239000003513 alkali Substances 0.000 title claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 17
- 241000675108 Citrus tangerina Species 0.000 title 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 title 1
- 241000207199 Citrus Species 0.000 claims abstract description 24
- 235000020971 citrus fruits Nutrition 0.000 claims abstract description 24
- 239000000706 filtrate Substances 0.000 claims abstract description 21
- 239000007787 solid Substances 0.000 claims abstract description 21
- 239000004744 fabric Substances 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 9
- 230000007935 neutral effect Effects 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 5
- 239000012535 impurity Substances 0.000 claims abstract description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 34
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000001914 filtration Methods 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 9
- 239000012528 membrane Substances 0.000 claims description 9
- 238000000108 ultra-filtration Methods 0.000 claims description 9
- 239000012141 concentrate Substances 0.000 abstract description 3
- 239000006227 byproduct Substances 0.000 abstract description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 238000009924 canning Methods 0.000 abstract 2
- 238000011112 process operation Methods 0.000 abstract 1
- 150000004676 glycans Chemical class 0.000 description 28
- 229920001282 polysaccharide Polymers 0.000 description 26
- 239000005017 polysaccharide Substances 0.000 description 26
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 description 15
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 description 15
- SRBFZHDQGSBBOR-IOVATXLUSA-N D-xylopyranose Chemical compound O[C@@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-IOVATXLUSA-N 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 238000005189 flocculation Methods 0.000 description 7
- 230000016615 flocculation Effects 0.000 description 7
- 210000004706 scrotum Anatomy 0.000 description 6
- 206010040882 skin lesion Diseases 0.000 description 6
- 231100000444 skin lesion Toxicity 0.000 description 6
- 238000001816 cooling Methods 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 235000013305 food Nutrition 0.000 description 4
- 241000196324 Embryophyta Species 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000001814 pectin Substances 0.000 description 3
- 229920001277 pectin Polymers 0.000 description 3
- 235000010987 pectin Nutrition 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 2
- 238000005349 anion exchange Methods 0.000 description 2
- PYMYPHUHKUWMLA-WDCZJNDASA-N arabinose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)C=O PYMYPHUHKUWMLA-WDCZJNDASA-N 0.000 description 2
- 210000004369 blood Anatomy 0.000 description 2
- 239000008280 blood Substances 0.000 description 2
- 238000004440 column chromatography Methods 0.000 description 2
- 238000010612 desalination reaction Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000008103 glucose Substances 0.000 description 2
- NOESYZHRGYRDHS-UHFFFAOYSA-N insulin Chemical compound N1C(=O)C(NC(=O)C(CCC(N)=O)NC(=O)C(CCC(O)=O)NC(=O)C(C(C)C)NC(=O)C(NC(=O)CN)C(C)CC)CSSCC(C(NC(CO)C(=O)NC(CC(C)C)C(=O)NC(CC=2C=CC(O)=CC=2)C(=O)NC(CCC(N)=O)C(=O)NC(CC(C)C)C(=O)NC(CCC(O)=O)C(=O)NC(CC(N)=O)C(=O)NC(CC=2C=CC(O)=CC=2)C(=O)NC(CSSCC(NC(=O)C(C(C)C)NC(=O)C(CC(C)C)NC(=O)C(CC=2C=CC(O)=CC=2)NC(=O)C(CC(C)C)NC(=O)C(C)NC(=O)C(CCC(O)=O)NC(=O)C(C(C)C)NC(=O)C(CC(C)C)NC(=O)C(CC=2NC=NC=2)NC(=O)C(CO)NC(=O)CNC2=O)C(=O)NCC(=O)NC(CCC(O)=O)C(=O)NC(CCCNC(N)=N)C(=O)NCC(=O)NC(CC=3C=CC=CC=3)C(=O)NC(CC=3C=CC=CC=3)C(=O)NC(CC=3C=CC(O)=CC=3)C(=O)NC(C(C)O)C(=O)N3C(CCC3)C(=O)NC(CCCCN)C(=O)NC(C)C(O)=O)C(=O)NC(CC(N)=O)C(O)=O)=O)NC(=O)C(C(C)CC)NC(=O)C(CO)NC(=O)C(C(C)O)NC(=O)C1CSSCC2NC(=O)C(CC(C)C)NC(=O)C(NC(=O)C(CCC(N)=O)NC(=O)C(CC(N)=O)NC(=O)C(NC(=O)C(N)CC=1C=CC=CC=1)C(C)C)CC1=CN=CN1 NOESYZHRGYRDHS-UHFFFAOYSA-N 0.000 description 2
- 238000005342 ion exchange Methods 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 239000002808 molecular sieve Substances 0.000 description 2
- 150000004804 polysaccharides Polymers 0.000 description 2
- 210000000582 semen Anatomy 0.000 description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 235000013311 vegetables Nutrition 0.000 description 2
- SATHPVQTSSUFFW-UHFFFAOYSA-N 4-[6-[(3,5-dihydroxy-4-methoxyoxan-2-yl)oxymethyl]-3,5-dihydroxy-4-methoxyoxan-2-yl]oxy-2-(hydroxymethyl)-6-methyloxane-3,5-diol Chemical compound OC1C(OC)C(O)COC1OCC1C(O)C(OC)C(O)C(OC2C(C(CO)OC(C)C2O)O)O1 SATHPVQTSSUFFW-UHFFFAOYSA-N 0.000 description 1
- 229920000189 Arabinogalactan Polymers 0.000 description 1
- 239000001904 Arabinogalactan Substances 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 241000186016 Bifidobacterium bifidum Species 0.000 description 1
- 229920000742 Cotton Polymers 0.000 description 1
- AEMOLEFTQBMNLQ-YMDCURPLSA-N D-galactopyranuronic acid Chemical compound OC1O[C@H](C(O)=O)[C@H](O)[C@H](O)[C@H]1O AEMOLEFTQBMNLQ-YMDCURPLSA-N 0.000 description 1
- GUBGYTABKSRVRQ-WFVLMXAXSA-N DEAE-cellulose Chemical compound OC1C(O)C(O)C(CO)O[C@H]1O[C@@H]1C(CO)OC(O)C(O)C1O GUBGYTABKSRVRQ-WFVLMXAXSA-N 0.000 description 1
- IAJILQKETJEXLJ-UHFFFAOYSA-N Galacturonsaeure Natural products O=CC(O)C(O)C(O)C(O)C(O)=O IAJILQKETJEXLJ-UHFFFAOYSA-N 0.000 description 1
- 102000004877 Insulin Human genes 0.000 description 1
- 108090001061 Insulin Proteins 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- UGXQOOQUZRUVSS-ZZXKWVIFSA-N [5-[3,5-dihydroxy-2-(1,3,4-trihydroxy-5-oxopentan-2-yl)oxyoxan-4-yl]oxy-3,4-dihydroxyoxolan-2-yl]methyl (e)-3-(4-hydroxyphenyl)prop-2-enoate Chemical compound OC1C(OC(CO)C(O)C(O)C=O)OCC(O)C1OC1C(O)C(O)C(COC(=O)\C=C\C=2C=CC(O)=CC=2)O1 UGXQOOQUZRUVSS-ZZXKWVIFSA-N 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 239000012491 analyte Substances 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000000840 anti-viral effect Effects 0.000 description 1
- 235000019312 arabinogalactan Nutrition 0.000 description 1
- 229920000617 arabinoxylan Polymers 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 239000002775 capsule Substances 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 210000002421 cell wall Anatomy 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000007598 dipping method Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 239000003480 eluent Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000003311 flocculating effect Effects 0.000 description 1
- 239000010794 food waste Substances 0.000 description 1
- 230000005714 functional activity Effects 0.000 description 1
- 229930182830 galactose Natural products 0.000 description 1
- 210000000232 gallbladder Anatomy 0.000 description 1
- 229940125396 insulin Drugs 0.000 description 1
- 230000000968 intestinal effect Effects 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000004310 lactic acid Substances 0.000 description 1
- 235000014655 lactic acid Nutrition 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000010813 municipal solid waste Substances 0.000 description 1
- 210000000822 natural killer cell Anatomy 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 230000036961 partial effect Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 235000013324 preserved food Nutrition 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000009754 rhamnogalacturonan I Substances 0.000 description 1
- 210000000697 sensory organ Anatomy 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 229930193551 sterin Natural products 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 238000012549 training Methods 0.000 description 1
Classifications
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Molecular Biology (AREA)
- Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
本发明公开了一种柑橘罐头加工碱处理水中阿拉伯聚糖的纯化方法，该方法先将碱处理水pH调节至中性；然后将中性液体在50℃下真空浓缩至总固形物的质量分数为1.5％～1.9％；将总固形物含量合格的浓缩液的pH调节至1.0～3.5后在83～95℃下均匀加热10min以上，产生絮凝物，滤布过滤含絮凝物混合液，收集滤液；滤液经过一次超滤，去除小分子杂质，得阿拉伯聚糖浓缩液；将浓缩液喷雾干燥得阿拉伯聚糖粉末。本发明的原料来源廉价、丰富，属于柑橘罐头加工的副产品。工艺操作简单，纯化时间短，生产过程绿色环保，适合产业化应用。同时减少罐头加工中废弃物的排放，对柑橘罐头加工具有积极意义。The invention discloses a method for purifying arabinan in alkali-treated water for processing canned citrus. In the method, the pH of the alkali-treated water is first adjusted to neutral; 1.5% to 1.9%; adjust the pH of the concentrated solution with qualified total solids content to 1.0 to 3.5, and then heat evenly at 83 to 95°C for more than 10 minutes to generate flocs, filter the mixed liquid containing flocs with filter cloth, and collect the filtrate The filtrate is ultra-filtered once to remove small molecular impurities to obtain arabinan concentrate; the concentrate is spray-dried to obtain arabinan powder. The raw material source of the invention is cheap and abundant, and belongs to the by-product of canned citrus processing. The process operation is simple, the purification time is short, the production process is green and environmentally friendly, and it is suitable for industrial application. At the same time, reducing waste discharge in canning processing has positive significance for citrus canning 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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| CN111040042A (en) * | 2019-12-13 | 2020-04-21 | 浙江大学 | A kind of wolfberry polysaccharide, preparation method and application thereof |
| CN116508994A (en) * | 2023-05-06 | 2023-08-01 | 浙江大学 | A kind of probiotic RG-I pectin microcapsule and preparation method thereof |
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| 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 |
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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 |
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| 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 | A kind of probiotic RG-I pectin microcapsule and preparation method thereof |
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