CN106799167A - The method that a kind of double films of ultrafiltration/nanofiltration efficiently purify pumpkin oligosaccharide - Google Patents
The method that a kind of double films of ultrafiltration/nanofiltration efficiently purify pumpkin oligosaccharide Download PDFInfo
- Publication number
- CN106799167A CN106799167A CN201710018754.3A CN201710018754A CN106799167A CN 106799167 A CN106799167 A CN 106799167A CN 201710018754 A CN201710018754 A CN 201710018754A CN 106799167 A CN106799167 A CN 106799167A
- Authority
- CN
- China
- Prior art keywords
- ultrafiltration
- nanofiltration
- pumpkin
- oligosaccharide
- membrane
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/58—Multistep processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
- B01D61/027—Nanofiltration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/145—Ultrafiltration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
- B01D65/02—Membrane cleaning or sterilisation ; Membrane regeneration
- B01D65/06—Membrane cleaning or sterilisation ; Membrane regeneration with special washing compositions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2311/00—Details relating to membrane separation process operations and control
- B01D2311/26—Further operations combined with membrane separation processes
- B01D2311/2649—Filtration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2321/00—Details relating to membrane cleaning, regeneration, sterilization or to the prevention of fouling
- B01D2321/16—Use of chemical agents
- B01D2321/164—Use of bases
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Water Supply & Treatment (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Nanotechnology (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention discloses the method that a kind of double films of ultrafiltration/nanofiltration efficiently purify pumpkin oligosaccharide.Be applied in pumpkin oligosaccharide production technology for ultrafiltration, nanofiltration by the method, reaches the purpose of efficiently purification pumpkin oligosaccharide.The macromoleculars such as milipore filter retention albumen, polysaccharide, NF membrane is through small molecules such as inorganic salts, monose and plays inspissation.The present invention realizes the separation of pumpkin oligosaccharide, refined and concentration using ultrafiltration and nanofiltration, and production technology is compact, easy to operate, treatment conditions are gentle, preparation efficiency is high, energy consumption is low and oligosaccharide good separating effect.The double membrane technologies of ultrafiltration nanofiltration are preferable pumpkin oligosaccharide methods of purification, efficiently remove big molecular impurity and small molecular weight impurity, improve the concentration and quality of the oligomeric sugar product of pumpkin.
Description
Technical field
The present invention relates to a kind of extracting method of pumpkin oligosaccharide, the double films of more particularly to a kind of ultrafiltration/nanofiltration are efficient
The method for purifying pumpkin oligosaccharide.
Background technology
Oligosaccharide (oligosaccharide) can be described as oligosaccharides again, be connected into directly by glycosidic bond by 2-10 monose
The low polymerization sugar of chain or side chain, molecular weight is between 200-300D.Because monosaccharide molecule binding site is different with bond type,
Form the abundant oligosaccharide of species.Oligosaccharide has good functional characteristic, can be originated as sweet taste, but not by human body hydrochloric acid in gastric juice,
Gastric enzyme is degraded, not in intestinal absorption, into large intestine after selectively promote the propagation of beneficial bacterium and suppress pathogen and diarrhoea, also
The functions such as protection liver, reduce serum cholesterol, anti-caries tooth.Oligosaccharide receives much concern because of its unique functional characteristic, and future exists
There are good researching value and application potential in the fields such as functional food, feed and additive.
Pumpkin (Cucurbita moschata) is Curcurbitaceae herbaceous plant, and in China, various regions plantation is extensive, is a kind of suitable
Together in the popular vegetables of diabetic population.China and in the world many countries all once using pumpkin as a kind of effectively prevention and
Treat the food of diabetes, numerous studies have demonstrated that the functional sugar composition such as polysaccharide, oligosaccharide in pumpkin have it is significant
Effect of lowering blood sugar.And used as a kind of composition of natural botanical source, the security of pumpkin oligosaccharide is also widely approved.
Membrane separation technique, mainly including counter-infiltration, nanofiltration, micro-filtration, ultrafiltration and membrane technology etc. electrodialysis, is to use band micropore
, the film being made up of macromolecular material, it is big according to mixed system molecular weight under certain temperature, pressure and environmental condition
The small technology that different materials is efficiently separated, purified and concentrated, its technique integration degree is high and easily operated, in work
Large-scale production is capable of achieving in industry.Ultrafiltration membrane aperture is gathered in 10-100nm mainly for separating of protein, nucleic acid in liquid phase substance
The macromolecular compounds such as compound, starch.The separating mechanism of ultra-filtration process is commonly considered as pressure-actuated sieve aperture separation process, but
The chemical substance on film surface is also the key factor that influence is separate.Ultra-filtration process is the mechanical retention (sieve on film surface
Point), the stop (obstruction) in fenestra, the three kinds of forms of absorption in film surface and fenestra.Compared to microfiltration membranes, its fenestra compared with
Small, filtering accuracy is higher, practical operation pressure is slightly higher.Nanofiltration membrane aperture in 1-10nm, be it is a kind of between counter-infiltration and ultrafiltration it
Between pressure-driven membrane separating process, be mainly used between 200-500D organic matter removing.The separating mechanism model of NF membrane
Current view has:Steric hindrance-duct model, solution-diffusion, spatial diffusion model, space-charge model, fixed electricity
Lotus model.Compared with milipore filter, NF membrane has certain charged capacity；Compared with anti-seepage membrane, NF membrane is not again substantially non-porous
, therefore its separating mechanism there is also difference while there is general character.Currently with the double membrane technologies of ultrafiltration/nanofiltration to pumpkin
Oligosaccharide carries out purification, and there is not yet reported.
The content of the invention
It is an object of the invention to provide the method that a kind of double films of ultrafiltration/nanofiltration efficiently purify pumpkin oligosaccharide, south is improved
The concentration and quality of the oligomeric sugar product of melon.
The method that a kind of double films of ultrafiltration/nanofiltration efficiently purify pumpkin oligosaccharide, is carried out in accordance with the following steps：
(1) pumpkin oligosaccharide crude extract is diluted 3-6 times, and crosses 15-30 μm of filter bag, final feed liquid electrical conductivity reaches
4000-4500ppm, 15-25 DEG C of feed temperature；
(2) ultrafiltration is carried out, ultrafiltration section working frequency is 26-28Hz, inlet hydraulic is 0.5-0.7MPa, 20-25 DEG C of temperature,
It is 15-19L/h through flow velocity；
(3) when feed liquid stoste is when being concentrated into the 1/4-1/2 of material liquid volume after ultrafiltration, 1 times of dilution is added water, instead
Multiple ultrafiltration 2-8 times；
(4) nanofiltration is carried out, nanofiltration section working frequency is 36-39Hz, and inlet hydraulic is 1.5-1.8MPa, permeate initial flow
Speed is 15-18L/h, and feed liquid is constantly concentrated, and nanofiltration final stage flow velocity constantly declines, and is finally down to 3-5L/h, cycles of concentration
It is 3-5 times, feed temperature is constantly raised in nanofiltration process, is eventually raised to 30-35 DEG C；
(5) Membrane cleaning operation is carried out after the completion of operation every time, using the alkaline cleaning fluid of pH value 9-10, heating 40-50 takes the photograph
Family name's degree wash cycles 20-45 minutes, clean 2-4 times, to membrane flux recovery rate>95%.
The preparation method of the pumpkin oligosaccharide crude extract is：By pumpkin remove seed stripping and slicing, plus the 2-5 times of water mashing of weight,
Digested using pectase, amylase or Pullulanase, centrifuging and taking supernatant is concentrated into the 1/2-1/5 of former supernatant volume, added
The 2-5 times of ethanol precipitation of volume 80%, centrifuging and taking supernatant.
The equipment of ultrafiltration and nanofiltration that carries out is the multi-functional wound membrane element testing machine of 1812/2319 type.
The ultrafiltration membrane material is PES, and membrane aperture is 0.01 μm, and molecular cut off is 3000D.
The nanofiltration membrane material is PAN, and membrane aperture is 1-2nm, and molecular cut off is 200-300D.
The ultrafiltration membrane material, the membrane structure of nanofiltration membrane material are rolled film.
The aperture of the ultrafiltration membrane material is 0.01 μm；The aperture of the nanofiltration membrane material is 1-2nm.
Compared with prior art, the present invention has the advantages that：Ultrafiltration, nanofiltration are applied to pumpkin by the present invention
In oligosaccharide production technology, the purpose of efficiently purification pumpkin oligosaccharide is reached.The macromoleculars such as milipore filter retention albumen, polysaccharide, receive
Filter membrane is through small molecules such as inorganic salts, monose and plays certain inspissation.The present invention is realized using ultrafiltration and nanofiltration
It is the separation of pumpkin oligosaccharide, refined and concentrate, production technology is compact, easy to operate, treatment conditions are gentle, preparation efficiency is high,
Energy consumption is low and oligosaccharide good separating effect.The double membrane technologies of ultrafiltration nanofiltration are preferable pumpkin oligosaccharide methods of purification, are efficiently gone
Except big molecular impurity and small molecular weight impurity, the concentration and quality of the oligomeric sugar product of pumpkin are improved.
Brief description of the drawings
Fig. 1 is pumpkin oligosaccharide liquid chromatographic detection figure prepared by the present invention.
Specific embodiment
Below in conjunction with the accompanying drawings, specific embodiment of the invention is described in detail, it is to be understood that guarantor of the invention
Shield scope is not limited by specific embodiment.
Embodiment 1
The method that a kind of double films of ultrafiltration/nanofiltration efficiently purify pumpkin oligosaccharide, is carried out in accordance with the following steps：
(1) by pumpkin remove seed stripping and slicing, plus 3 times of water mashing of weight, using pectinase enzymatic hydrolysis, centrifuging and taking supernatant, concentration
To the 1/3 of former supernatant volume, 3 times of ethanol precipitations of volume 80% are added, centrifuging and taking supernatant obtains pumpkin oligosaccharide and slightly carries
Liquid；
(2) pumpkin oligosaccharide crude extract is crossed into 20 μm of filter bags and is diluted to electrical conductivity 4411ppm, 21 DEG C of feed temperature；
(3) ultrafiltration is carried out, ultrafiltration section working frequency is 26.7Hz, and inlet hydraulic is 0.6MPa, is 16L/ through flow velocity
h；
(4) when feed liquid stoste is when being concentrated into the 1/3 of material liquid volume after ultrafiltration, 1 times of dilution, ultrafiltration 5 are added water
It is secondary；
(5) nanofiltration is carried out, nanofiltration section working frequency is 36Hz, and inlet hydraulic is 1.5MPa, and permeate initial flow rate is
15L/h, because feed liquid is constantly concentrated, nanofiltration final stage flow velocity constantly declines, and is finally down to 4L/h, feed liquid in nanofiltration process
Temperature is constantly raised, and is eventually raised to 30.7 DEG C；
(5) Membrane cleaning operation is carried out after the completion of operation every time, using the alkaline cleaning fluid of pH value 9.5, heats 45 degrees Celsius
Wash cycles 30 minutes, clean 3 times, to membrane flux recovery rate>95%.
Device therefor is the multi-functional wound membrane element testing machine of 1812/2319 type in embodiment；Ultrafiltration membrane material is poly- for PES
Ether sulfone resin (PES), membrane aperture is 0.01 μm, and molecular cut off is 3000D；Nanofiltration membrane material used is polyacrylonitrile (PAN),
Membrane aperture is 1-2nm, and molecular cut off is 200-300D；Milipore filter, NF membrane membrane structure are rolled film.
Pumpkin oligosaccharide liquid chromatographic detection manufactured in the present embodiment as shown in Figure 1, molecular weight detection result show by
Molecular weight distribution concentrates on 300-3000D after membrane filtration, reaches the Expected Results of ultrafiltration and nanofiltration.Pumpkin oligosaccharide purity is
94%, concentration is 150mg/ml, and the membrane filtration rate of recovery is 92%.
Embodiment 2
The method that a kind of double films of ultrafiltration/nanofiltration efficiently purify pumpkin oligosaccharide, is carried out in accordance with the following steps：
(1) by pumpkin remove seed stripping and slicing, plus 2 times of water mashing of weight, using amylase enzymolysis, centrifuging and taking supernatant, concentration
To the 1/2 of former supernatant volume, 2 times of ethanol precipitations of volume 80% are added, centrifuging and taking supernatant obtains pumpkin oligosaccharide and slightly carries
Liquid；
(2) pumpkin oligosaccharide crude extract is crossed into 20 μm of filter bags and is diluted to electrical conductivity 4233ppm, 23 DEG C of feed temperature；
(3) ultrafiltration section working frequency is 27.1Hz, and inlet hydraulic is 0.6MPa, is 16L/h through flow velocity；
(4) when feed liquid stoste is when being concentrated into be concentrated into material liquid volume 1/4 after ultrafiltration, 1 times of dilution is added water,
Ultrafiltration 4 times；
(5) nanofiltration is carried out, nanofiltration section working frequency is 38.7Hz, and inlet hydraulic is 1.6MPa, and permeate initial flow rate is
17L/h, because feed liquid is constantly concentrated, nanofiltration final stage flow velocity constantly declines, and is finally down to 3L/h.Feed liquid in nanofiltration process
Temperature is constantly raised, and is eventually raised to 31.1 DEG C；
(6) Membrane cleaning operation is carried out after the completion of operation every time, using the alkaline cleaning fluid of pH value 9,40 degrees Celsius of heating is followed
Ring is cleaned 20 minutes, is cleaned 4 times, to membrane flux recovery rate>95%.
Device therefor is the multi-functional wound membrane element testing machine of 1812/2319 type in scheme；Ultrafiltration membrane material is PES polyethers
Sulphone resin (PES), membrane aperture is 0.01 μm, and molecular cut off is 3000D；Nanofiltration membrane material used is polyacrylonitrile (PAN), film
Aperture is 1-2nm, and molecular cut off is 200-300D；Milipore filter, NF membrane membrane structure are rolled film.
Pumpkin oligosaccharide purity manufactured in the present embodiment is 93%, and concentration is 150mg/ml, and the membrane filtration rate of recovery is 91%.
Embodiment 3
The method that a kind of double films of ultrafiltration/nanofiltration efficiently purify pumpkin oligosaccharide, is carried out in accordance with the following steps：
(1) by pumpkin remove seed stripping and slicing, plus 5 times of water mashing of weight, being digested using Pullulanase, centrifuging and taking supernatant is dense
The 1/5 of former supernatant volume is reduced to, is added, 4 times of ethanol precipitations of volume 80%, centrifuging and taking supernatant obtains pumpkin oligosaccharide thick
Extract
(2) pumpkin oligosaccharide crude extract is crossed into 20 μm of filter bags and is diluted to electrical conductivity 4052ppm, 19 DEG C of feed temperature；
(3) ultrafiltration section working frequency is 27.6Hz, and inlet hydraulic is 0.7MPa, is 18L/h through flow velocity；
(4) when feed liquid stoste is when being concentrated into be concentrated into material liquid volume 1/2 after ultrafiltration, 1 times of dilution is added water,
Ultrafiltration is multiple repeatedly；
(4) nanofiltration is carried out, nanofiltration section working frequency is 38.7Hz, and inlet hydraulic is 1.8MPa, and permeate initial flow rate is
18L/h, because feed liquid is constantly concentrated, nanofiltration final stage flow velocity constantly declines, and is finally down to 3L/h.Feed liquid in nanofiltration process
Temperature is constantly raised, and is eventually raised to 33 DEG C；
(5) Membrane cleaning operation is carried out after the completion of operation every time, using the alkaline cleaning fluid of pH value 10,50 degrees Celsius of heating is followed
Ring is cleaned 45 minutes, is cleaned 2 times, to membrane flux recovery rate>95%.
Device therefor is the multi-functional wound membrane element testing machine of 1812/2319 type in scheme；Ultrafiltration membrane material is PES polyethers
Sulphone resin (PES), membrane aperture is 0.01 μm, and molecular cut off is 3000D；Nanofiltration membrane material used is polyacrylonitrile (PAN), film
Aperture is 1-2nm, and molecular cut off is 200-300D；Milipore filter, NF membrane membrane structure are rolled film.
Pumpkin oligosaccharide purity manufactured in the present embodiment is 94%, and concentration is 150mg/ml, and the membrane filtration rate of recovery is 92%.
Embodiment 4
The method that a kind of double films of ultrafiltration/nanofiltration efficiently purify pumpkin oligosaccharide, is carried out in accordance with the following steps：
(1) by pumpkin remove seed stripping and slicing, 0.01 times of nano-attapulgite of parts by weight is added, then add the water of 3 times of weight to beat
Slurry, using pectinase enzymatic hydrolysis, centrifuging and taking supernatant is concentrated into the 1/3 of former supernatant volume, adds 3 times of ethanol of volume 80% to sink
Form sediment, centrifuging and taking supernatant obtains pumpkin oligosaccharide crude extract；
(2) pumpkin oligosaccharide crude extract is crossed into 20 μm of filter bags and is diluted to electrical conductivity 4411ppm, 21 DEG C of feed temperature；
(3) ultrafiltration is carried out, ultrafiltration section working frequency is 26.7Hz, and inlet hydraulic is 0.6MPa, is 16L/ through flow velocity
h；
(4) when feed liquid stoste is when being concentrated into the 1/3 of material liquid volume after ultrafiltration, 1 times of dilution, ultrafiltration 5 are added water
It is secondary；
(5) nanofiltration is carried out, nanofiltration section working frequency is 36Hz, and inlet hydraulic is 1.5MPa, and permeate initial flow rate is
15L/h, because feed liquid is constantly concentrated, nanofiltration final stage flow velocity constantly declines, and is finally down to 4L/h, feed liquid in nanofiltration process
Temperature is constantly raised, and is eventually raised to 30.7 DEG C；
(5) Membrane cleaning operation is carried out after the completion of operation every time, using the alkaline cleaning fluid of pH value 9.5, heats 45 degrees Celsius
Wash cycles 30 minutes, clean 3 times, to membrane flux recovery rate>95%.
Device therefor is the multi-functional wound membrane element testing machine of 1812/2319 type in embodiment；Ultrafiltration membrane material is poly- for PES
Ether sulfone resin (PES), membrane aperture is 0.01 μm, and molecular cut off is 3000D；Nanofiltration membrane material used is polyacrylonitrile (PAN),
Membrane aperture is 1-2nm, and molecular cut off is 200-300D；Milipore filter, NF membrane membrane structure are rolled film.
Pumpkin oligosaccharide purity manufactured in the present embodiment is 98%, and concentration is 150mg/ml, and the membrane filtration rate of recovery is 96%.
Knowable to above-mentioned data, nano-attapulgite is added to improve the pumpkin oligosaccharide purity and the rate of recovery of preparation.
Embodiment 5
The method that a kind of double films of ultrafiltration/nanofiltration efficiently purify pumpkin oligosaccharide, is carried out in accordance with the following steps：
(1) by pumpkin remove seed stripping and slicing, plus 2 times of water mashing of weight, using amylase and papain enzymolysis, centrifuging and taking
Supernatant, is concentrated into the 1/2 of former supernatant volume, adds 2 times of ethanol precipitations of volume 80%, and centrifuging and taking supernatant obtains pumpkin
Oligosaccharide crude extract；
(2) pumpkin oligosaccharide crude extract is crossed into 20 μm of filter bags and is diluted to electrical conductivity 4233ppm, 23 DEG C of feed temperature；
(3) ultrafiltration section working frequency is 27.1Hz, and inlet hydraulic is 0.6MPa, is 16L/h through flow velocity；
(4) when feed liquid stoste is when being concentrated into be concentrated into material liquid volume 1/4 after ultrafiltration, 1 times of dilution is added water,
Ultrafiltration 4 times；
(5) nanofiltration is carried out, nanofiltration section working frequency is 38.7Hz, and inlet hydraulic is 1.6MPa, and permeate initial flow rate is
17L/h, because feed liquid is constantly concentrated, nanofiltration final stage flow velocity constantly declines, and is finally down to 3L/h.Feed liquid in nanofiltration process
Temperature is constantly raised, and is eventually raised to 31.1 DEG C；
(6) Membrane cleaning operation is carried out after the completion of operation every time, using the alkaline cleaning fluid of pH value 9,40 degrees Celsius of heating is followed
Ring is cleaned 20 minutes, is cleaned 4 times, to membrane flux recovery rate>95%.
Device therefor is the multi-functional wound membrane element testing machine of 1812/2319 type in scheme；Ultrafiltration membrane material is PES polyethers
Sulphone resin (PES), membrane aperture is 0.01 μm, and molecular cut off is 3000D；Nanofiltration membrane material used is polyacrylonitrile (PAN), film
Aperture is 1-2nm, and molecular cut off is 200-300D；Milipore filter, NF membrane membrane structure are rolled film.
Pumpkin oligosaccharide purity manufactured in the present embodiment is 96%, and concentration is 150mg/ml, and the membrane filtration rate of recovery is 95%.
Knowable to above-mentioned data, amylase and papain enzymolysis are added to improve the pumpkin oligosaccharide purity and the rate of recovery of preparation,
Than individually adding the effect of amylase good.
Embodiment 6
The method that a kind of double films of ultrafiltration/nanofiltration efficiently purify pumpkin oligosaccharide, is carried out in accordance with the following steps：
(1) by pumpkin remove seed stripping and slicing, the black moss of wart of 0.2 times of weight is added, then adds 5 times of water mashing of weight, using general Shandong
Blue enzyme enzymolysis, centrifuging and taking supernatant is concentrated into the 1/5 of former supernatant volume, adds, 4 times of ethanol precipitations of volume 80%, centrifuging and taking
Supernatant, obtains pumpkin oligosaccharide crude extract
(2) pumpkin oligosaccharide crude extract is crossed into 20 μm of filter bags and is diluted to electrical conductivity 4052ppm, 19 DEG C of feed temperature；
(3) ultrafiltration section working frequency is 27.6Hz, and inlet hydraulic is 0.7MPa, is 18L/h through flow velocity；
(4) when feed liquid stoste is when being concentrated into be concentrated into material liquid volume 1/2 after ultrafiltration, 1 times of dilution is added water,
Ultrafiltration is multiple repeatedly；
(4) nanofiltration is carried out, nanofiltration section working frequency is 38.7Hz, and inlet hydraulic is 1.8MPa, and permeate initial flow rate is
18L/h, because feed liquid is constantly concentrated, nanofiltration final stage flow velocity constantly declines, and is finally down to 3L/h.Feed liquid in nanofiltration process
Temperature is constantly raised, and is eventually raised to 33 DEG C；
(5) Membrane cleaning operation is carried out after the completion of operation every time, using the alkaline cleaning fluid of pH value 10,50 degrees Celsius of heating is followed
Ring is cleaned 45 minutes, is cleaned 2 times, to membrane flux recovery rate>95%.
Device therefor is the multi-functional wound membrane element testing machine of 1812/2319 type in scheme；Ultrafiltration membrane material is PES polyethers
Sulphone resin (PES), membrane aperture is 0.01 μm, and molecular cut off is 3000D；Nanofiltration membrane material used is polyacrylonitrile (PAN), film
Aperture is 1-2nm, and molecular cut off is 200-300D；Milipore filter, NF membrane membrane structure are rolled film.
Pumpkin oligosaccharide purity manufactured in the present embodiment is 98%, and concentration is 150mg/ml, and the membrane filtration rate of recovery is 95%.
Knowable to above-mentioned data, the black moss of wart is added to improve the pumpkin oligosaccharide purity and the rate of recovery of preparation.
Disclosed above is only specific embodiment of the invention, but, the present invention is not limited to this, any this area
What technical staff can think change should all fall into protection scope of the present invention.
Claims (7)
1. the method that a kind of double films of ultrafiltration/nanofiltration efficiently purify pumpkin oligosaccharide, it is characterised in that carry out in accordance with the following steps：
(1) pumpkin oligosaccharide crude extract is diluted 3-6 times, and crosses 15-30 μm of filter bag, final feed liquid electrical conductivity reaches 4000-
4500ppm, 15-25 DEG C of feed temperature；
(2) ultrafiltration is carried out, ultrafiltration section working frequency is 26-28Hz, and inlet hydraulic is 0.5-0.7MPa, and 20-25 DEG C of temperature is passed through
Flow velocity is 15-19L/h；
(3) when feed liquid stoste is when being concentrated into the 1/4-1/2 of material liquid volume after ultrafiltration, 1 times of dilution is added water, is surpassed repeatedly
Filter 2-8 times；
(4) nanofiltration is carried out, nanofiltration section working frequency is 36-39Hz, and inlet hydraulic is 1.5-1.8MPa, and permeate initial flow rate is
15-18L/h, feed liquid is constantly concentrated, and nanofiltration final stage flow velocity constantly declines, and is finally down to 3-5L/h, and cycles of concentration is 3-5
Times, feed temperature is constantly raised in nanofiltration process, is eventually raised to 30-35 DEG C；
(5) Membrane cleaning operation is carried out after the completion of operation every time, using the alkaline cleaning fluid of pH value 9-10, heats 40-50 degrees Celsius
Wash cycles 20-45 minutes, clean 2-4 times, to membrane flux recovery rate>95%.
2. the method that the double films of ultrafiltration/nanofiltration according to claim 1 efficiently purify pumpkin oligosaccharide, it is characterised in that institute
The preparation method for stating pumpkin oligosaccharide crude extract is：By pumpkin remove seed stripping and slicing, plus the 2-5 times of water mashing of weight, using pectase,
Amylase or Pullulanase are digested, and centrifuging and taking supernatant is concentrated into the 1/2-1/5 of former supernatant volume, adds 2-5 times of volume
80% ethanol precipitation, centrifuging and taking supernatant.
3. the method that the double films of ultrafiltration/nanofiltration according to claim 1 efficiently purify pumpkin oligosaccharide, it is characterised in that institute
State carry out ultrafiltration and nanofiltration equipment be the multi-functional wound membrane element testing machine of 1812/2319 type.
4. the method that the double films of ultrafiltration/nanofiltration according to claim 1 efficiently purify pumpkin oligosaccharide, it is characterised in that institute
Ultrafiltration membrane material is stated for PES, membrane aperture is 0.01 μm, and molecular cut off is 3000D.
5. the method that the double films of ultrafiltration/nanofiltration according to claim 1 efficiently purify pumpkin oligosaccharide, it is characterised in that institute
Nanofiltration membrane material is stated for PAN, membrane aperture is 1-2nm, and molecular cut off is 200-300D.
6. the method that the double films of ultrafiltration/nanofiltration according to claim 1 efficiently purify pumpkin oligosaccharide, it is characterised in that institute
State ultrafiltration membrane material, the membrane structure of nanofiltration membrane material and be rolled film.
7. the method that the double films of ultrafiltration/nanofiltration according to claim 6 efficiently purify pumpkin oligosaccharide, it is characterised in that institute
The aperture for stating ultrafiltration membrane material is 0.01 μm；The aperture of the nanofiltration membrane material is 1-2nm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710018754.3A CN106799167A (en) | 2017-01-11 | 2017-01-11 | The method that a kind of double films of ultrafiltration/nanofiltration efficiently purify pumpkin oligosaccharide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710018754.3A CN106799167A (en) | 2017-01-11 | 2017-01-11 | The method that a kind of double films of ultrafiltration/nanofiltration efficiently purify pumpkin oligosaccharide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106799167A true CN106799167A (en) | 2017-06-06 |
Family
ID=58985498
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710018754.3A Pending CN106799167A (en) | 2017-01-11 | 2017-01-11 | The method that a kind of double films of ultrafiltration/nanofiltration efficiently purify pumpkin oligosaccharide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106799167A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108640953A (en) * | 2018-04-27 | 2018-10-12 | 中国农业大学 | Using macroreticular resin to the process for purification of pumpkin oligosaccharide |
| CN109275829A (en) * | 2018-07-20 | 2019-01-29 | 浙江工业大学 | A kind of fruit juice functional component enrichment method based on ultrafiltration nanofiltration coupling technique |
| CN109645297A (en) * | 2019-01-02 | 2019-04-19 | 旬阳县太极缘生物科技有限公司 | The minimizing technology of mono-and di-saccharides in a kind of honey raisin tree fruit juice |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1070195A (en) * | 1992-09-04 | 1993-03-24 | 中国人民武装警察部队河北省总队医院 | A kind of method of from soyflour, extracting oligose |
| CN1259519A (en) * | 1998-12-12 | 2000-07-12 | 中国科学院新疆化学研究所 | Purification method of oligosaccharide |
| CN1302809A (en) * | 2000-01-05 | 2001-07-11 | 中国科学院大连化学物理研究所 | Process for preparing chitoligose by coupling enzyme degradation of chitosan with membrane separation |
| CN101074269A (en) * | 2006-05-18 | 2007-11-21 | 徐华民 | Process for separating and extracting cucurbic active polysaccharide |
| CN101555507A (en) * | 2009-05-18 | 2009-10-14 | 苏理 | Method for using pulullan to prepare high-purity maltotriose |
| CN102702274A (en) * | 2012-06-12 | 2012-10-03 | 华东理工大学 | Method for preparing high-purity soybean oligosaccharide from soybean whey wastewater |
| CN104042714A (en) * | 2014-07-02 | 2014-09-17 | 河南中医学院 | Preparation method of peach kernel protein, polysaccharide and oligosaccharide |
| CN105166320A (en) * | 2015-08-07 | 2015-12-23 | 青岛大学 | Preparation method of peanut protein oligosaccharide |
| CN105440087A (en) * | 2015-12-08 | 2016-03-30 | 李尚锋 | Extraction method for oligose in soybean deep processing process |
| WO2016086947A1 (en) * | 2014-12-05 | 2016-06-09 | Glycom A/S | Crystalline difucosyllactose |
-
2017
- 2017-01-11 CN CN201710018754.3A patent/CN106799167A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1070195A (en) * | 1992-09-04 | 1993-03-24 | 中国人民武装警察部队河北省总队医院 | A kind of method of from soyflour, extracting oligose |
| CN1259519A (en) * | 1998-12-12 | 2000-07-12 | 中国科学院新疆化学研究所 | Purification method of oligosaccharide |
| CN1302809A (en) * | 2000-01-05 | 2001-07-11 | 中国科学院大连化学物理研究所 | Process for preparing chitoligose by coupling enzyme degradation of chitosan with membrane separation |
| CN101074269A (en) * | 2006-05-18 | 2007-11-21 | 徐华民 | Process for separating and extracting cucurbic active polysaccharide |
| CN101555507A (en) * | 2009-05-18 | 2009-10-14 | 苏理 | Method for using pulullan to prepare high-purity maltotriose |
| CN102702274A (en) * | 2012-06-12 | 2012-10-03 | 华东理工大学 | Method for preparing high-purity soybean oligosaccharide from soybean whey wastewater |
| CN104042714A (en) * | 2014-07-02 | 2014-09-17 | 河南中医学院 | Preparation method of peach kernel protein, polysaccharide and oligosaccharide |
| WO2016086947A1 (en) * | 2014-12-05 | 2016-06-09 | Glycom A/S | Crystalline difucosyllactose |
| CN105166320A (en) * | 2015-08-07 | 2015-12-23 | 青岛大学 | Preparation method of peanut protein oligosaccharide |
| CN105440087A (en) * | 2015-12-08 | 2016-03-30 | 李尚锋 | Extraction method for oligose in soybean deep processing process |
Non-Patent Citations (3)
| Title |
|---|
| 孙俊良: "《食品生物技术》", 31 October 2011, 郑州大学出版社 * |
| 崔立勋主编: "《生物药物分离与纯化技术》", 31 January 2015, 中国标准出版社 * |
| 田维亮主编: "《化学工程与工艺专业实验》", 28 February 2015, 华东理工大学出版社 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108640953A (en) * | 2018-04-27 | 2018-10-12 | 中国农业大学 | Using macroreticular resin to the process for purification of pumpkin oligosaccharide |
| CN108640953B (en) * | 2018-04-27 | 2020-12-15 | 中国农业大学 | Refining method of pumpkin oligosaccharide by adopting macroporous resin |
| CN109275829A (en) * | 2018-07-20 | 2019-01-29 | 浙江工业大学 | A kind of fruit juice functional component enrichment method based on ultrafiltration nanofiltration coupling technique |
| CN109645297A (en) * | 2019-01-02 | 2019-04-19 | 旬阳县太极缘生物科技有限公司 | The minimizing technology of mono-and di-saccharides in a kind of honey raisin tree fruit juice |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106008645B (en) | A kind of method that momordica grosvenori glycoside V is extracted from Momordica grosvenori | |
| CN101455398B (en) | Soya-dregs water soluble diet fiber preparation method using nano filtration and spray-drying method | |
| CN100491404C (en) | Fractional extraction method of aloe polysaccharide | |
| CN104031158B (en) | A kind of technique extracting polysaccharide sulfate from Thallus Laminariae (Thallus Eckloniae) | |
| CN103478838B (en) | Honeysuckle kudzuvine root beverage and preparation method thereof | |
| CN101849656B (en) | Method for producing purple sweet potato clarified juice | |
| CN106799167A (en) | The method that a kind of double films of ultrafiltration/nanofiltration efficiently purify pumpkin oligosaccharide | |
| CN111718410A (en) | Method for preparing yolk immunoglobulin | |
| CN106008211A (en) | Method for extraction of cynarin from cynara scolymus by membrane integration technology | |
| CN108299547A (en) | A method of preparing glycoprotein from Sclerotium of Pleurotus tuber regium | |
| CN1128151C (en) | Method for extracting soy bean oligosaccharide from soy bean whey water | |
| CN103130664A (en) | Process method of extracting gamma-aminobutyric acid through membrane separation technique | |
| CN102603478A (en) | Method for separating and purifying erythritol from mother liquid obtained after repeated crystallization of erythritol | |
| CN102784193A (en) | Method for preparing hedysarum polybotrys extract by adopting coupling technology | |
| RU2354140C1 (en) | Method of processing plant raw materials to produce pectin and food products containing pectin and line for this implementation | |
| CN106674369A (en) | Preparation method of lentinan | |
| CN110256597A (en) | A kind of method that embrane method reduces heavy-metal residual in ganoderma lucidum polysaccharide | |
| CN105294873A (en) | Extraction method for laminarin | |
| CN106318995B (en) | A method of levulan and gluconic acid are prepared using inulin | |
| CN102372788A (en) | Mactra veneriformis glycosaminoglycan extraction method | |
| CN113481259B (en) | Method for extracting starch syrup and rice protein isolate by using broken rice | |
| CN101962635A (en) | Three-step two aqueous phase extraction method of ginger protease | |
| CN210560185U (en) | Device for purifying and recovering protein peptide by membrane method | |
| CN101416693B (en) | Method for extracting natural watermelon syrup from watermelon | |
| CN104876986B (en) | A kind of method of anthocyanin in extraction purple sweetpotato |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170606 |