CN104988602B - Pectin fiber and preparation method thereof - Google Patents
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- CN104988602B CN104988602B CN201510454197.0A CN201510454197A CN104988602B CN 104988602 B CN104988602 B CN 104988602B CN 201510454197 A CN201510454197 A CN 201510454197A CN 104988602 B CN104988602 B CN 104988602B
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- 239000001814 pectin Substances 0.000 title claims abstract description 91
- 229920001277 pectin Polymers 0.000 title claims abstract description 91
- 235000010987 pectin Nutrition 0.000 title claims abstract description 91
- 239000000835 fiber Substances 0.000 title claims abstract description 76
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000002121 nanofiber Substances 0.000 claims abstract description 31
- 239000007864 aqueous solution Substances 0.000 claims abstract description 24
- 239000002904 solvent Substances 0.000 claims abstract description 23
- 238000009987 spinning Methods 0.000 claims abstract description 19
- 239000011259 mixed solution Substances 0.000 claims abstract description 18
- 239000006184 cosolvent Substances 0.000 claims abstract description 14
- 239000004094 surface-active agent Substances 0.000 claims abstract description 11
- 239000002202 Polyethylene glycol Substances 0.000 claims description 43
- 229920001223 polyethylene glycol Polymers 0.000 claims description 43
- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 39
- 238000001523 electrospinning Methods 0.000 claims description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 25
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 24
- 239000000243 solution Substances 0.000 claims description 21
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 12
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 12
- 239000012046 mixed solvent Substances 0.000 claims description 10
- 230000005684 electric field Effects 0.000 claims description 8
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 7
- 230000032050 esterification Effects 0.000 claims description 7
- 238000005886 esterification reaction Methods 0.000 claims description 7
- 229920004890 Triton X-100 Polymers 0.000 claims description 5
- 239000013504 Triton X-100 Substances 0.000 claims description 5
- 235000020971 citrus fruits Nutrition 0.000 claims description 4
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims description 4
- 229920000053 polysorbate 80 Polymers 0.000 claims description 4
- 241000208340 Araliaceae Species 0.000 claims description 3
- 241000207199 Citrus Species 0.000 claims description 3
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 claims description 3
- 235000003140 Panax quinquefolius Nutrition 0.000 claims description 3
- RVGRUAULSDPKGF-UHFFFAOYSA-N Poloxamer Chemical compound C1CO1.CC1CO1 RVGRUAULSDPKGF-UHFFFAOYSA-N 0.000 claims description 3
- 235000008434 ginseng Nutrition 0.000 claims description 3
- 229960000502 poloxamer Drugs 0.000 claims description 3
- 229920001983 poloxamer Polymers 0.000 claims description 3
- ATHHXGZTWNVVOU-UHFFFAOYSA-N N-methylformamide Chemical compound CNC=O ATHHXGZTWNVVOU-UHFFFAOYSA-N 0.000 claims 2
- 230000009435 amidation Effects 0.000 claims 1
- 238000007112 amidation reaction Methods 0.000 claims 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 abstract description 15
- 238000005406 washing Methods 0.000 abstract description 9
- 238000000034 method Methods 0.000 abstract description 6
- 238000002156 mixing Methods 0.000 abstract description 5
- 150000002148 esters Chemical class 0.000 description 24
- PYMYPHUHKUWMLA-UHFFFAOYSA-N 2,3,4,5-tetrahydroxypentanal Chemical compound OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 description 17
- 229940040387 citrus pectin Drugs 0.000 description 17
- 239000009194 citrus pectin Substances 0.000 description 17
- -1 polyoxyethylene Polymers 0.000 description 10
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 241001274660 Modulus Species 0.000 description 5
- 239000003795 chemical substances by application Substances 0.000 description 5
- 238000010041 electrostatic spinning Methods 0.000 description 5
- 238000010438 heat treatment Methods 0.000 description 5
- 239000008240 homogeneous mixture Substances 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 238000009835 boiling Methods 0.000 description 3
- 229920002521 macromolecule Polymers 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000005311 nuclear magnetism Effects 0.000 description 3
- 238000010992 reflux Methods 0.000 description 3
- IAZDPXIOMUYVGZ-WFGJKAKNSA-N Dimethyl sulfoxide Chemical group [2H]C([2H])([2H])S(=O)C([2H])([2H])[2H] IAZDPXIOMUYVGZ-WFGJKAKNSA-N 0.000 description 2
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical compound C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 230000003213 activating effect Effects 0.000 description 2
- 230000004071 biological effect Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- 238000002791 soaking Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 102000010834 Extracellular Matrix Proteins Human genes 0.000 description 1
- 108010037362 Extracellular Matrix Proteins Proteins 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 238000000944 Soxhlet extraction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- 230000003110 anti-inflammatory effect Effects 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 210000000988 bone and bone Anatomy 0.000 description 1
- 210000002449 bone cell Anatomy 0.000 description 1
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- 230000004154 complement system Effects 0.000 description 1
- 206010012601 diabetes mellitus Diseases 0.000 description 1
- 125000003963 dichloro group Chemical group Cl* 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 210000002744 extracellular matrix Anatomy 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000003349 gelling agent Substances 0.000 description 1
- 239000000416 hydrocolloid Substances 0.000 description 1
- 239000000017 hydrogel Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002351 pectolytic effect Effects 0.000 description 1
- 229920002627 poly(phosphazenes) Polymers 0.000 description 1
- 229920000867 polyelectrolyte Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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- Artificial Filaments (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The invention provides a pectin fiber and a preparation method thereof, belongs to the field of macromolecular fiber, and is used for solving the problem that the PEO content in a conventional pectin and PEO mixed fiber is too high. The pectin fiber comprises the components by the mass percentage: 80%-100% of pectin, and 0-20% of polyethylene oxide. The invention also provides the preparation method of the pectin fiber. The method comprises the steps: firstly, mixing a pectin aqueous solution and a polyethylene oxide aqueous solution, then adding a surfactant and a cosolvent, to obtain a mixed solution, and spinning the mixed solution, to obtain an electrospinned nanofiber; and then dissolving the obtained electrospinned nanofiber in a selective solvent, washing, and thus obtaining the pectin fiber. The content of polyethylene oxide in the pectin fiber is lower than 20%, and the pectin fiber has excellent biocompatibility and mechanical properties.
Description
Technical field
The invention belongs to macromolecular fibre field, more particularly to a kind of pectin fiber and preparation method thereof.
Background technology
Pectin (pectin) is the polyanionic natural heteropolysaccharide that a class derives from plant, based on its good gelling
Matter, is widely used as gellant and thickening agent in food industry.Pectin have in itself multiple inherence biological activitys, including antiinflammatory,
Antitumor, adjust complement system, support bone cell growth etc., having attracted the extensive concern of people in recent years, be prepared to nanometer/
Micron particle, hydrogel, porous three-dimensional support etc., control for treatment of cancer, colonic drug delivery, bone tissue engineer, diabetes
The biomedical sectors (munarin, f.et al.int.j.biol.macromol.2012,51,681 689) such as treatment.Macromolecule
The fibre structure of natural extracellular matrix simulated by fiber, and has the features such as high porosity, hole intercommunication, in biomedical neck
The application in domain all has the advantage (liu, w.et al.adv.healthcaremater.2012,1,10 25) of uniqueness.Therefore,
Pectin fiber has broad application prospects in biomedical sector, and its preparation is also particularly significant.
Prepare in the technology of macromolecular fibre at present, the method simple, direct, with low cost that electrostatic spinning is well recognized as.
However, due to the polyelectrolyte property of pectin, pure aqueous pectin solution can not form stable jet it is impossible to straight under electric field action
Connect electrospinning and obtain pectin fiber (stijnman, a.c.et al.food hydrocolloids 2011,25,1393 1398).
By adding synthesis polyphosphazene polymer ethylene oxide (peo) of easy spinning in aqueous pectin solution, pectin is assisted together by peo
Spinning, obtain pectin and peo composite fibre (rockwell, p.l.et al.carbohyd.polym.2014,107,110
118).However, because the property of spinning solution limits, the mass fraction synthesizing macromolecule peo in fiber is up to 50%.So high
Content synthesis macromolecule be not needed in a lot of bio-medical scenes, and once be placed in physiological aqueous phase condition will
Dissolution, leads to material to lose fibre structure, mechanical performance reduce (duan, b.et al.eur.polym.j.2006,42,2013
2022).
Content of the invention
The invention aims to solving the problems, such as existing pectin and peo too high levels in the composite fibre of peo, and
A kind of pectin fiber and preparation method thereof is provided.
Present invention firstly provides a kind of pectin fiber, according to mass percent, comprising: 80%～100% pectin and 0～
20% polyethylene glycol oxide.
Preferably, the source of described pectin is Citrus, Fructus Citri Limoniae, Fructus Mali pumilae, Helianthi, Radix Betae or Radix Ginseng.
Preferably, the weight average molecular weight of described pectin is 100,000～1,500,000, and esterification degree is 20%～80%, amide
Change degree is 0～40%.
Preferably, the viscosity-average molecular weight of described polyethylene glycol oxide is 500,000～10,000,000.
The present invention also provides a kind of preparation method of pectin fiber, comprising:
Step one: aqueous pectin solution and polyethylene glycol oxide aqueous solution are subsequently adding surfactant and cosolvent,
Obtain mixed solution, mixed solution is carried out spinning, obtains electro spinning nano fiber；
Step 2: the electro spinning nano fiber that step one is obtained is dissolved in selective solvent and being washed, obtains pectin fine
Dimension.
Preferably, in described aqueous pectin solution and polyoxyethylene aqueous solution pectin and polyethylene glycol oxide mass ratio
For 70:30～96:4.
Preferably, described surfactant is Triton X-100, Tween 80, polysorbas20 or Poloxamer 127.
Preferably, described cosolvent is dimethyl sulfoxide, dimethylformamide, glycerol or propylene glycol.
Preferably, described spinning is to carry out spinning under the high voltage electric field of 5～30kv.
Preferably, described selective solvent be dichloromethane, the mixed solvent of chloroform, dichloromethane and ethanol or
Chloroform and the mixed solvent of ethanol.
Beneficial effects of the present invention
Present invention firstly provides a kind of pectin fiber, according to mass percent, comprising: 80%～100% pectin and 0～
20% polyethylene glycol oxide.Compare with prior art, in the pectin fiber of the present invention, the content of polyethylene glycol oxide is less than 20%,
Because the content of polyethylene glycol oxide is relatively low, even if dissolution, the structure of pectin nanofiber is maintained to, and mechanical performance is not yet
Impacted, the pectin fiber of the therefore present invention has excellent biocompatibility and mechanical performance.
The present invention also provides a kind of preparation method of pectin fiber, and the method uses the polyethylene glycol oxide of high molecular, lacks
The surfactant of amount and cosolvent, to adjust the property of aqueous pectin solution, ensure that when polyoxyethylene content is relatively low still
So realize the successful electrospinning of pectin nanofiber, the method using selective solvent washing can be in the structure keeping nanofiber
Do not reduce the content of polyethylene glycol oxide further under the premise of not destroying the biological activity of pectin or completely remove polyethylene glycol oxide.Should
Preparation method is simple, be easily achieved, and in the pectin fiber obtaining, the content of polyethylene glycol oxide is less than 20%.
Brief description
Electro spinning nano fiber and the nucleus magnetic hydrogen spectrum figure of high ester citrus pectin fiber that Fig. 1 obtains for the embodiment of the present invention 1；
Electro spinning nano fiber and the load-deformation curve of high ester citrus pectin fiber that Fig. 2 obtains for the embodiment of the present invention 1
Figure；
Electro spinning nano fiber and the stereoscan photograph of high ester citrus pectin fiber that Fig. 3 obtains for the embodiment of the present invention 1.
Specific embodiment
Present invention firstly provides a kind of pectin fiber, according to mass percent, comprising: 80%～100% pectin and 0～
20% polyethylene glycol oxide.
According to the present invention, the source of described pectin is not particularly limited, preferably Citrus, Fructus Citri Limoniae, Fructus Mali pumilae, Helianthi,
Radix Betae or Radix Ginseng, the weight average molecular weight of described pectin is preferably 100,000～1,500,000, and esterification degree is 20%～80%, amidatioon
Degree is 0～40%.The viscosity-average molecular weight of described polyethylene glycol oxide is preferably 500,000～10,000,000.
The present invention also provides a kind of preparation method of pectin fiber, comprising:
Step one: aqueous pectin solution and polyethylene glycol oxide aqueous solution are subsequently adding surfactant and cosolvent,
Obtain mixed solution, mixed solution is carried out spinning, obtains electro spinning nano fiber；
Step 2: the electro spinning nano fiber that step one is obtained is dissolved in selective solvent and being washed, obtains pectin fine
Dimension.
According to the present invention, first respectively pectin and polyethylene glycol oxide are made into aqueous pectin solution and polyoxyethylene aqueous solution,
The mass percent concentration of described aqueous pectin solution is preferably 2%～10%, the mass percent of polyoxyethylene aqueous solution
Concentration is preferably 2%～10%, then by aqueous pectin solution and polyethylene glycol oxide aqueous solution, described aqueous pectin solution and
In polyoxyethylene aqueous solution, the mass ratio of pectin and polyethylene glycol oxide is preferably 70:30～96:4, is subsequently adding surface activity
Agent and cosolvent, obtain mixed solution, mixed solution are preferably stirred at room temperature standing after 3～24h and remove bubble removing, then will
Mixed solution carries out spinning, described spinning preferably carrying out under the high voltage electric field of 5～30kv, more preferably voltage be 5～
20kv, is then collecting fiber, more preferably spinning head and the distance of catcher are 10～15cm at spinning head 5～20cm,
Obtain electro spinning nano fiber；
Described surfactant is preferably Triton X-100, Tween 80, polysorbas20 or Poloxamer 127, described surface
The mass percent concentration of activating agent is preferably 0.5%～3%, more preferably 0.5%～2%；Described cosolvent is preferably
Dimethyl sulfoxide, dimethylformamide, glycerol or propylene glycol, the mass percent concentration of addition is preferably 2%～10%, more
It is preferably 5%～10%.
According to the present invention, the electro spinning nano fiber obtaining is dissolved in selective solvent and is washed, remove surface activity
Agent and cosolvent, and reduce the content of polyethylene glycol oxide further or remove polyethylene glycol oxide completely, obtain pectin fiber.Described
Selective solvent be can dissolving polyoxyethylene, surfactant, cosolvent, but can not pectolytic solvent, excellent
Elect the mixed solvent of dichloromethane, chloroform, dichloromethane and ethanol or the mixed solvent of chloroform and ethanol as, described mixing
In solvent, dichloromethane is preferably 80:20～95:5 with the percent by volume of ethanol, and the percent by volume of chloroform and ethanol is preferred
For 93:7；Described washing is preferably washing by soaking or the mode of extracting washing, and the method for described washing by soaking is preferably: will
Electro spinning nano fiber is positioned in solvent and soaks, and removes old solvent at interval of 6～24h, adds fresh solvent, changes number of times
3～10 times；The method of described extracting washing is preferably: electro spinning nano fiber is placed in the sample room of cable type extractor according, will be molten
Agent is placed in the solvent bottle of cable type extractor according, and heating makes solvent boiling reflux, repeatedly rinses fiber, extracts 2～5 days.
Below the present invention is further illustrated using specific embodiment, but the present invention is not limited to this.
Embodiment 1: polyethylene glycol oxide mass fraction is the preparation of 1.5% high ester citrus pectin fiber
(1) electrostatic spinning: weighing 0.55g molecular weight first is 880,000, and esterification degree is 74% citrus pectin, with 9.45g
Redistilled water mixes, and is stirred overnight, prepared mass percent concentration is 5.5% high ester citrus pectin aqueous solution under room temperature；
Weigh the polyethylene glycol oxide that 0.5g molecular weight is 5,000,000, mix with 9.5g redistilled water, be stirred overnight under room temperature, prepared matter
Amount percent concentration is 5% polyoxyethylene aqueous solution.Mass ratio according to pectin and polyethylene glycol oxide is 95:5 by high ester
Citrus pectin aqueous solution and polyethylene glycol oxide aqueous solution, are separately added into 1% Triton X-100 and 5% in solution
Dimethyl sulfoxide, mixed solution is stirred at room temperature 5h, then stands overnight, and obtains bubble-free homogeneous mixture solotion, will be upper
State under the high voltage electric field that mixed solution is placed in 12kv, collecting fiber at spinning head 15cm, obtaining electro spinning nano fiber；
(2) dichloromethane extracting: weigh the above-mentioned electro spinning nano fiber of 10mg, be placed in the sample room of cable type extractor according, measure
150ml dichloromethane is placed in the solvent bottle of the cable type extractor according of 250ml, and heating makes solvent boiling reflux, repeatedly rinses fiber 3
My god, extracting closes heating power supply after finishing, and treats that solvent is cooled to room temperature, takes out fibre plate, obtain high ester citrus fruit after vacuum drying
Glue fiber.
Electro spinning nano fiber and the nucleus magnetic hydrogen spectrum figure of high ester citrus pectin fiber that Fig. 1 obtains for the embodiment of the present invention 1, from
Fig. 1 can be seen that the characteristic peak of polyethylene glycol oxide in 3.74ppm, and the characteristic peak of pectin, in 3.84ppm, contrasts dichloromethane and takes out
The ratio at two peaks after in advance, after being calculated extracting, the mass fraction of polyethylene glycol oxide is 1.5%.The characteristic peak of Triton X-100
It is wholly absent it was demonstrated that being completely removed after 3.63～3.69ppm, extracting.The characteristic peak of remaining dmso exists on a small quantity
2.75ppm, is wholly absent it was demonstrated that being completely removed after extracting.
The electro spinning nano fiber that obtain embodiment 1 and high ester citrus pectin fiber carry out measuring mechanical property, stress-answer
Varied curve is as shown in Fig. 2 result shows: electro spinning nano fiber Young's moduluss are 192.3mpa, through the fruit after dichloromethane extracting
Glue fiber Young's moduluss are 224.5mpa.
Electro spinning nano fiber and the stereoscan photograph of high ester citrus pectin fiber that embodiment 1 obtains as shown in figure 3, its
Middle a is electro spinning nano fiber, and b is high ester citrus pectin fiber, and Fig. 3 illustrates that washing process makes the diameter of fiber reduce, but not
Destroy the pattern of fiber.
Embodiment 2: polyethylene glycol oxide mass fraction is the preparation of 10% low ester Helianthi pectin fiber
(1) electrostatic spinning: weighing 0.6g molecular weight first is 500,000, and esterification degree is 40% Helianthi pectin, with 9.4g
Water mixes, and is stirred overnight, prepared mass percent concentration is 6% low ester Helianthi aqueous pectin solution under room temperature.Weigh 0.5g
Molecular weight is 1,000,000 polyethylene glycol oxide, mixes with 9.5g water, is stirred overnight under room temperature, and prepared mass percent concentration is 5%
Polyoxyethylene aqueous solution.Mass ratio according to pectin and polyethylene glycol oxide is that 80:20 by Helianthi aqueous pectin solution and gathers
Ethylene oxide aqueous solution, is separately added into 2% pool Luo Samu 127 and 5% dimethylformamide in solution, will mix
Close solution and 5h is stirred at room temperature, then stand overnight, obtain bubble-free homogeneous mixture solotion, above-mentioned mixed solution is placed in
Under the high voltage electric field of 8kv, collecting fiber at spinning head 15cm, obtaining electro spinning nano fiber；
(2) chloroform: weigh the above-mentioned electro spinning nano fiber of 10mg, be positioned in 30ml chloroform and soak 2 days, little every 6
The fresh chloroform of Shi Genghuan, takes out fibre plate, obtains low ester Helianthi pectin fiber after vacuum drying.
Nuclear-magnetism and Mechanical test results show, polyethylene glycol oxide in the low ester Helianthi pectin fiber that embodiment 2 obtains
Mass fraction is 10%, and without surfactant and cosolvent, Young's moduluss are 153.5mpa.
Embodiment 3: polyethylene glycol oxide mass fraction is the preparation of 0% high ester apple pectin fiber
(1) electrostatic spinning: weighing 0.4g molecular weight first is 950,000, and esterification degree is 70% apple pectin, with 9.6g bis-
Secondary distilled water mixing, is stirred overnight under room temperature, prepared mass percent concentration is 4% high ester apple pectin aqueous solution.Weigh
0.5g molecular weight is 5,000,000 polyethylene glycol oxide, mixes with 9.5g redistilled water, is stirred overnight under room temperature, prepared quality hundred
Divide the polyoxyethylene aqueous solution that specific concentration is 5%.Mass ratio according to pectin and polyethylene glycol oxide is 96:4 by high ester Fructus Mali pumilae
Aqueous pectin solution and polyethylene glycol oxide aqueous solution, are separately added into 1% Tween 80 and 5% glycerol in solution,
Mixed solution is stirred at room temperature 5h, then stands overnight, obtain bubble-free homogeneous mixture solotion, above-mentioned mixed solution is put
Under the high voltage electric field of 20kv, collecting fiber at spinning head 15cm, obtaining electro spinning nano fiber；
(2) chloroform/ethanol (93/7) MIXED SOLVENT EXTRACTION: weigh the above-mentioned electro spinning nano fiber of 10mg, be placed in soxhlet extraction
The sample room of device, measures the solvent bottle that 150ml chloroform/ethanol (93/7) mixed solvent is placed in the cable type extractor according of 250ml, heating
Make solvent boiling reflux, repeatedly rinse fiber 5 days, extracting closes heating power supply after finishing, treat that solvent is cooled to room temperature, take out fiber
Piece, obtains high ester apple pectin fiber after vacuum drying.
Nuclear-magnetism and Mechanical test results show, the high ester apple pectin fiber that embodiment 3 obtains does not contain polyethylene glycol oxide, table
Face activating agent, cosolvent, Young's moduluss are 283.6mpa.
Embodiment 4 polyethylene glycol oxide mass fraction is the preparation of 20% low ester citrus pectin fiber
(1) electrostatic spinning: weighing 0.7g molecular weight first is 300,000, and esterification degree is 30% citrus pectin, with 9.3g water
Mixing, is stirred overnight under room temperature, prepared mass percent concentration is 7% low ester citrus pectin aqueous solution.Weigh 0.5g molecule
Measure the polyethylene glycol oxide for 600,000, mix with 9.5g water, be stirred overnight under room temperature, prepared mass percent concentration be 5% poly-
Ethylene oxide aqueous solution.Mass ratio according to pectin and polyethylene glycol oxide is 70:30 by citrus pectin aqueous solution and polyoxyethylene
Aqueous solution mixes, and is separately added into 1% polysorbas20 and 5% propylene glycol, mixed solution is stirred at room temperature in solution
6h, then stand overnight, obtains bubble-free homogeneous mixture solotion, above-mentioned mixed solution is placed under the high voltage electric field of 7kv, away from
Collect fiber away from spinning head 12cm, obtain electro spinning nano fiber；
(2) dichloromethane/alcohol mixed solvent washing: weigh the above-mentioned electro spinning nano fiber of 10mg, be positioned over 30ml dichloro
Soak 2 days in methane/ethanol (90/10) mixed solvent, changed fresh dichloromethane/ethanol (90/10) mixing every 4 hours
Solvent, takes out fibre plate, obtains low ester citrus pectin fiber after vacuum drying.
Nuclear-magnetism and Mechanical test results show, the matter of polyethylene glycol oxide in the low ester citrus pectin fiber that embodiment 4 obtains
Amount fraction is 20%, and without surfactant and cosolvent, Young's moduluss are 135.7mpa.
Claims (9)
1. a kind of pectin fiber is it is characterised in that according to mass percent, comprising: 80%～100% pectin and 0～20%
Polyethylene glycol oxide；
A kind of preparation method of described pectin fiber is it is characterised in that include:
Step one: aqueous pectin solution and polyethylene glycol oxide aqueous solution are subsequently adding surfactant and cosolvent, obtain
Mixed solution, mixed solution is carried out spinning, obtains electro spinning nano fiber；
Step 2: the electro spinning nano fiber that step one is obtained is dissolved in selective solvent and being washed, and obtains pectin fiber.
2. a kind of pectin fiber according to claim 1 it is characterised in that the source of described pectin be Citrus, Fructus Citri Limoniae,
Fructus Mali pumilae, Helianthi, Radix Betae or Radix Ginseng.
3. a kind of pectin fiber according to claim 1 is it is characterised in that the weight average molecular weight of described pectin is 100,000
～150 ten thousand, esterification degree is 20%～80%, and degree of amidation is 0～40%.
4. a kind of pectin fiber according to claim 1 is it is characterised in that the viscosity-average molecular weight of described polyethylene glycol oxide
For 500,000～10,000,000.
5. a kind of pectin fiber according to claim 1 is it is characterised in that described aqueous pectin solution and polyethylene glycol oxide
In aqueous solution, the mass ratio of pectin and polyethylene glycol oxide is 70:30～96:4.
6. a kind of pectin fiber according to claim 1 it is characterised in that described surfactant be Triton X-100,
Tween 80, polysorbas20 or Poloxamer 127.
7. a kind of pectin fiber according to claim 1 it is characterised in that described cosolvent be dimethyl sulfoxide, two
Methylformamide, glycerol or propylene glycol.
8. a kind of pectin fiber according to claim 1 is it is characterised in that described spinning is the high pressure in 5～30kv
Carry out spinning under electric field.
9. a kind of pectin fiber according to claim 1 it is characterised in that described selective solvent be dichloromethane,
The mixed solvent of chloroform, dichloromethane and ethanol or the mixed solvent of chloroform and ethanol.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510454197.0A CN104988602B (en) | 2015-07-29 | 2015-07-29 | Pectin fiber and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510454197.0A CN104988602B (en) | 2015-07-29 | 2015-07-29 | Pectin fiber and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN104988602A CN104988602A (en) | 2015-10-21 |
| CN104988602B true CN104988602B (en) | 2017-02-01 |
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