CN104225669A - Bioactive bacterial cellulose-zein composite film and preparation method thereof - Google Patents
Bioactive bacterial cellulose-zein composite film and preparation method thereof Download PDFInfo
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- 229920002494 Zein Polymers 0.000 title claims abstract description 57
- 239000005019 zein Substances 0.000 title claims abstract description 57
- 229940093612 zein Drugs 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 56
- 230000000975 bioactive effect Effects 0.000 title claims abstract description 30
- 239000002131 composite material Substances 0.000 title claims abstract description 27
- 230000001580 bacterial effect Effects 0.000 title claims abstract description 14
- 229920002749 Bacterial cellulose Polymers 0.000 claims abstract description 74
- 239000005016 bacterial cellulose Substances 0.000 claims abstract description 74
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 62
- 239000002121 nanofiber Substances 0.000 claims abstract description 47
- 239000012153 distilled water Substances 0.000 claims abstract description 37
- 239000000463 material Substances 0.000 claims abstract description 37
- 239000000243 solution Substances 0.000 claims abstract description 31
- 238000003756 stirring Methods 0.000 claims abstract description 27
- 239000012528 membrane Substances 0.000 claims abstract description 26
- 239000002105 nanoparticle Substances 0.000 claims abstract description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 22
- 230000000844 anti-bacterial effect Effects 0.000 claims abstract description 21
- 238000000746 purification Methods 0.000 claims abstract description 19
- 238000001035 drying Methods 0.000 claims abstract description 18
- 238000003828 vacuum filtration Methods 0.000 claims abstract description 16
- 238000010008 shearing Methods 0.000 claims abstract description 10
- 239000000126 substance Substances 0.000 claims abstract description 10
- 102000011632 Caseins Human genes 0.000 claims abstract description 9
- 108010076119 Caseins Proteins 0.000 claims abstract description 9
- 239000006185 dispersion Substances 0.000 claims abstract description 9
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229940080237 sodium caseinate Drugs 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 8
- 239000002245 particle Substances 0.000 claims abstract 4
- 239000011259 mixed solution Substances 0.000 claims abstract 3
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract 3
- 229920002678 cellulose Polymers 0.000 claims description 45
- 239000001913 cellulose Substances 0.000 claims description 45
- 238000005516 engineering process Methods 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 15
- 235000002837 Acetobacter xylinum Nutrition 0.000 claims description 13
- ULGZDMOVFRHVEP-RWJQBGPGSA-N Erythromycin Chemical compound O([C@@H]1[C@@H](C)C(=O)O[C@@H]([C@@]([C@H](O)[C@@H](C)C(=O)[C@H](C)C[C@@](C)(O)[C@H](O[C@H]2[C@@H]([C@H](C[C@@H](C)O2)N(C)C)O)[C@H]1C)(C)O)CC)[C@H]1C[C@@](C)(OC)[C@@H](O)[C@H](C)O1 ULGZDMOVFRHVEP-RWJQBGPGSA-N 0.000 claims description 10
- 238000011218 seed culture Methods 0.000 claims description 10
- 230000008859 change Effects 0.000 claims description 9
- 238000000855 fermentation Methods 0.000 claims description 9
- 230000004151 fermentation Effects 0.000 claims description 9
- 230000001476 alcoholic effect Effects 0.000 claims description 8
- 230000007935 neutral effect Effects 0.000 claims description 7
- 239000003963 antioxidant agent Substances 0.000 claims description 6
- 230000003078 antioxidant effect Effects 0.000 claims description 6
- MGSRCZKZVOBKFT-UHFFFAOYSA-N thymol Chemical compound CC(C)C1=CC=C(C)C=C1O MGSRCZKZVOBKFT-UHFFFAOYSA-N 0.000 claims description 6
- 235000006708 antioxidants Nutrition 0.000 claims description 5
- 229960003276 erythromycin Drugs 0.000 claims description 5
- 239000011173 biocomposite Substances 0.000 claims description 4
- 238000000265 homogenisation Methods 0.000 claims description 4
- 239000005844 Thymol Substances 0.000 claims description 3
- 239000013543 active substance Substances 0.000 claims description 3
- 229960000790 thymol Drugs 0.000 claims description 3
- QNVSXXGDAPORNA-UHFFFAOYSA-N Resveratrol Natural products OC1=CC=CC(C=CC=2C=C(O)C(O)=CC=2)=C1 QNVSXXGDAPORNA-UHFFFAOYSA-N 0.000 claims description 2
- LUKBXSAWLPMMSZ-OWOJBTEDSA-N Trans-resveratrol Chemical compound C1=CC(O)=CC=C1\C=C\C1=CC(O)=CC(O)=C1 LUKBXSAWLPMMSZ-OWOJBTEDSA-N 0.000 claims description 2
- 230000004913 activation Effects 0.000 claims description 2
- 238000009835 boiling Methods 0.000 claims description 2
- 239000000835 fiber Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 235000021283 resveratrol Nutrition 0.000 claims description 2
- 229940016667 resveratrol Drugs 0.000 claims description 2
- 241001136169 Komagataeibacter xylinus Species 0.000 claims 3
- 235000015097 nutrients Nutrition 0.000 claims 2
- 239000012670 alkaline solution Substances 0.000 claims 1
- 229940088623 biologically active substance Drugs 0.000 claims 1
- 239000011148 porous material Substances 0.000 claims 1
- 238000009849 vacuum degassing Methods 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 15
- 230000004071 biological effect Effects 0.000 abstract description 13
- 230000003064 anti-oxidating effect Effects 0.000 abstract description 6
- 240000008042 Zea mays Species 0.000 abstract 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 abstract 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 abstract 1
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 235000005822 corn Nutrition 0.000 abstract 1
- 108060006613 prolamin Proteins 0.000 abstract 1
- 241000894006 Bacteria Species 0.000 description 41
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 18
- 239000007864 aqueous solution Substances 0.000 description 15
- 238000011081 inoculation Methods 0.000 description 15
- 108090000623 proteins and genes Proteins 0.000 description 15
- 102000004169 proteins and genes Human genes 0.000 description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 244000235858 Acetobacter xylinum Species 0.000 description 10
- 239000008187 granular material Substances 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 9
- 239000012531 culture fluid Substances 0.000 description 9
- 238000007731 hot pressing Methods 0.000 description 7
- 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 6
- 239000001888 Peptone Substances 0.000 description 6
- 108010080698 Peptones Proteins 0.000 description 6
- 239000012296 anti-solvent Substances 0.000 description 6
- 229940041514 candida albicans extract Drugs 0.000 description 6
- 239000001963 growth medium Substances 0.000 description 6
- 235000019319 peptone Nutrition 0.000 description 6
- 229910052708 sodium Inorganic materials 0.000 description 6
- 239000011734 sodium Substances 0.000 description 6
- 239000012138 yeast extract Substances 0.000 description 6
- 238000013461 design Methods 0.000 description 5
- 239000012533 medium component Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000002525 ultrasonication Methods 0.000 description 5
- 230000003115 biocidal effect Effects 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 4
- 229910021641 deionized water Inorganic materials 0.000 description 4
- 238000003760 magnetic stirring Methods 0.000 description 4
- 235000013305 food Nutrition 0.000 description 3
- 230000005764 inhibitory process Effects 0.000 description 3
- 230000003385 bacteriostatic effect Effects 0.000 description 2
- 239000012876 carrier material Substances 0.000 description 2
- 239000000306 component Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000007970 homogeneous dispersion Substances 0.000 description 2
- 230000002209 hydrophobic effect Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 239000012567 medical material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 210000000582 semen Anatomy 0.000 description 2
- 238000004088 simulation Methods 0.000 description 2
- 101710091977 Hydrophobin Proteins 0.000 description 1
- 241000589516 Pseudomonas Species 0.000 description 1
- 241000191967 Staphylococcus aureus Species 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 239000004599 antimicrobial Substances 0.000 description 1
- 230000000680 avirulence Effects 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011176 biofiber Substances 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003519 biomedical and dental material Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000013270 controlled release Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000001815 facial effect Effects 0.000 description 1
- 239000005003 food packaging material Substances 0.000 description 1
- 238000001802 infusion Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 150000008442 polyphenolic compounds Chemical class 0.000 description 1
- 235000013824 polyphenols Nutrition 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 229960003600 silver sulfadiazine Drugs 0.000 description 1
- UEJSSZHHYBHCEL-UHFFFAOYSA-N silver(1+) sulfadiazinate Chemical compound [Ag+].C1=CC(N)=CC=C1S(=O)(=O)[N-]C1=NC=CC=N1 UEJSSZHHYBHCEL-UHFFFAOYSA-N 0.000 description 1
- 238000000935 solvent evaporation Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W90/00—Enabling technologies or technologies with a potential or indirect contribution to greenhouse gas [GHG] emissions mitigation
- Y02W90/10—Bio-packaging, e.g. packing containers made from renewable resources or bio-plastics
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- Agricultural Chemicals And Associated Chemicals (AREA)
- Medicinal Preparation (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
Abstract
本发明公开了生物活性细菌纤维素-玉米醇溶蛋白复合膜及其制备方法。该方法先进行细菌纤维素膜的制备与纯化；纯化后的细菌纤维素膜放入蒸馏水中搅拌均匀，用高速剪切机剪切，经过高压微射流均质，得纳米纤维分散液；将玉米醇溶蛋白和水难溶性生物活性物质溶解在乙醇-水溶液中，得醇溶液；将酪蛋白酸钠溶解在水中，搅拌下加入所述醇溶液中，得混合液；除去乙醇，离心，得到富含有生物活性分子的玉米醇溶蛋白纳米颗粒；纳米纤维分散液与富含有生物活性的玉米醇溶蛋白颗粒混合，搅拌均匀，并进行超声处理；真空抽滤，快速成膜；干燥。本发明的复合膜材料具有良好的机械性能、生物相容性、可生物降解性，且该膜具备可调控的抗菌、抗氧化等生物活性。
The invention discloses a bioactive bacterial cellulose-zein composite film and a preparation method thereof. The method first carries out the preparation and purification of the bacterial cellulose membrane; the purified bacterial cellulose membrane is put into distilled water and stirred evenly, sheared with a high-speed shearing machine, and homogenized by high-pressure micro-jet to obtain a nanofiber dispersion; the corn Dissolve prolamin and poorly water-soluble bioactive substances in ethanol-water solution to obtain alcohol solution; dissolve sodium caseinate in water, add to the alcohol solution under stirring to obtain a mixed solution; remove ethanol and centrifuge to obtain rich Zein nanoparticles containing bioactive molecules; nanofiber dispersion liquid mixed with bioactive zein particles, stirred evenly, and subjected to ultrasonic treatment; vacuum filtration, rapid film formation; drying. The composite membrane material of the invention has good mechanical properties, biocompatibility and biodegradability, and the membrane has adjustable biological activities such as antibacterial and antioxidation.
Description
Technical field
The present invention relates to the preparation method of a kind of high strength bioactive Bacterial cellulose-Compound Film of Zein material, raw material all adopt food stage and can be degradable biomaterial, belong to the association area such as the bio-medical materials such as wound dressing, food industry technology.
Background technology
Bacterial cellulose (Bacterial Cellulose, BC) is fermented by Pseudomonas such as acetobacter xylinums and produces, and the nanofibre polymer without side chain be made up of β-Isosorbide-5-Nitrae glycosidic bond, just more and more receives the concern of people.Compared with traditional cellulose, Bacterial cellulose has many advantages, as purity is high, there is high mechanical properties, high retentiveness, good biocompatibility, breathable moisture permeability, biodegradable, avirulence, to liquid, there is the characteristics such as very strong absorbability, be therefore widely used in the fields such as bio-medical material, food, papermaking, cosmetics (Biofibre facial mask, eye mask).But owing to limitting by self property, the practical ranges of single BC material is often narrower, limits it and further applies.
In order to give bacteria cellulose material with functions such as specific antibacterial antioxidation, mostly prior art is to adopt direct infusion method Bacterial cellulose to be placed in some bioactive substance solution, rear lyophilizing, or topple over after solution blending, the methods such as oven dry prepare composite film material, these class methods length consuming time, is unfavorable for suitability for industrialized production.And most of bioactive substance, as Polyphenols antimicrobial and antioxidant agent, silver sulfadiazine etc., often there is the problems such as poor solubility, stability is not enough, therefore the antibacterial antioxidation class material actual utility prepared of the method is little.
Summary of the invention
In order to solve above-mentioned the deficiencies in the prior art part, the object of the present invention is to provide the preparation method of a kind of high strength bioactive Bacterial cellulose-Compound Film of Zein material, the method overcome prior art and prepare the defects such as bacterial cellulose composite membrane material material length consuming time, actual utility be low.
Zein (zein) is the main protein in Semen Maydis, water insoluble, dissolve in the alcoholic solution of 60% ~ 95%, this albumen is as natural degradable material, itself has strong-hydrophobicity and does not need to be cross-linked, can not in water violent released load thing, self assembly can be there is during solvent evaporation and formed there is the nano-particle of different shape, therefore, the first-selection of bag carrier material is become.But Bacterial cellulose hydrophilic is extremely strong, how realizes the homogeneous dispersibility of Hydrophilic Nanofibrous in hydrophobic proteins, become key of the present invention.
First the present invention utilizes anti-solvent technology to prepare can the water solublity zein granule of load active factors (natural antibacterial agent/antioxidant), carries out homogeneous compound with the Bacterial cellulose nanofiber through high pressure microjet homogeneous preparation; And adopt the mode of the industrial copy paper of simulation to prepare high strength bacteria cellulose-base active bio composite film material fast first.The present invention adopts nanorize embedding techniques (i.e. the preparation of anti-solvent technology can the granule of load active factors), select suitable bag carrier material, the embedding of these active substances is wherein formed reactive nanoparticles, reach and strengthen its dissolubility and stability, and reaching the object extending the useful effect cycle (controlled release), rear simulation industry papermaking technology prepares composite film material fast.Obtained composite film material has the antibacterial antioxidative biological activity of specificity, the feature such as high strength, environmental protection on the one hand; On the other hand, this film preparation mode Lv color Jie Neng ﹑ rapidly and efficiently, for large-scale industrial production high strength bioactive bacteria cellulose-base composite film material provides New Century Planned Textbook and technical foundation.
The present invention to achieve these goals, adopts following technical scheme:
The preparation method of biological activity Bacterial cellulose-Compound Film of Zein material, comprises the following steps:
1) preparation of bacteria cellulose film: utilize acetobacter xylinum strain inoculation to prepare bacteria cellulose film in seed culture fluid;
2) purification of bacteria cellulose film
Be soaked in aqueous slkali after bacteria cellulose film clear water is rinsed, boil; Bacteria cellulose film is soaked in distilled water and boils, change water; Repeat to boil 2-5 time for twice; Then by bacteria cellulose film, it is soaked in distilled water, until neutral;
3) preparation of nanofiber dispersion liquid
By step 2) in bacteria cellulose film after the purification that obtains put into distilled water and stir, shear with high-speed shearing machine, then through high pressure microjet homogenizing, obtain nanofiber dispersion liquid;
4) preparation of the zein nano-particle of bioactive molecule is rich in
Zein and slightly water-soluble bioactive substance are dissolved in ethanol-water solution, obtain alcoholic solution; Sodium caseinate is dissolved in water, adds in described alcoholic solution under stirring, obtain mixed liquor; After stirring, remove ethanol by Rotary Evaporators, centrifugal, obtain the zein nano-particle being rich in bioactive molecule; In described mixed liquor, the mass fraction of zein is 1% ~ 5%, and the mass fraction of bioactive substance is 0.1% ~ 1%, and the mass fraction of sodium caseinate is 1% ~ 5%; Described slightly water-soluble bioactive substance is the antibacterial of slightly water-soluble and/or antioxidant;
5) preparation of Bacterial cellulose nanofiber and zein nano-particle mixed liquor
By step 3) in obtained nanofiber dispersion liquid and step 4) the bioactive zein granule that has been rich in prepared mixes, stirs, and carry out supersound process, obtain nanofiber and zein nano-particle mixed liquor; The mass ratio of described nanofiber and zein granule is (1 ~ 10): 1;
6) the biological compounded wet film preparation of Bacterial cellulose
Nanofiber and zein nano-particle mixed liquor are first carried out vacuum outgas, simulates industrial papermaking technology, vacuum filtration, film forming, obtain that there is the biological compounded wet film of bioactive Bacterial cellulose;
7) dry
The biological compounded wet film of bioactive Bacterial cellulose that has obtained in step (6) is carried out freeze-day with constant temperature or hot-pressing drying, obtains biological activity Bacterial cellulose-Compound Film of Zein.
For realizing the object of the invention further, preferably, step 3) in, described distilled water and the mass ratio of Bacterial cellulose are (1 ~ 5): 1.
Step 3) in, the rotating speed of described high-speed shearing machine is 8000 ~ 12000rpm, and shear time is 10 ~ 20min.
Step 3) in, the homogenization pressure of described high pressure microjet is 5000 ~ 20000psi, and homogenization cycles is 1 ~ 20 time.
Step 4) in, in ethanol-water solution, ethanol mass concentration is 60% ~ 95%; Described centrifugal rotating speed is 1000rpm ~ 5000rpm, and the centrifugal time is 10min ~ 30min; Antibacterial and/or the antioxidant of described slightly water-soluble is erythromycin, thymol or resveratrol.
Step 5) in, the time of supersound process is 10min ~ 20min, and ultrasonic power is 100W ~ 200W, and work efficiency is 40% ~ 60%, and operating temperature is 20 DEG C ~ 30 DEG C.
Step 6) in, the time of described vacuum outgas is 20min ~ 60min; Described vacuum filtration selects aperture to be that the cellulose microporosity filter membrane of 0.45-0.65 μm carries out vacuum filtration, fast filming to bacterial fibers and zein granule mixed liquor.
Step 7) in, described freeze-day with constant temperature is 25 ~ 60 DEG C of freeze-day with constant temperature; Described hot-pressing drying is 85 ~ 100 DEG C, carries out drying under 0.1 ~ 0.2MPa.
Described utilize acetobacter xylinum strain inoculation to prepare bacteria cellulose film be get activation in seed culture fluid after acetobacter xylinum strain inoculation in seed culture fluid, shaken cultivation, the mass ratio by 1 ~ 10% is inoculated in fermentation culture, shakes up, quiescent culture, obtains bacteria cellulose film.Fermentation culture composition: 1.8%-2.2%D-glucose, 0.45%-0.6% peptone, 0.45%-0.6% yeast extract, 0.11%-0.115% citric acid, 0.25%-0.30%Na
2hPO
412H
2o, all the other are distilled water, pH3-5; Cultural method: inoculation acetobacter xylinum is to seed culture fluid, and at 30 DEG C-35 DEG C after shaken cultivation 12h, the ratio inoculation fermentation culture medium of 1 ~ 10%, shakes up, and quiescent culture 5 days, obtains bacteria cellulose film at 30 DEG C.
Product of the present invention can be used for the bio-medical materials such as wound dressing, Living Packaging Materials in Foodstuff and beauty and make-up material;
Compared with existing product, the present invention has following beneficial effect:
(1) the present invention utilizes anti-solvent technology to prepare the water solublity zein granule being rich in bioactive substance uniquely, gives Bacterial cellulose-Compound Film of Zein material biological activity and exceptional function.
(2) mode that the present invention proposes to simulate paper industry copy paper first prepares the ideamonger of bacteria cellulose-base composite film material fast, make material preparation method rapidly and efficiently, green safety is pollution-free, for large-scale industrial production provides New Century Planned Textbook and technical foundation.
(3) the present invention adopts repeatedly through high pressure microjet homogeneous preparation Bacterial cellulose nanofiber stable uniform dispersion liquid, and adopt anti-solvent technology to prepare the water-solubility protein granule being rich in bioactive substance, achieve the homogeneous dispersion of Bacterial cellulose nanofiber in hydrophobic proteins of strongly hydrophilic.
Accompanying drawing explanation
Fig. 1 is the surface atom power plane graph of embodiment 2, sweep limits 5 microns × 5 microns, scale 500nm;
Fig. 2 is the surface atom power plane graph of comparative example 2, sweep limits 5 microns × 5 microns, scale 500nm;
Fig. 3 is the projection Electronic Speculum figure of zein granule.The form of the zein granule using anti-solvent technology to prepare is shown in figure;
Fig. 4 is the transmission electron microscope Electronic Speculum figure of embodiment 3 Bacterial cellulose nanofiber, the pure molten protein body of Semen Maydis and erythromycin mixed liquor.The homogeneous dispersion of hydrophilic Bacterial cellulose nanofiber in hydrophobin is shown in figure.
Detailed description of the invention
For understanding the present invention better, below in conjunction with meeting with embodiment, the invention will be further described, but embodiments of the present invention are not limited thereto.
Embodiment 1
The preparation of step 1, bacteria cellulose film
Medium component: 2.0%D-glucose, 0.5% peptone, 0.5% yeast extract, 0.115% citric acid, 0.27%Na
2hPO
412H
2o, all the other are distilled water, pH5.0
Cultural method: inoculation acetobacter xylinum is to seed culture fluid, and at 30 DEG C after shaken cultivation 12h, the ratio inoculation fermentation culture medium of 10%, shakes up, and quiescent culture 5 days, obtains bacteria cellulose film at 30 DEG C.
The purification of step 2, bacteria cellulose film
Get the bacteria cellulose film of above-mentioned preparation, 3 times are rinsed with clear water, being soaked in concentration is in 0.2mol/L NaOH solution, takes out, then be soaked in distilled water by this film at 90 DEG C after boiling 30min, 30min is boiled at 90 DEG C, change water, repeat 3 times, be then soaked in distilled water, until neutral, obtain the bacteria cellulose film after purification;
The preparation of step 3, Bacterial cellulose nanofiber aqueous solution
The Bacterial cellulose of above-mentioned purification is put into distilled water, the mass ratio of distilled water and Bacterial cellulose is 1:1, after stirring, with high-speed shearing machine high speed shear 20min under 12000rpm, afterwards by high pressure microjet homogenizing 10 times under 20000psi, obtain Bacterial cellulose nanofiber aqueous solution;
Step 4, be rich in the preparation of biological activity zein nano-particle
Accurately take the thymol that 1.25g zein and 0.25g non-modified are crossed, being dissolved in 25mL ethanol contend percentage composition is in the ethanol-water solution of 80%, obtains zein solution; 1.25g sodium caseinate is dissolved in 62.5mL deionized water, it is poured into rapidly in the zein solution in stirring, uses magnetic stirring apparatus fully to stir and makes its mix homogeneously.After this mixed liquor is placed in Rotary Evaporators, removing ethanol, then under 4000rpm centrifugal 10min, obtain being rich in bioactive zein nano-particle;
The preparation of step 5, Bacterial cellulose nanofiber and zein nano-particle mixed liquor
Mix obtaining Bacterial cellulose nanofiber aqueous solution in step 3 with the bioactive protein body that is rich in that step 4 obtains, Bacterial cellulose nanofiber (dry weight) is 5:1 with the mass ratio of protein body, after stirring, this mixed liquor is placed in ultrasonication machine, selection ultrasonic time is 20min, ultrasonic power is 120W, and work efficiency is 50%, and design temperature is 25 DEG C.
Step 6, vacuum filtration, fast filming
Get mixed liquor obtained in step 5, degassed 30min under the vacuum condition of 1.0MPa, selects the cellulose microporosity filter membrane in 0.65um aperture to carry out vacuum filtration to this mixed liquor, simulates industrial papermaking technology, fast filming, obtains having the biological compounded wet film of high-intensity fine fungin of antibacterial activity;
Step 7, drying
The biological compounded wet film of Bacterial cellulose step 6 obtained is at 90 DEG C, and hot-pressing drying under 0.1MPa, namely obtains the high-intensity fine fungin biological composite membrane material with antibacterial activity.
Comparative example 1
The preparation of step 1, bacteria cellulose film
Medium component: 2.0%D-glucose, 0.5% peptone, 0.5% yeast extract, 0.115% citric acid, 0.27%Na
2hPO
412H
2o, all the other are distilled water, pH 4.5.
Cultural method: inoculation acetobacter xylinum is to seed culture fluid, and at 30 DEG C after shaken cultivation 12h, the ratio inoculation fermentation culture medium of 10%, shakes up, and quiescent culture 5 days, obtains bacteria cellulose film at 30 DEG C.
The purification of step 2, bacteria cellulose film
Get the bacteria cellulose film of above-mentioned preparation, 3 times are rinsed with clear water, be soaked in 0.2mol/L NaOH solution, take out boil 30min at 90 DEG C after, then this film is soaked in distilled water, 30min is boiled at 90 DEG C, change water, repeat 3 times, be then soaked in distilled water, until neutral, obtain the bacteria cellulose film after purification;
The preparation of step 3, Bacterial cellulose nanofiber aqueous solution
The Bacterial cellulose of above-mentioned purification is put into distilled water, the mass ratio of distilled water and Bacterial cellulose is 1:1, after stirring, with high-speed shearing machine high speed shear 20min under 12000rpm, afterwards by high pressure microjet homogenizing 10 times under 20000psi, obtain Bacterial cellulose nanofiber aqueous solution;
The preparation of step 4, Bacterial cellulose nanofiber mixed liquor
Mix obtaining Bacterial cellulose nanofiber aqueous solution in step 3 according to a certain percentage with distilled water, the mass ratio of nanofiber and distilled water is 1:(500 ~ 1000), after stirring, be placed in ultrasonication machine, selection ultrasonic time is 30min, ultrasonic power is 320W, and work efficiency is 45%, and design temperature is 25 DEG C.
Step 5, vacuum filtration, fast filming
Get mixed liquor obtained in step 4, degassed 30min under the vacuum condition of 1.0MPa, selects the cellulose microporosity filter membrane in 0.65um aperture to carry out vacuum filtration to this mixed liquor, simulates industrial papermaking technology, fast filming, obtain high strength bacterial cellulose wet-coating;
Step 6, drying
The biological compounded wet film of Bacterial cellulose step 5 obtained is at 90 DEG C, and hot-pressing drying under 0.1MPa, namely obtains having high-intensity fine fungin biomembrane material.
Obtained composite film material will be tested above carry out the test of mechanical strength, obtain as following table 1 result:
The contrast of table 1 embodiment 1 and comparative example 1
As shown in Table 1, embodiment 1 is compared with comparative example 1, and the Young's modulus of composite film material, hot strength and elongation at break are all significantly improved, and particularly hot strength improves larger.Illustrate compared with original technology, present invention achieves the good combination of hydrophilic Bacterial cellulose and hydrophobicity zein, the composite film material mechanical performance of preparation gets a promotion, overcome prior art and prepare the defects such as protein-based membrane material mechanical strength is not enough, the composite film material simultaneously prepared has the biological activitys such as specific antibacterial antioxidation, can be applicable to the medical field such as active food packaging material or wound adjuvant.
Embodiment 2
The preparation of step 1, bacteria cellulose film
Medium component: 1.8%D-glucose, 0.45% peptone, 0.45% yeast extract, 0.120% citric acid, 0.25%Na
2hPO
412H
2o, all the other are distilled water, pH4.8.
Cultural method: inoculation acetobacter xylinum is to seed culture fluid, and at 30 DEG C after shaken cultivation 12h, the ratio inoculation fermentation culture medium of 15%, shakes up, and quiescent culture 5 days, obtains bacteria cellulose film at 30 DEG C.
The purification of step 2, bacteria cellulose film
Get the bacteria cellulose film of above-mentioned preparation, 3 times are rinsed with clear water, be soaked in 0.4mol/L NaOH solution, take out boil 30min at 90 DEG C after, then this film is soaked in distilled water, 30min is boiled at 90 DEG C, change water, repeat 4 times, be then soaked in distilled water, until neutral, obtain the bacteria cellulose film after purification;
The preparation of step 3, Bacterial cellulose nanofiber aqueous solution
The Bacterial cellulose of above-mentioned purification is put into distilled water, the mass ratio of distilled water and Bacterial cellulose is 1:1, after stirring, with high-speed shearing machine high speed shear 20min under 12000rpm, afterwards by high pressure microjet homogenizing 8 times under 20000psi, obtain Bacterial cellulose nanofiber aqueous solution;
Step 4, be rich in the preparation of biological activity zein nano-particle
Accurately take 1.25g zein and 0.125g without the erythromycin of modification, be dissolved in 25mL 80% ethanol-water solution; 1.25g sodium caseinate is dissolved in 62.5mL deionized water, it is poured into rapidly in the alcoholic solution in stirring, uses magnetic stirring apparatus fully to stir and makes its mix homogeneously.After this mixed liquor is placed in Rotary Evaporators, removing ethanol, then under 4000rpm centrifugal 10min, obtain the zein nano-particle with antibiotic property;
The preparation of step 5, Bacterial cellulose nanofiber and zein nano-particle mixed liquor
Mix obtaining Bacterial cellulose nanofiber aqueous solution in step 3 with the bioactive protein body that is rich in that step 4 obtains, Bacterial cellulose nanofiber (dry weight) is 5:2 with the mass ratio of protein body, after stirring, this mixed liquor is placed in ultrasonication machine, selection ultrasonic time is 20min, ultrasonic power is 120W, and work efficiency is 40%, and design temperature is 25 DEG C.
Step 6, vacuum filtration, fast filming
Get mixed liquor obtained in step 5, degassed 30min under the vacuum condition of 1.0MPa, selects the cellulose microporosity filter membrane in 0.45um aperture to carry out vacuum filtration to this mixed liquor, simulates industrial papermaking technology, fast filming, obtains having the biological compounded wet film of high-intensity fine fungin of antibacterial activity;
Step 7, drying
The biological compounded wet film of Bacterial cellulose step 6 obtained is at 90 DEG C, and hot-pressing drying under 0.1MPa, namely obtains the high-intensity fine fungin biological composite membrane material with antibacterial activity.
Comparative example 2
The preparation of step 1, bacteria cellulose film
Medium component: 1.8%D-glucose, 0.45% peptone, 0.45% yeast extract, 0.120% citric acid, 0.25%Na
2hPO
412H
2o, all the other are distilled water, pH 4.5.
Cultural method: inoculation acetobacter xylinum is to seed culture fluid, and at 30 DEG C after shaken cultivation 12h, the ratio inoculation fermentation culture medium of 15%, shakes up, and quiescent culture 5 days, obtains bacteria cellulose film at 30 DEG C.
The purification of step 2, bacteria cellulose film
Get the bacteria cellulose film of above-mentioned preparation, 3 times are rinsed with clear water, be soaked in 0.4mol/L NaOH solution, take out boil 30min at 90 DEG C after, then this film is soaked in distilled water, 30min is boiled at 90 DEG C, change water, repeat 4 times, be then soaked in distilled water, until neutral, obtain the bacteria cellulose film after purification;
The preparation of step 3, Bacterial cellulose nanofiber aqueous solution
The Bacterial cellulose of above-mentioned purification is put into distilled water, the mass ratio of distilled water and Bacterial cellulose is 1:1, after stirring, with high-speed shearing machine high speed shear 20min under 12000rpm, afterwards by high pressure microjet homogenizing 8 times under 20000psi, obtain Bacterial cellulose nanofiber aqueous solution;
Step 4, be rich in the preparation of biological activity zein nano-particle
Accurately take 1.25g zein, be dissolved in 25mL 80% ethanol-water solution; 1.25g sodium caseinate is dissolved in 62.5mL deionized water, it is poured into rapidly in the alcoholic solution in stirring, uses magnetic stirring apparatus fully to stir and makes its mix homogeneously.After this mixed liquor is placed in Rotary Evaporators, removing ethanol, then under 4000rpm centrifugal 10min, obtain the zein nano-particle with antibiotic property;
The preparation of step 5, Bacterial cellulose nanofiber and zein nano-particle mixed liquor
Mix obtaining Bacterial cellulose nanofiber aqueous solution in step 3 with the bioactive protein body that is rich in that step 4 obtains, Bacterial cellulose nanofiber (dry weight) is 5:2 with the mass ratio of protein body, after stirring, this mixed liquor is placed in ultrasonication machine, selection ultrasonic time is 20min, ultrasonic power is 120W, and work efficiency is 40%, and design temperature is 25 DEG C.
Step 6, vacuum filtration, fast filming
Get mixed liquor obtained in step 5, degassed 30min under the vacuum condition of 1.0MPa, selects the cellulose microporosity filter membrane in 0.45um aperture to carry out vacuum filtration to this mixed liquor, simulates industrial papermaking technology, fast filming, obtains having the biological compounded wet film of high-intensity fine fungin of antibacterial activity;
Step 7, drying
The biological compounded wet film of Bacterial cellulose step 6 obtained is at 90 DEG C, and hot-pressing drying under 0.1MPa, namely obtains the high-intensity fine fungin biological composite membrane material with antibacterial activity.
Obtained composite film material will be tested above carry out the test of atomic force microscope and mechanical strength, obtain following result:
The contrast of table 2 embodiment 2 and comparative example 2
As shown in Table 2, embodiment 2 is compared with comparative example 2, and the roughness change on film surface is little, also can find out significantly from accompanying drawing 3 and the atomic plane graph of accompanying drawing 4 composite film surface, two kinds of film surface changes are little, and surface is all in graininess, and roughness is similar.And as can be seen from hot strength and Young's modulus data also, the mechanical strength change of two kinds of films is little, illustrates and add active component on the roughness on film surface and mechanical strength impact thereof not quite.Compared with original technology, this patent, while maintaining bacteria cellulose-base composite film material mechanical strength, also imparts composite film material biological activity, has widened its range of application.
Embodiment 3
The preparation of step 1, bacteria cellulose film
Medium component: 2.2%D-glucose, 0.6% peptone, 0.6% yeast extract, 0.110% citric acid, 0.30%Na
2hPO
412H
2o, all the other are distilled water, pH 4.0.
Cultural method: inoculation acetobacter xylinum is to seed culture fluid, and at 30 DEG C after shaken cultivation 12h, the ratio inoculation fermentation culture medium of 12%, shakes up, and quiescent culture 5 days, obtains bacteria cellulose film at 30 DEG C.
The purification of step 2, bacteria cellulose film
Get the bacteria cellulose film of above-mentioned preparation, 3 times are rinsed with clear water, be soaked in 0.2mol/L KOH solution, take out boil 30min at 90 DEG C after, then this film is soaked in distilled water, 30min is boiled at 90 DEG C, change water, repeat 5 times, be then soaked in distilled water, until neutral, obtain the bacteria cellulose film after purification;
The preparation of step 3, Bacterial cellulose nanofiber aqueous solution
The Bacterial cellulose of above-mentioned purification is put into distilled water, the mass ratio of distilled water and Bacterial cellulose is 1:1, after stirring, with high-speed shearing machine high speed shear 20min under 12000rpm, afterwards by high pressure microjet homogenizing 9 times under 20000psi, obtain Bacterial cellulose nanofiber aqueous solution;
Step 4, be rich in the preparation of biological activity zein nano-particle
Accurately take 1.25g zein and 0.5g without the erythromycin of modification, be dissolved in 25mL 80% ethanol-water solution; 1.25g sodium caseinate is dissolved in 62.5mL deionized water, it is poured into rapidly in the alcoholic solution in stirring, uses magnetic stirring apparatus fully to stir and makes its mix homogeneously.After this mixed liquor is placed in Rotary Evaporators, removing ethanol, then under 4000rpm centrifugal 10min, obtain the zein nano-particle with antibiotic property;
The preparation of step 5, Bacterial cellulose nanofiber and zein nano-particle mixed liquor
Mix obtaining Bacterial cellulose nanofiber aqueous solution in step 3 with the bioactive protein body that is rich in that step 4 obtains, Bacterial cellulose nanofiber (dry weight) is 5:2 with the mass ratio of protein body, after stirring, this mixed liquor is placed in ultrasonication machine, selection ultrasonic time is 20min, ultrasonic power is 120W, and work efficiency is 60%, and design temperature is 25 DEG C.
Step 6, vacuum filtration, fast filming
Get mixed liquor obtained in step 5, degassed 30min under the vacuum condition of 1.0MPa, selects the cellulose microporosity filter membrane in 0.65um aperture to carry out vacuum filtration to this mixed liquor, simulates industrial papermaking technology, fast filming, obtains having the biological compounded wet film of high-intensity fine fungin of antibacterial activity;
Step 7, drying
The biological compounded wet film of Bacterial cellulose step 6 obtained is at 90 DEG C, and hot-pressing drying under 0.1MPa, namely obtains the high-intensity fine fungin biological composite membrane material with antibacterial activity.
Composite film material obtained is above carried out bacteriostatic test test, obtains result as follows:
The contrast of table 3 embodiment and comparative example's bacteriostatic test
From the contrast of table 3 pair staphylococcus aureus inhibition zone, composite film material prepared by embodiment has larger inhibition zone, comparative example does not then all have inhibition zone, not there is antibiotic property, illustrate that the present invention is after with the addition of active component (antibacterial), really bacterial cellulose composite membrane material material antibacterial activity is imparted, compared with original technology, the present invention has stronger broad spectrum activity, when namely preparing activated protein granule by anti-solvent technology, correspondingly can add dissimilar bioactive ingredients (antibacterial/antioxidation) according to demand, the bacteria cellulose composite membrane correspondingly prepared has the biological activity such as antibacterial/antioxidation accordingly, and there is higher mechanical strength, range of application is more extensive.
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