Browsing by Subject "Electrospinning"

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Open Access
Amidoxime functionalized Polymers of Intrinsic Microporosity (PIM-1) electrospun ultrafine fibers for rapid removal of uranyl ions from water
(Elsevier, 2018) Satılmış, Berk; Işık, T.; Demir, M. M.; Uyar, Tamer
The Polymers of Intrinsic Microporosity (PIM-1) is considered as one of the most promising polymer candidates for adsorption applications owing to its high surface area and the ability to tailor the functionality for the targeted species. This study reports a facile method for the preparation of amidoxime functionalized PIM-1 fibrous membrane (AF-PIM-FM) by electrospinning technique and its practical use for the extraction of U(VI) ions from aqueous systems via column sorption under continuous flow. Fibrous membrane form of amidoxime functionalized PIM-1 (AF-PIM-FM) was prepared by electrospinning method owing to its excellent processability in dimethylformamide. Bead-free and uniform fibers were obtained as confirmed by SEM imaging and average fiber diameter was 1.69 ± 0.34 μm for AF-PIM-FM. In addition, electrospun PIM-1 fibrous membrane (PIM-FM) was prepared as a control group. Structural and thermal characterization of powder and membrane forms of the materials were performed using FT-IR, 1 H NMR, XPS, Elemental analyses, TGA, and DSC. The porosity of the samples was measured by N2 sorption isotherms confirming amidoxime PIM-1 still maintain their porosity after functionalization. Amidoxime functionality along with membrane structure makes AF-PIM-FM a promising material for uranyl adsorption. First, a comparison between powder and membrane form of amidoxime functionalized PIM-1 was investigated using batch adsorption process. Although membrane form has shown slightly lower adsorption performance in the batch adsorption process, the advantage of using the membrane in column adsorption processes makes membrane form more feasible for real applications. In addition, amidoxime modification enhanced the uranium adsorption ability of PIM-FM up to 20 times. The effect of initial concentration and pH were investigated along with regeneration of the adsorbents. AF-PIM-FM was successfully used for five adsorption-desorption cycles without having any damage on the fibrous structure.
Open Access
Amine modified electrospun PIM-1 ultrafine fibers for an efficient removal of methyl orange from an aqueous system
(Elsevier, 2018) Satılmış, B.; Uyar, Tamer
Polymers of Intrinsic Microporosity (PIM-1) is a promising material for adsorption and separation applications. While PIM-1 displays high affinity for neutral species, it shows lack of interaction with charged molecules in an aqueous system due to non-polar nature of it. Functionalization of PIM-1 provides an advantage of tailoring the interaction ability as well as the adsorption performance of PIM-1 towards target pollutants. In this study, electrospun Polymer of Intrinsic Microporosity (PIM-1) fibrous membrane (PIM-FM) was reacted with borane dimethyl sulfide complex to obtain amine modified PIM-1 fibrous membrane (AM-PIM-FM). Furthermore, PIM-1 film, which is referred as PIM-1 dense membrane (PIM-DM), was also modified under the same conditions as a control material. Structural analyses have confirmed that nitrile groups of PIM-1 have been fully converted to amine group as a result of the reduction reaction. Average fiber diameter of parent PIM-1 fibers was found 2.3 ± 0.3 μm, and it remained almost the same after the amine modification. In addition, no physical damage has been observed on fiber structure based on the SEM analysis. Both amine modified PIM-1 dense and fibrous membranes became insoluble in common organic solvents. Before the modification, water contact angle of PIM-FM was 138 ± 2° which also remained almost the same after the modification, showing water contact angle of 131 ± 8°. The insolubility along with amine functionality make membranes promising materials for adsorption of anionic dyes from wastewater. Here, dye (i.e. Methyl Orange) removal ability of AM-PIM-FM from an aqueous system was investigated and compared with parent PIM-1 (PIM-FM) as well as dense membrane form (AM-PIM-DM). AM-PIM-FM shows extremely higher adsorption capacity than that of PIM-FM and AM-PIM-DM. The maximum adsorption capacity of AM-PIM-FM was found 312.5 mg g−1 for Methyl Orange. Langmuir isotherm model was found more favorable for the adsorption. AM-PIM-FM was employed effectively in continuous adsorption/desorption studies for several times without having any damage on fiber morphology using batch adsorption process. Furthermore, AM-PIM-FM was successfully used as a molecular filter for the removal of methyl orange from an aqueous system. The results indicate that AM-PIM-FM could be a promising adsorbent for removal of anionic molecules from an aqueous system.
Open Access
Antibacterial activity of cyclodextrin-Azo dye inclusion complex encapsulated electrospun polycaprolactone nanofibers
(Wiley-VCH Verlag GmbH & Co. KGaA, 2021-10-12) Demirci, Serkan; Çelebioğlu, Aslı; Demirci, S. K.; İdil, Ö.
Polycaprolactone (PCL) nanofibers incorporating azo dye/γ-cyclodextrin inclusion complex (Azo/γ-CD-IC) were successfully produced. The characteristics of the Azo/γ-CD-IC and PCL/Azo/γ-CD-IC nanofibers were investigated by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and thermogravimetric analysis (TGA). Based on the SEM analysis the prepared nanofiber has a smooth surface with a size diameter below 500 nm. Meanwhile, the thermal stability of Azo was further improved after being embedded into Azo/γ-CD-IC and the PCL/Azo/γ-CD-IC nanofibers. Proton nuclear magnetic resonance (1H-NMR) was used to calculate the molar ratio of Azo/γ-CD. The antibacterial activity of the PCL/Azo/γ-CD-IC and PCL/Azo nanofibers was investigated using colony counting method and bacterial strains of Escherichia coli and Staphylococcus aureus were used. The results indicated that PCL/Azo/γ-CD-IC nanofibers have enhanced antibacterial activity against Escherichia coli and Staphylococcus aureus compared to PCL/Azo owing to inclusion complexation. Therefore, these PCL/Azo/γ-CD-IC nanofibers might have potential applications in the biomedical field.
Open Access
Antibacterial electrospun nanofibers from triclosan/cyclodextrin inclusion complexes
(Elsevier, 2014) Celebioglu A.; Umu, O. C. O.; Tekinay, T.; Uyar, Tamer
The electrospinning of nanofibers (NF) from cyclodextrin inclusion complexes (CD-IC) with an antibacterial agent (triclosan) was achieved without using any carrier polymeric matrix. Polymer-free triclosan/CD-IC NF were electrospun from highly concentrated (160% CD, w/w) aqueous triclosan/CD-IC suspension by using two types of chemically modified CD; hydroxypropyl-beta-cyclodextrin (HPβCD) and hydroxypropyl-gamma-cyclodextrin (HPγCD). The morphological characterization of the electrospun triclosan/CD-IC NF by SEM elucidated that the triclosan/HPβCD-IC NF and triclosan/HPγCD-IC NF were bead-free having average fiber diameter of 520±250nm and 1100±660nm, respectively. The presence of triclosan and the formation of triclosan/CD-IC within the fiber structure were confirmed by 1H-NMR, FTIR, XRD, DSC, and TGA studies. The initial 1:1molar ratio of the triclosan:CD was kept for triclosan/HPβCD-IC NF after the electrospinning and whereas 0.7:1molar ratio was observed for triclosan/HPγCD-IC NF and some uncomplexed triclosan was detected suggesting that the complexation efficiency of triclosan with HPγCD was lower than that of HPβCD. The antibacterial properties of triclosan/CD-IC NF were tested against Gram-negative (Escherichia coli) and Gram-positive (Staphylococcus aureus) bacteria. It was observed that triclosan/HPβCD-IC NF and triclosan/HPγCD-IC NF showed better antibacterial activity against both bacteria compared to uncomplexed pure triclosan.
Open Access
Antibacterial electrospun poly(lactic acid) (PLA) nanofibrous webs incorporating triclosan/cyclodextrin inclusion complexes
(2013) Kayaci F.; Umu O.C.O.; Tekinay, T.; Uyar, T.
Solid triclosan/cyclodextrin inclusion complexes (TR/CD-IC) were obtained and then incorporated in poly(lactic acid) (PLA) nanofibers via electrospinning. α-CD, β-CD, and γ-CD were tested for the formation of TR/CD-IC by a coprecipitation method; however, the findings indicated that α-CD could not form an inclusion complex with TR, whereas β-CD and γ-CD successfully formed TR/CD-IC crystals, and the molar ratio of TR to CD was found to be 1:1. The structural and thermal characteristics of TR/CD-IC were investigated by 1H NMR, FTIR, XRD, DSC, and TGA studies. Then, the encapsulation of TR/β-CD-IC and TR/γ-CD-IC in PLA nanofibers was achieved. Electrospun PLA and PLA/TR nanofibers obtained for comparison were uniform, whereas the aggregates of TR/CD-IC crystals were present and distributed within the PLA fiber matrix as confirmed by SEM and XRD analyses. The antibacterial activity of these nanofibrous webs was investigated. The results indicated that PLA nanofibers incorporating TR/CD-IC showed better antibacterial activity against Staphylococcus aureus and Escherichia coli bacteria compared to PLA nanofibers containing only TR without CD-IC. Electrospun nanofibrous webs incorporating TR/CD-IC may be applicable in active food packaging due to their very high surface area and nanoporous structure as well as efficient antibacterial property. © 2013 American Chemical Society.
Open Access
Antibacterial electrospun zein nanofibrous web encapsulating thymol/cyclodextrin-inclusion complex for food packaging
(Elsevier, 2017-10) Aytac Z.; Ipek, S.; Durgun, Engin; Tekinay, T.; Uyar, Tamer
Thymol (THY)/γ-Cyclodextrin(γ-CD) inclusion complex (IC) encapsulated electrospun zein nanofibrous webs (zein-THY/γ-CD-IC-NF) were fabricated as a food packaging material. The formation of THY/γ-CD-IC (1:1 and 2:1) was proved by experimental (X-ray diffraction (XRD), thermal gravimetric analysis (TGA), 1H NMR) and computational techniques. THY/γ-CD-IC (2:1) exhibited higher preservation rate and stability than THY/γ-CD-IC (1:1). It is worth mentioning that zein-THY/γ-CD-IC-NF (2:1) preserved much more THY as observed in TGA and stability of THY/γ-CD-IC (2:1) was higher, as shown by a modelling study. Therefore, much more THY was released from zein-THY/γ-CD-IC-NF (2:1) than zein-THY-NF and zein-THY/γ-CD-IC-NF (1:1). Similarly, antibacterial activity of zein-THY/γ-CD-IC-NF (2:1) was higher than zein-THY-NF and zein-THY/γ-CD-IC-NF (1:1). It was demonstrated that zein-THY/γ-CD-IC-NF (2:1) was most effective in inhibiting the growth of bacteria on meat samples. These webs show potential application as an antibacterial food packaging material.
Open Access
Antibacterial nanofibers of pullulan/tetracycline-cyclodextrin inclusion complexes for fast-disintegrating oral drug delivery
(Elsevier Inc., 2021-12-08) Hsiung, E.; Celebioglu, A.; Chowdhury, R.; Kilic, M. E.; Durgun, Engin; Altier, C.; Uyar, T.
Tetracycline is a widely used antibiotic suffering from poor water solubility and low bioavailability. Here, hydroxypropyl-beta-cyclodextrin (HPβCD) was used to form inclusion complexes (IC) of tetracycline with 2:1 M ratio (CD:drug). Then, tetracycline-HPβCD-IC was mixed with pullulan- a non-toxic, water-soluble biopolymer - to form nanofibrous webs via electrospinning. The electrospinning of pullulan/tetracycline-HPβCD-IC was yielded into defect-free nanofibers collected in the form of a self-standing and flexible material with the loading capacity of ∼ 7.7 % (w/w). Pullulan/tetracycline nanofibers was also generated as control sample having the same drug loading. Tetracycline was found in the amorphous state in case of pullulan/tetracycline-HPβCD nanofibers due to inclusion complexation. Through inclusion complexation with HPβCD, enhanced aqueous solubility and faster release profile were provided for pullulan/tetracycline-HPβCD-IC nanofibers compared to pullulan/tetracycline one. Additionally, pullulan/tetracycline-HPβCD-IC nanofibers readily disintegrated when wetted with artificial saliva while pullulan/tetracycline nanofibers were not completely absorbed by the same simulate environment. Electrospun nanofibers showed promising antibacterial activity against both gram-positive and gram-negative bacteria. Briefly, our findings indicated that pullulan/tetracycline-HPβCD-IC nanofibers could be an attractive material as orally fast disintegrating drug delivery system for the desired antibiotic treatment thanks to its promising physicochemical and antibacterial properties.
Open Access
Antioxidant vitamin E/cyclodextrin inclusion complex electrospun nanofibers: enhanced water solubility, prolonged shelf life, and photostability of vitamin E
(American Chemical Society, 2017) Çelebioğlu, Aslı; Uyar, Tamer
Here, we demonstrated the electrospinning of polymer-free nanofibrous webs from inclusion complex (IC) between hydroxypropyl-β-cyclodextrin (HPβCD) and Vitamin E (Vitamin E/HPβCD-IC NF). The inclusion complexation between HPβCD and Vitamin E was prepared by using two different molar ratios (Vitamin E/HPβCD; 1:2 and 1:1), which correspond to theoretical value of ∼13% (w/w) and 26% (w/w) loading of Vitamin E in the nanofiber (NF) matrix. After electrospinning and storage, a very high loading of Vitamin E (up to ∼11% w/w, with respect to fiber matrix) was preserved in Vitamin E/HPβCD-IC NF. Because of the cyclodextrin inclusion complexation, only a minimal weight loss (only ∼2% w/w) was observed. While pure Vitamin E is insoluble in water, Vitamin E/HPβCD-IC NF web has displayed fast-dissolving behavior. Because of the greatly enhanced water-solubility of Vitamin E, Vitamin E/HPβCD-IC NF web has shown effective antioxidant activity. Additionally, Vitamin E/HPβCD-IC NF web has provided enhanced photostability for the sensitive Vitamin E by the inclusion complexation in which Vitamin E/HPβCD-IC NF still kept its antioxidant activity even after exposure to UV-light. Moreover, a 3 year-old Vitamin E/HPβCD-IC NF sample has shown very similar antioxidant efficiency when compared with freshly prepared Vitamin E/HPβCD-IC NF indicating that long-term stability was achieved for Vitamin E in the CD-IC fiber matrix. In brief, our results suggested that polymer-free electrospun Vitamin E/HPβCD-IC nanofibrous webs could have potential applications in food, pharmaceuticals, and healthcare thanks to its efficient antioxidant activity along with enhanced water-solubility, prolonged shelf life, and high photostability of Vitamin E.
Open Access
Atomic layer deposition of NiOOH/Ni(OH) 2 on PIM-1-based N-Doped carbon nanofibers for electrochemical water splitting in alkaline medium
(Wiley‐VCH Verlag GmbH & Co. KGaA, Weinheim, 2019) Patil, Bhushan; Satılmış, Bekir; Khalily, Mohammad Aref; Uyar, Tamer
Portable and flexible energy devices demand lightweight and highly efficient catalytic materials for use in energy devices. An efficient water splitting electrocatalyst is considered an ideal future energy source. Well‐aligned high‐surface‐area electrospun polymers of intrinsic microporosity (PIM‐1)‐based nitrogen‐doped carbon nanofibers were prepared as a free‐standing flexible electrode. A non‐noble‐metal catalyst NiOOH/Ni(OH)2 was precisely deposited over flexible free‐standing carbon nanofibers by using atomic layer deposition (ALD). The morphology, high surface area, nitrogen doping, and Ni states synergistically showed a low onset potential (ηHER=−40 and ηOER=290 mV vs. reversible hydrogen electrode), small overpotential at η10 [oxygen evolution reaction (OER)=390.5 mV and hydrogen evolution reaction (HER)=−147 mV], excellent kinetics (Tafel slopes for OER=50 mV dec−1 and HER=41 mV dec−1), and high stability (>16 h) towards water splitting in an alkaline medium (0.1 m KOH). The performance was comparable with that of state‐of‐the‐art noble‐metal catalysts (e.g., Ir/C, Ru/C for OER, and Pt/C for HER). Post‐catalytic characterization with X‐ray photoelectron spectroscopy (XPS) and Raman spectroscopy further proved the durability of the electrode. This study provides insight into the design of 1D‐aligned N‐doped PIM‐1 electrospun carbon nanofibers as a flexible and free‐standing NiOOH/Ni(OH)2 decorated electrode as a highly stable nanocatalyst for water splitting in an alkaline medium.
Open Access
Atomic layer deposition of ruthenium nanoparticles on electrospun carbon nanofibers: a highly efficient nanocatalyst for the hydrolytic dehydrogenation of methylamine borane
(American Chemical Society, 2018) Khalily, Mohammad Aref; Yurderi, M.; Haider, Ali; Bulut, A.; Patil, Bhushan; Zahmakiran, M.; Uyar, Tamer
We report the fabrication of a novel and highly active nanocatalyst system comprising electrospun carbon nanofiber (CNF)-supported ruthenium nanoparticles (NPs) (Ru@CNF), which can reproducibly be prepared by the ozone-assisted atomic layer deposition (ALD) of Ru NPs on electrospun CNFs. Polyacrylonitrile (PAN) was electropsun into bead-free one-dimensional (1D) nanofibers by electrospinning. The electrospun PAN nanofibers were converted into well-defined 1D CNFs by a two-step carbonization process. We took advantage of an ozone-assisted ALD technique to uniformly decorate the CNF support by highly monodisperse Ru NPs of 3.4 ± 0.4 nm size. The Ru@CNF nanocatalyst system catalyzes the hydrolytic dehydrogenation of methylamine borane (CH3NH2BH3), which has been considered as one of the attractive materials for the efficient chemical hydrogen storage, with a record turnover frequency of 563 mol H2/mol Ru × min and an excellent conversion (>99%) under air at room temperature with the activation energy (Ea) of 30.1 kJ/mol. Moreover, Ru@CNF demonstrated remarkable reusability performance and conserved 72% of its inherent catalytic activity even at the fifth recycle.
Open Access
Bacteria encapsulated electrospun nanofibrous webs for remediation of methylene blue dye in water
(Elsevier, 2017-04) Sarioglu O.F.; Keskin, N. O. S.; Celebioglu A.; Tekinay, T.; Uyar, Tamer
In this study, preparation and application of novel biocomposite materials that were produced by encapsulation of bacterial cells within electrospun nanofibrous webs are described. A commercial strain of Pseudomonas aeruginosa which has methylene blue (MB) dye remediation capability was selected for encapsulation, and polyvinyl alcohol (PVA) and polyethylene oxide (PEO) were selected as the polymer matrices for the electrospinning of bacteria encapsulated nanofibrous webs. Encapsulation of bacterial cells was monitored by scanning electron microscopy (SEM) and fluorescence microscopy, and the viability of encapsulated bacteria was checked by live/dead staining and viable cell counting assay. Both bacteria/PVA and bacteria/PEO webs have shown a great potential for remediation of MB, yet bacteria/PEO web has shown higher removal performances than bacteria/PVA web, which was probably due to the differences in the initial viable bacterial cells for those two samples. The bacteria encapsulated electrospun nanofibrous webs were stored at 4 °C for three months and they were found as potentially storable for keeping encapsulated bacterial cells alive. Overall, the results suggest that electrospun nanofibrous webs are suitable platforms for preservation of living bacterial cells and they can be used directly as a starting inoculum for bioremediation of water systems.
Open Access
Bacteria immobilized electrospun polycaprolactone and polylactic acid fibrous webs for remediation of textile dyes in water
(Elsevier, 2017-10) Sarioglu O.F.; S. Keskin, N. O.; Celebioglu A.; Tekinay, T.; Uyar, Tamer
In this study, preparation and application of novel biocomposite materials for textile dye removal which are produced by immobilization of specific bacteria onto electrospun nanofibrous webs are presented. A textile dye remediating bacterial isolate, Clavibacter michiganensis, was selected for bacterial immobilization, a commercial reactive textile dye, Setazol Blue BRF-X, was selected as the target contaminant, and electrospun polycaprolactone (PCL) and polylactic acid (PLA) nanofibrous polymeric webs were selected for bacterial integration. Bacterial adhesion onto nanofibrous webs was monitored by scanning electron microscopy (SEM) imaging and optical density (OD) measurements were performed for the detached bacteria. After achieving sufficient amounts of immobilized bacteria on electrospun nanofibrous webs, equivalent web samples were utilized for testing the dye removal capabilities. Both bacteria/PCL and bacteria/PLA webs have shown efficient remediation of Setazol Blue BRF-X dye within 48 h at each tested concentration (50, 100 and 200 mg/L), and their removal performances were very similar to the free-bacteria cells. The bacteria immobilized webs were then tested for five times of reuse at an initial dye concentration of 100 mg/L, and found as potentially reusable with higher bacterial immobilization and faster dye removal capacities at the end of the test. Overall, these findings suggest that electrospun nanofibrous webs are available platforms for bacterial integration and the bacteria immobilized webs can be used as starting inocula for use in remediation of textile dyes in wastewater systems.
Open Access
Bacteria-immobilized electrospun fibrous polymeric webs for hexavalent chromium remediation in water
(Springer Berlin Heidelberg, 2016) Sarioglu, O.F.; Celebioglu A.; Tekinay, T.; Uyar, Tamer
The development of hexavalent chromium remediating fibrous biocomposite mats through the immobilization of a hexavalent chromium reducing bacterial strain, Morganella morganiiSTB5, on the surfaces of electrospun polystyrene and polysulfone webs is described. The bacteria-immobilized biocomposite webs have shown removal yields of 93.60 and 93.79 % for 10 mg/L, 99.47 and 90.78 % for 15 mg/L and 70.41 and 68.27 % for 25 mg/L of initial hexavalent chromium within 72 h, respectively, and could be reused for at least five cycles. Storage test results indicate that the biocomposite mats can be stored without losing their bioremoval capacities. Scanning electron microscopy images of the biocomposite webs demonstrate that biofilms of M. morganii STB5 adhere strongly to the fibrous polymeric surfaces and are retained after repeated cycles of use. Overall, the results suggest that reusable bacteria-immobilized fibrous biocomposite webs might be applicable for continuous hexavalent chromium remediation in water systems.
Open Access
Bioactive surface design based on functional composite electrospun nanofibers for biomolecule immobilization and biosensor applications
(American Chemical Society, 2014-03-24) Uzun, S. D.; Kayaci, F.; Uyar, T.; Timur, S.; Toppare, L.
The combination of nanomaterials and conducting polymers attracted remarkable attention for development of new immobilization matrices for enzymes. Hereby, an efficient surface design was investigated by modifying the graphite rod electrode surfaces with one-step electrospun nylon 6,6 nanofibers or 4% (w/w) multiwalled carbon nanotubes (MWCNTs) incorporating nylon 6,6 nanofibers (nylon 6,6/4MWCNT). High-resolution transmission electron microscopy study confirmed the successful incorporation of the MWCNTs into the nanofiber matrix for nylon 6,6/4MWCNT sample. Then, these nanofibrous surfaces were coated with a conducting polymer, (poly-4-(4,7-di(thiophen-2-yl)-1H-benzo[d]imidazol-2-yl) benzaldehyde) (PBIBA) to obtain a high electroactive surface area as new functional immobilization matrices. Due to the free aldehyde groups of the polymeric structures, a model enzyme, glucose oxidase was efficiently immobilized to the modified surfaces via covalent binding. Scanning electron microscope images confirmed that the nanofibrous structures were protected after the electrodeposition step of PBIBA and a high amount of protein attachment was successfully achieved by the help of high surface to volume ratio of electroactive nanofiber matrices. The biosensors were characterized in terms of their operational and storage stabilities and kinetic parameters (K mapp and Imax). The resulting novel glucose biosensors revealed good stability and promising Imax values (10.03 and 16.67 μA for nylon 6,6/PBIBA and nylon 6,6/4MWCNT/PBIBA modified biosensors, respectively) and long shelf life (32 and 44 days for nylon 6,6/PBIBA and nylon 6,6/4MWCNT/PBIBA modified biosensors, respectively). Finally, the biosensor was tested on beverages for glucose detection. © 2014 American Chemical Society.
Open Access
Biocatalytic protein membranes fabricated by electrospinning
(Elsevier B.V., 2016) Kabay, G.; Kaleli, G.; Sultanova, Z.; Ölmez, T. T.; Şeker, U. Ö. Ş.; Mutlu, M.
In this study, a protein-based catalytic membrane was produced by electrospinning. Membrane activity was characterised in terms of response current for various glucose concentrations. We focused on the preparation of a scaffold by converting a globular protein to other structural forms using catastrophic solvents. A scaffolding protein, bovine serum albumin, and an enzyme, glucose oxidase (GOD), were selected as a model natural carrier matrix and a biologically active agent, respectively. Beta-mercaptoethanol (β-ME) was used to convert the globular protein to an amyloid-like form. A structural stabilising agent, 2,2,2-triflouroethanol (TFE), was used to maintain the final α-helical structure of the amyloid-like protein. The TFE:PBS (phosphate-buffered saline) ratio and various electrospinning parameters were analysed to minimise activity loss. Using this approach, we applied electrospinning to an active enzyme to obtain biocatalytic nanofibrous membranes. After optimising the protein electrospinning process, the activities of the protein nanofibrous membranes were monitored. GOD remained active in the new membrane structure. The highest enzyme activity was observed for the membranes prepared with a 1.5:1 (v:v) TFE:PBS solvent ratio. In that particular case, the immobilized enzyme created a current of 0.7 μA and the apparent activity was 2547 ± 132 U/m2.
Open Access
Carvacrol loaded electrospun fibrous films from zein and poly(lactic acid) for active food packaging
(Elsevier B.V., 2018) Altan, A.; Aytaç, Zeynep; Uyar, Tamer
The composite fibrous films were developed from zein and poly(lactic acid) (PLA) by incorporating carvacrol at three different concentrations (5, 10 and 20%) using electrospinning. The morphology and size of fibers obtained from both zein and PLA were affected by the level of the incorporated carvacrol. The Fourier transform infrared (FTIR) spectroscopy and thermogravimetric analysis (TGA) results showed that carvacrol was encapsulated in electrospun zein and PLA fibers. The antioxidant activity of carvacrol loaded zein fibers ranged from 62 to 75%, while antioxidant capacity of PLA fibers varied from 53 to 65% for 5-20% carvacrol content. The composite fibrous films showed a sustained diffusion controlled release behavior. Preliminary studies on whole wheat bread samples showed that carvacrol loaded electrospun zein and PLA fibers are able to preserve bread samples, indicating that they are good candidates for active food packaging applications to extend the shelf life of whole wheat bread.
Open Access
Catechin encapsulated antioxidant electrospun nanofibers: A comparative study between cyclodextrin complex nanofibers and poly(vinyl alcohol) nanofibers
(American Chemical Society, 2023-05-31) Yıldız, Zehra İrem; Topuz, Fuat; Uyar, Tamer
Catechin is a plant polyphenol with a strong antioxidant effect. However, its use is limited due to its poor water solubility and sensitivity to light and oxygen. Here, catechin could be solubilized by inclusion complexation with cyclodextrin (CD) (CD-IC), and their solutions were electrospun into fibers in the presence and absence of poly(vinyl alcohol) (PVA) to compare the stabilization of catechin for its antioxidant activity. The antioxidant activity of catechin/CD IC nanofibers was also compared to that of the powder form. Scanning electron microscopy (SEM) analysis revealed the production of bead-free nanofibers. The successful incorporation of catechin into nanofibers was confirmed by Fourier-transform infrared spectroscopy (FTIR) analysis of catechin CC bond stretching. Likewise, 1H NMR spectroscopic analysis revealed the characteristic aromatic protons of catechin. The formation of inclusion complexes was confirmed by X-ray diffraction (XRD) and dissolution testing by the disappearance of crystalline peaks and rapid fiber dissolution, respectively. Finally, antioxidant testing demonstrated the higher antioxidant activity of polymer-free CD-IC nanofibers.
Open Access
Colon targeted delivery of niclosamide from β-cyclodextrin inclusion complex incorporated electrospun Eudragit® L100 nanofibers
(Elsevier BV, 2021-01) Çoban, Ö.; Aytaç, Zeynep; Yıldız, Zehra İrem; Uyar, Tamer
Electrospun nanofibers incorporated with inclusion complex (IC) of niclosamide (NIC) and hydroxypropyl-beta-cyclodextrin (HPβCD) (NIC-HPβCD-IC) was produced from pH-responsive polymer (Eudragit® L100, EUD), which disintegrates at pH values higher than 6, (EUD-NIC-HPβCD-IC-NF) for targeted delivery of NIC to the colon. Pristine EUD nanofibers (EUD-NF), only NIC loaded (EUD-NIC-NF) and physical mixture of NIC and HPβCD loaded EUD nanofibers (EUD-NIC-HPβCD-NF) were also produced as reference. SEM images revealed the bead-free and uniform morphology of nanofibers. XRD, TGA, and DSC were also performed for both NIC-HPβCD-IC and electrospun nanofibers and it was seen that there are some NIC molecules, which cannot make IC. Dissolution studies were carried out for 240 min at pH 1.2 and pH 7 simulating stomach and colon, respectively. EUD-NIC-NF released almost 53 % of NIC in 120 min, whereas EUD-NIC-HPβCD-NF (15 %) and EUD-NIC-HPβCD-IC-NF (8 %) released at most 15 % of NIC in 120 min. Then, remained NIC in the nanofibers released into the colon for the next 120 min. The slight difference in the release of NIC into stomach from EUD-NIC-HPβCD-NF and EUD-NIC-HPβCD-IC-NF might be due to the uncomplexed NIC molecules in EUD-NIC-HPβCD-IC-NF. More importantly, EUD-NIC-HPβCD-IC-NF was quite effective for preventing the release of NIC in the stomach in contrast to EUD-NIC-NF, which has already released more than half amount of NIC in 120 min. In conclusion, this study might open new areas for developing targeted delivery systems by the combination of nanofibers and CD-ICs for hydrophobic drugs such as NIC.
Open Access
Conscientious design of Zn-S/Ti-N layer by transformation of ZnTiO3 on electrospun ZnTiO3@TiO2 nanofibers: stability and reusable photocatalytic performance under visible irradiation
(American Chemical Society, 2018) Ranjith, K. S.; Uyar, Tamer
Herein, we report the rational design of Zn-S/Ti-N on TiO2 as a hierarchical nanoarchitecture from the ZnTiO3@TiO2 nanofibers (NFs) through electrospinning followed by a hydrothermal process using l-cysteine as an S/N source. Controlling the hydrothermal temperature, the hierarchical form of NFs exhibited highly efficient visible catalytic behavior for organic dye (i.e., Rhodamine B) degradation since S and N based surface function on the oxide surface resulted in unique interlayer induced strain coupled surface defects. The surface functionalization of the ZnTiO3 surface with S and N was solidly confirmed by X-ray photo-electrospectroscopy (XPS) and energy-dispersive X-ray (EDX) with elemental mapping results. Inducing the S/N functionality at higher hydrothermal temperature reverses the structural arrangement of ZnTiO3 favoring the interaction of S preferably with Zn and Ti with N for the formation of ZnS/TiN@TiO2 NFs. The tunable band function through the Zn-S/Ti-N cofunctionalization exhibited effective long-term catalytic performance under UV and visible irradiation with a degradation rate of 0.0362 and 0.0313 min-1, which is nearly 3.1 and 1.3 times higher than that of the ZnTiO3@TiO2 and ZnTiO3-S/N@TiO2 NFs, respectively. The catalysts are highly photoactive after multiple photocatalytic cycles with stable surface and structural features under visible irradiation. The study could provide new opportunities for designing hierarchical structures in ternary form of nanoscale architectures for effective visible photocatalytic activity. Copyright
Open Access
Core-shell nanofibers of curcumin/cyclodextrin inclusion complex and polylactic acid: enhanced water solubility and slow release of curcumin
(Elsevier, 2017-02) Aytaç, Zeynep; Uyar, Tamer
Core-shell nanofibers were designed via electrospinning using inclusion complex (IC) of model hydrophobic drug (curcumin, CUR) with cyclodextrin (CD) in the core and polymer (polylactic acid, PLA) in the shell (cCUR/HPβCD-IC-sPLA-NF). CD-IC of CUR and HPβCD was formed at 1:2 molar ratio. The successful formation of core-shell nanofibers was revealed by TEM and CLSM images. cCUR/HPβCD-IC-sPLA-NF released CUR slowly but much more in total than PLA-CUR-NF at pH 1 and pH 7.4 due to the restriction of CUR in the core of nanofibers and solubility improvement shown in phase solubility diagram, respectively. Improved antioxidant activity of cCUR/HPβCD-IC-sPLA-NF in methanol:water (1:1) is related with the solubility enhancement achieved in water based system. The slow reaction of cCUR/HPβCD-IC-sPLA-NF in methanol is associated with the shell inhibiting the quick release of CUR. On the other hand, cCUR/HPβCD-IC-sPLA-NF exhibited slightly higher rate of antioxidant activity than PLA-CUR-NF in methanol:water (1:1) owing to the enhanced solubility. To conclude, slow release of CUR was achieved by core-shell nanofiber structure and inclusion complexation of CUR with HPβCD provides high solubility. Briefly, electrospinning of core-shell nanofibers with CD-IC core could offer slow release of drugs as well as solubility enhancement for hydrophobic drugs.