2. Nanostructured Wound Dressings
- guaranteeing breathability;
- maintaining a suitable physiological temperature;
- ensuring a balanced moist environment, avoiding dehydration and cell death;
- promoting debridement;
- allowing proliferation and migration of fibroblasts and keratinocytes, and an enhanced collagen synthesis;
- protecting the wound from bacteria and other external soiling; and,
3. Cellulose and Its Derivatives
3.2. Cellulose Acetate (CA)
4. Application in Wound Healing: Synergistic Effect with Specialized Biomolecules
4.1. Drug Loading
4.2. Nanoparticles (NPs)
4.3. Natural Extracts
4.4. Wound Healing Alternative Methods Containing Cellulose-Based Compounds
5. Conclusions and Future Perspectives
Conflicts of Interest
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|Black 100% cotton jeans Blue 80/20% cotton/polyester jeans||DMSO||Pretreatment: (1) to dissolve the dyes, HNO3 (0.5–1.0 to 1.5–2.0 M) was used at 50 °C for 20 min.|
Cellulose recovery: (1) PES and other organic contaminants were dissolved in DMSO at 50 °C; (2) the bleaching process resorted to NaClO diluted in HCl for 2 h at 40 °C.
|1.0 and 1.5 M HNO3 were sufficient to dissolve the dyes in 20 min;|
The complete dissolution of PES and other organic contaminants took 6 h for the blue and 10 h for the black samples;
The solvents used were recovered as well as the extracted PES, turning the entire process highly sustainable.
|Black 100% cotton samples|
Blue 80/20% cotton/polyester samples
|Pretreatment: (1) for dye removal various concentrations of HNO3 were applied to the samples at 50 °C; (2) to regenerate the acid from the solution, dyes were absorbed with activated carbon.|
Dissolution and extraction of PES: (1) pre-treated fabrics were exposed to various amounts of DMCHA at 50 °C to dissolve PES; (2) after, filtration was done with CO2 for 1 h to extract the solidified polymer and the solvent was regenerated.
Recovery of cellulose: (1) the portion of cotton resultant from the PES dissolution was washed and dried.
|1.0 M HNO3 applied for 15 min at 50 °C was sufficient for dye removal from the blue sample;|
To remove dye from the black sample HNO3 was used at 1.5 M for 20 min at 50 °C;
100% cotton samples required 10 h for PES and organic contaminants dissolution, while 80/20% cotton/PES needed 6 h;
High purity cotton and PES fibers were recovered from the textile waste.
|Post-consumer cotton waste: white and colored cotton wastes||Alkali/urea aqueous system:|
NaOH/ CH₄N₂O and LiOH/ CH₄N₂O;
|Pretreatment: (1) cotton shirts were cut in small pieces; (2) these were hydrolyzed in H2SO4 and autoclaved at 120 °C for 12 min.|
Wet spinning: (1) dried hydrolyzed cotton was dissolved in two aqueous solutions, LiOH/Urea/dH2O and NaOH/urea/dH2O, at concentrations of 3.25% and 5%.
|Uniform regenerated fibers were obtained with diameters ranging from 23.9 to 33.0 μm;|
A structural shift from cellulose I in the original/hydrolyzed cotton fibers to cellulose II in the regenerated fibers was observed;
A small amount of dye was lost during hydrolysis but no dye leaching was observed during spinning;
The intrinsic color of the regenerated fibers eliminates the need for dyeing processes.
|Waste nylon/cotton blended fabrics (WNCFs)||[AMIM]Cl||Pretreatment: (1) WNCFs were subjected to cutting and shredding processes; (2) the pieces of WNCFs were dewaxed in Soxhlet apparatus with NaOH solution (2 wt.%) for 2 h at 80 °C; (3) dried WNCFs were immersed in boiling water for 2 h, and then dried again at 80 °C in a vacuum oven for 24 h. Cellulose recovery: (1) dried blended fabrics were mixed with IL, at 110 °C under stirring, until complete dissolution of cellulose; (2) the solution was filtered; (3) a cotton cellulose/[AMIM]Cl mixture was obtained; (4) the precipitate was washed with dH2O, and dried at 50 °C for 48 h.||[AMIM]Cl showed to be an effective solvent to extract cellulose from WNCFs;Optimal operation conditions were attained with 3 wt.% waste fabrics and 110 °C for 80 min; |
The crystal structure of cotton cellulose from WNCFs was transformed from cellulose I into cellulose II after separation from nylon 6 by [AMIM]Cl;
The highest yield obtained from the regenerated cellulose films was of ≈ 58%.
|Pretreatment: (1) samples were ground into powder; (2) to attain a DP of ≈ 1000, the powder was treated with 10% NaOH for various time periods; (3) the pretreated substrates were washed with dH2O until neutral pH was reached, and dried in an oven at 60 °C overnight;|
Cellulose recovery: (1) fibers are wet spun at a polymer concentration of 6 wt.% in the binary solvent system of [Bmim]OAc and DMSO at a ratio of 20/80; (2) filaments were extruded through the spinneret into a coagulation bath containing dH2O at RT; (3) the fibers were washed in warm dH2O (60 °C) for 2 h and air dried at RT.
|The addition of an aprotic solvent (DMSO) accelerated dissolution of the cellulosic materials (pre-swelling) while reducing the viscosity of the spinning dope; |
Use of binary solvent system of IL and DMSO at high concentration (1/4) reduces the overall process cost;
The regenerated discolored cellulose fibers had similar morphology and mechanical properties to those of viscose fibers.
|Cotton waste garments (CWG)||NMMO||Pretreatment: (1) CWG or denim were prepared and purified; (2) the purified samples were deconstructed into a pulp; (3) to produce fibers designated by ReCell, both pulps either from cotton waste or wood pulp were combined: ReCell-1, pulp from fabrics washed 50 times with ECE-phosphate based detergent, to mimic the effect of domestic washing cycles; ReCell-2, prepared from a blend of 20% cellulose recovered after purification of treated cotton fabrics (easy care finished cotton fabric was washed 50 times with ECE-phosphate based detergent and subsequently purified in acid-alkali) and 80% wood pulp; ReCell-Denim fibers, pulp from waste denim was washed once with ECE-phosphate based detergent; Lyocell, fibers were produced from purified CWG in NMMO solution without wood pulp;|
Dissolution and fiber spinning: (1) pulp from different fibers was mixed with NMMO at increasing temperatures and under vacuum conditions; (2) the spinning temperature was established at 115 °C.
|The surface of all studied fibers appeared to be smooth;|
Fibers spun from CWG had higher molecular weight than standard lyocell fibers;
ReCell-2 exhibited superior mechanical and molecular properties in relation to the typical fibers regenerated from wood pulp.
|Bleached softwood kraft pulp (BSWK)||Pretreatment: (1) periodate oxidation of BSWK was performed resorting to NaIO4 and NaCl under stirring at RT for 12 h; (2) the modified pulp was filtered and washed three times with dH2O; (3) modified cellulose was dispersed in NaOH solution at temperatures < 0 °C for 10 min under stirring; (4) chitosan was added to the cellulose dispersion at RT and 300 rpm for 30 min to induce the fibers crosslinking;|
Fiber extrusion: (1) the solution was extruded in the form of fibers into a coagulation bath of H2SO4/Na2SO4 at RT; (2) fibers were washed to remove excess of acid.
|The fibers tenacity, in result of chitosan crosslinking, was comparable to that of viscose rayon;|
Crosslinked cellulose fibers become less hydrophilic, a desirable property for high-quality textile applications;
Toxic CS2 were avoided;The entire process is water-based, simple and environmentally friendly, without requiring cellulose purification and removal of hemicellulose.
|White postconsumer textiles (cotton/polyester blend)||[DBNH][OAc]||Pretreatment: (1) cotton/PES samples were shredded and blended to obtain a mixture with a concentration of 50 wt.% cotton and 50 wt.% PES; (2) the samples suffered alkaline washing to remove silicate; (3) cotton/PES blends were submitted to O3 and H2O2 to adjust the viscosity and to bleach the material, respectively; (4) acid washing was performed to remove the metals present;|
Recovery of dry-jet wet spun textile grade cellulose [M] and PES [S] fibers: (1) [M1], [S1], [S2]: cotton/PES blends were mixed with [DBNH] [OAc] for 1h at 80 °C with a concentration of cotton of 6.5 wt.%; (2) [M2]: similar conditions but higher amount of cotton, 10.5 wt.%.
|Spun fibers displayed properties similar to Lyocell, with linear densities between 0.75–2.95 dtex, breaking tenacities of 27–48 cN/tex, and elongations of 7–9%; |
PES undergoes visible degradation once dispersed in [DBNH][OAc], this is evident by the decrease of its MMD and tensile properties.
|Waste fruit peels (WFP)||Isolation of cellulose: (1) different seasonal fruits were used and fruit bran was prepared to extract cellulose; (2) to remove hemicellulose and lignin content an alkali hydrolysis was done with KOH at RT; (3) samples were bleached in NaClO2 at 70 °C for 1 h; (4) to disintegrate fibrils and form finest cellulose an acid hydrolysis was done with H2SO4 at 80 °C for 1 h; (5) at each step the suspension was neutralized, washed and centrifuged.||A photocatalyst cellulose/MoS2 was developed by in situ hydrothermal approach with high photocatalytic activity;|
Increase in photodegradation efficacy results from the existence of cellulose as support for MoS2, which causes a delay in the recombination of photo-generated charge carriers.
|Empty fruit brunch (EFB)||LTTMs: mixture of L-malic acid-sucrose-dH2O at molar ratio of 2/4/2 (w/w/w) or mixture of cactus malic acid-sucrose-dH2O at molar ratio of 2/4/5 (w/w/w)||Delignification of EFB: (1) the EFB was pretreated with LTTMs in a ratio of 1/20 (w/w) at 80 °C for 6 h in an oil bath with magnetic stirring; (2) cellulose fibers were washed with dH2O for the precipitation of lignin; (3) the precipitated lignin and cellulose fibers were separated by filtration and then dried.||The EFB recovered cellulose fibers using cactus malic acid-LTTMs showed the lowest lignin content;|
LTTMs-delignified EFB displays a great potential for producing specialty papers for pulp and paper industries.
|Raw material||Solvents||Catalyst||Acetylating Agent||Methods||Observations||Ref.|
|Waste cotton fabrics (WCFs)||[Hmim]HSO4||(CH3CO)2O||Pretreatment: (1) WCFs were cut and shredded, and used without further purification or bleaching;|
Acetylation: (1) WCFs, (CH3CO)2O and 0.1–0.4 molar equivalents of ionic liquids (ILs) were mixed and heated at 100 °C for 1–5 h; (2) the mixture was poured into ethanol and stirred for 30 min; (3) the solid consisting of CA and unreacted cellulose was filtered and washed with ethanol three times and then dried at 60 °C for 24 h; (4) the sample was then refluxed for 24 h by the Soxhlet extraction method using dH2O; (5) the filtrate was dried in a vacuum oven at 60 °C for 24 h to obtain the water-soluble CA.
|There is no water-soluble CA without an ILs catalyst;|
Conversion of water-soluble CA increases significantly with the increase content of ILs in a 1 h reaction time;
Conversion of water-soluble CA decreases with ILs amount when the reaction time is 2, 3, 4 and 5 h. This relates to the increase of DS values and, consequent, decrease in solubility;
Highest conversion was obtained with 0.2 molar equivalents of ILs in a 3 h reaction.
Cotton seed hull
|Iodine||(CH3CO)2O||Pretreatment: (1) samples were pulverized with a hammer mill; (2) scouring step: samples were suspended in 6% solution of NaOH, heated in a water bath for 35 min, filtered, and washed with water at 95 °C; (3) bleaching step: the material was suspended in a NaOH solution at pH 12.0 with 1.5% H2O2 for 1 h, in 95 °C water bath; (4) water and caustic were removed by filtration and the pH was adjusted to 7.0; (5) the resulting powder was dried at 40 °C overnight.|
Acetylation: (1) samples, (CH3CO)2O and iodine were heated at 80–100 °C for 20–24 h; (2) the mixture was cooled to RT and treated with a saturated solution of Na2S2O3, while stirring; (3) the mixture was poured into ethanol and stirred for 30 min; (4) the solid, which contained CA, was filtered, washed and dried at 60 °C; (5) CA was dissolved in CH2Cl2 and filtered; (6) the filtrate was evaporated under vacuum at RT.
|The process was optimized by varying the temperature and the amounts of (CH3CO)2O and iodine; |
The best yields obtained were of 15–24%, which corresponded to a conversion of 50–80% of the starting cellulose.
|Rice straw (RS)||H3PW12O40||(CH3CO)2O||Pretreatment: (1) RS was cut and washed, dried and crushed into powder by a grinder; (2) powder was Soxhlet extracted using a toluene-ethanol mixture for 24 h to remove wax, pigments and oils, followed by drying; (3) the dewaxed powder was stirred in KOH solution with H2O2; (4) the mixture was then cooled to RT, filtered and washed until the filtrate became neutral, and finally dried.|
Acetylation: (1) samples, CH3COOH, (CH3CO)2O, CH2Cl2, and H3PW12O40 were mixed; (2) the mixture was refluxed; (3) the mixture was filtered and the residue collected; (4) acetone was added, the material was filtered and the filtrate was evaporated after stirring; (5) the solid was dried overnight at 80 °C.
|83 wt.% content of cellulose was obtained after pretreatment with 4% KOH and immersion in CH3COOH for 5 h; |
Acetone-soluble CA with DS values around 2.2 were obtained by changing the amount of H3PW12O40 and the acetylation time.
|Green landscaping waste (GLW)||CH3COOH||H2SO4||(CH3CO)2O||Pretreatment: (1) GLWs and H3PO4 solution were loaded into a reactor at 150 °C for 15 min and under stirring to carry out the hydrolysis process; (2) the final product was filtered.|
Acetylation: (1) CH3COOH, (CH3CO)2O and H2SO4 were mixed with GLWs; (2) the mixture was heated to 60 °C under stirring; (3) the reacted mixture was cooled to RT, filtered and evaporated to recover CA; (4) CA was dried at 80 °C for 12 h.
|Diluted H3PO4 disrupted the crystalline structure of cellulose and increased the amorphous region, rendering the cellulose more accessible to (CH3CO)2O, leading to a more effective acylation; |
Acetylation of pinewood without pretreatment registered an 8.3% yield of CA (low);
High acetylation levels were obtained with pretreatment at 150 °C, 1.8 h, 8 mL/g, 100 mL, 1.67 wt.% of H3PO4 in solution, and 150 rpm.
|Microcrystalline cellulose (MCC) Cotton linter pulp |
Wheat straw pulp Bamboo pulp
Bleached softwood sulfite dissolving pulp
Bleached hardwood kraft pulp (HP)
|DMSO||NaOH||C4H6O2||Pretreatment: delignification with NaClO2 and KOH;|
Acetylation (transesterification): (1) cellulose was dissolved in DMSO; (2) NaOH was added dropwise to activate the -OH groups; (3) C4H6O2 was poured into the mixture under stirring for 15 min to obtain CA.
|Cellulose was esterified within 15 min;|
CA-MCC solution displayed the lowest viscosity, while the CA-HP solution had the highest values, showing also higher DPs, which hindered the DS;
DS values for all CA samples were above 2.52, confirming a successful synthesis;
- Most of the obtained fibers were triacetate fibers with DS higher than 2.75;
CA fibers with high DPs exhibited the lowest DS;
The yields of the obtained subtracts were: CA-MCC 89.21%, CA-CP 84.75%, CA-WP 72.38%, CA-BP 68.83%, CA-SP 66.28%, and CA-HP 58.59%.
|Babassu coconut shells (BCS)||CH3COOH||H2SO4||(CH3CO)2O||Pretreatment (organosolv process): (1) pretreatment of endocarp of BCS; (2) reaction of raw material with 80% ethanol/20% HNO3 v/v for 3 h under reflux (at ≈ 100 °C); (3) reaction with NaOH for 1 h at RT; (4) obtained samples were washed to reach pH 7.0. |
Acetylation: (1) CH3COOH was added to the obtained cellulose (30 m at RT); (2) H2SO4 was added and stirred for 25 min, followed by the addition of (CH3CO)2O which was stirred for the same time; (3) stirring for 24 h at RT; (4) water was added to stop the reaction, the precipitated CA was filtered and washed with dH2O; (5) neutralization with 10% Na2CO3 (pH 7.0); (6) CA was washed for 2 days using dialysis tubing (water replaced every 6 h) and dried at 90 °C for 4 h.
|The organosolv extraction was rapid, effective (with yields of 70–95%) and eco-friendly;The yield of the acetylation reaction was estimated in 76%;|
The CA DS was determined at 2.63 ± 0.01.
|Sugarcane straw (SCS)||Glacial CH3COOH||H2SO4||(CH3CO)2O||Pretreatment: (1) (acid) SCS was treated with H2SO4 (10% v/v) at 100 °C for 1 h; (2) (alkaline) SCS was treated with NaOH (5% w/v) at 100°C for 1 h; (3) (chelating) SCS was treated with 0.5% C10H16N2O8 for 30 min at 70 °C; (4) (bleaching) SCS was treated with 5% (v/v) H2O2 and 0.1% MgSO4.|
Acetylation: (1) CH3COOH was added to SCS cellulose and stirred at 37.8 °C for 1 h; (2) glacial CH3COOH and H2SO4 were added to the mixture for 45 min; (3) (CH3CO)2O and H2SO4 were added after the mixture was cooled to 18.3 °C; (4) the temperature was increased to 35 °C and the mixture was stirred for 1.5 h; (5) water and glacial CH3COOH were added and stirred for 1 h; (6) the material obtained was washed with dH2O until reaching pH 7.0.
|Cellulose with 90% purity was obtained;|
CA presented a DS of 2.72 ± 0.19 and a percentage of acetyl groups of 41.05 ± 2.77%, characteristic of a triacetate.
|Sorghum straw (SS)||CH3COOH||H2SO4||(CH3CO)2O||Pretreatment (extraction): different cooking times (1.5–2.5 h) and alkali solutions (NaOH) (0.75–1.25% w/v) were applied at a ratio of 1/20 (w/v) of SS/NaOH at 90 °C; (2) samples were washed several times with dH2O until NaOH was completely removed, followed by drying at 50 °C for 12 h in oven; (3) (bleaching) SS acetate buffer (pH 4.5) and 2 wt.% NaClO2 were combined at 80 °C for 0–35 min and 20–25 mL; (4) samples were dried at 50 °C for 12 h.|
Acetylation: time ranged from 6 to 16 h; (1) bleached pulp was added to CH3COOH solution; (2) after 30 min, H2SO4 and (CH3CO)2O were added and stirred for 25 min; (3) (CH3CO)2O was added to the mixture and stirred for 30 min; (4) the mixture was left to rest for 6, 7, 8, 9, 10, 11, 13, 15 and 16 h, at 25 °C; (5) CA was precipitated in water and filtered; (6) the material was washed to remove the excess of CH3COOH.
|CA with the highest DS was obtained by acetylating cellulose with (CH3CO)2O for 16 h at RT;|
CA reached a DS of 2.6–2.7.
|Microfibrillated date seeds cellulose||CH3COOH||H2SO4||(CH3CO)2O||Acetylation: (1) (swelling) seeds were mixed with CH3COOH at RT for 2 h; (2) the mixture was poured in a cooled solution of (CH3CO)2O, CH3COOH and H2SO4; (3) dH2O was poured to the reaction at constant stirring to precipitate CA; (4) the residue was washed with dH2O until neutral pH was reached; (5) the obtained material was dried in an air oven at 50 °C.||A yield of 79% was obtained for cellulose triacetate.|||
Treated sisal (mercerized)
Mercerized cotton linters
|DMAc/LiCl||(CH3CO)2O||Pretreatment (mercerization): (1) samples were mercerized in 20% NaOH solution at 0 °C for 1 h; (2) alkali-swollen material was washed in dH2O until a constant pH was reached. |
Acetylation: (1) cellulose and DMAc were mixed, heated at 150 °C and stirred for 1 h; (2) LiCl was added and the mixture was heated to 170 °C; (3) (CH3CO)2O was added dropwise at 110 °C for 1 or 4 h; (4) precipitation was induced with CH3OH followed by purification via Soxhlet extraction and drying at 50 °C.
|LiCl did not influence the DS but affected aggregation during filtration; |
High LiCl content induced separation of the cellulose chains, which in turn reduced aggregation;
Mercerized products reached higher DS values than untreated samples.
|Waste polyester/cotton blended fabrics (WBFs)||[Hmim]HSO4||(CH3CO)2O||Pretreatment: (1) WBFs were cut and shredded. |
Acetylation: (1) (CH3CO)2O and [Hmim]HSO4 were added to WBFs powders at 100 °C for 12 h; (2) the mixture was poured into ethanol; (3) the solid, which consisted of CA and PET was filtered, washed and dried; (4) to extract acetone-soluble CA, part of the sample was refluxed using acetone; (5) the filtrate was dried and refluxed using DMF.
|[Hmim]HSO4 at 0.4 molar equivalents of IL was the most acetone-soluble formulation;|
The extraction yield of acetone-soluble CA was 49.3%, which corresponded to a conversion of 84.5% of WBFs original cellulose;
96.2% of the original PET were recovered.
|CH3COOH||H2SO4||(CH3CO)2O||Pretreatment (purification): (1) the material was mixed with NaOH at RT for 18 h; (2) the mixture was filtered and washed with dH2O; (3) the material was refluxed in a HNO3/ethanol solution at 20% v/v for 3 h (solution changed every hour); (4) the bagasse was washed with dH2O and oven dried at 105 °C for 3 h;|
Acetylation: (1) SB was mixed with CH3COOH and stirred for 30 min; (2) H2SO4 and CH3COOH were added to the system; (3) the mixture was filtered and (CH3CO)2O was added; (4) the solution was returned to the bagasse container and stirred for 30 min; (5) the mixture stood at 28 °C and dH2O was added to stop the reaction and precipitate CA; (6) CA was washed in dH2O and dried at RT overnight.
|After sugarcane bagasse purification, 75% of α-cellulose was attained; |
The CA viscosity-average molecular weight increased from 5.5 × 103 to 55.5 × 103 g/mol.
|Commercial cellulose||DMSO/TBAF||CDI||C11H16O2, CH3COOH, C18H36O2, and C5H4O3||Acetylation: (1) esterification of cellulose using carboxylic acids, activated in situ with CDI; (2) 15 min at RT was enough to obtain a clear solution.||Cellulose esters were prepared with DS values up to 1.9, without any required pretreatment;|
Esterification with C11H16O2, and C5H4O3 was the most effective.
|Type||Raw material||Main Agent||Methods||Observations||Ref.|
|CNF||Wheat straw (WS)|
Waste wheat straw (WWS)
|p-TsOH||Fractionation of WS and WWS using p-TsOH: (1) WS or WWS were added to the concentrated acid solution at continuous stirring; (2) after, it was filtered.|
Mechanical fibrillation: (1) two hydrolyzed fiber samples were mechanically fibrillated to produce LCNF.
Alkaline peroxide post-treatment: (1) bleaching was conducted at 60 °C by adding the obtained LCNF suspension to a H2O2 solution (stirring); (2) the pH of the suspension was adjusted to 11.5 with 4 M NaOH; (3) the resultant purified LCNF (P-LCNF) was dialyzed using dH2O until the pH was constant.
|Alkaline peroxide post-treatment was further conducted to obtain purified lignocellulosic nanofibrils (P-LCNF) with low lignin content and thin diameters;|
The low-temperature fractionation process on WS and WWS fibers could yield cellulose nanomaterials with potential value-added for a variety of applications and uncover a new efficient processing tool for agricultural wastes.
|Arecanut husk (AH)||HCl, NaOH||Isolation of cellulose nanofibrils: (1) the dried AH fibers were dewaxed with a mixture of toluene and ethanol for 48 h at 50 °C, followed by washing with boiling water and dried in air; (2) the dried fibers were then cut; (3) to remove lignin and hemicelluloses, a treatment with NaOH was applied at 50 °C for 4 h; (4) samples were washed to remove the alkali compounds and treated with HCl to break the cell walls and separate the microfibrils; (5) fibers were washed with dH2O to eliminate any acid traces; (6) fibers were grinded into a pulp form and treated again with alkali to remove the remaining non-cellulosic components, followed by acid hydrolysis; (7) the delignification was further carried out by bleaching with NaClO2 and glacial acetic acid for 2 h at 60 °C.||Highly crystalline and thermally stable cellulose nanofibrils, with very high aspect ratio, were prepared from AH fibers by HCl hydrolysis followed by mechanical fibrillation.|||
|Softwood sulfite pulp (SSP) |
Wheat straw (WSP1)
Refined fibrous wheat straw cellulose suspension (WSP2)
Refined beech wood (BWP1)
Refined fibrous beech wood pulp suspension (BWP2)
|Mechanical pretreatment: (1) SSP, WSP1 and WSP2 were milled; |
Mechanical high-shear disintegration: (1) mechanical treatment under high pressure was performed to separate the nanofibrillated cellulose from the suspensions.
|The homogeneity of the NFC material was determined as more important for its reinforcement potential than the DP.|||
|Waste jute bags (WJB)||Toluene/ethanol, NaOH, C2H6O, H2O2, HCl||Pretreatment (isolation of lignin and cellulose nanofibrils): (1) the WJB were chopped into small pieces, washed and dried; (2) the samples were dewaxed in a soxhlet apparatus using toluene/ethanol; |
Lignin and cellulose removal: (1) the pretreated jute fibers were subjected to soda cooking at high temperatures; (2) temperature was reduced to separate the fibers; (3) to precipitate lignin the pH was lowered and the samples filtered; (4) the mixture was subjected to C2H6O solution to increase its purity by dissolving the hemicellulose; (5) jute fibers pulp were bleached with H2O2 and the residual lignin dissolved; (6) bleached pulp was hydrolyzed with HCl resulting in defibrillation of the cellulose.
|It was possible to isolate cellulose nanofibrils and extract lignin by discarding the hemicellulose using a soda cooking pretreatment followed by fiber defibrillation by acidic hydrolysis.|||
|CNCs||Waste polyester/cotton blended fabrics (WBFs)||H3PW12O40||Separation treatment: (1) the WBFs were mixed with H3PW12O40 aqueous solution and heated to 120–170 °C for 3–8 h; (2) the solution was filtered and MCC were oven-dried in a vacuum oven at 60 °C for 6 h, and stored for further processing.||The optimal conditions for the separation treatment were determined as follows: 3.47 mmol/L of HPW concentration, solid/liquid ratio of 1/20, reaction temperature of 140 °C, and reaction time of 6 h;|
The yields of MCC and PES were 85.12% and 99.77%, respectively.
|Pineapple leaf (PL)||H2SO4||Pretreatment: (1) raw PL was ground; (2) the powder was treated with a NaOH aqueous solution for 4 h at 100 °C; (3) samples were bleached in acetate buffer and NaClO2 at 80 °C for 4 h;|
Isolation of cellulose nanocrystals: (1) treated PL was milled with a blender; (2) the samples were submitted to hydrolysis at 45 °C for 5 min in H2SO4; (3) the resulting suspension was ultrasonicated for 10 min and stored at 4 °C.
|The most successful extraction of high crystalline cellulose was attained with a hydrolysis process of 30 min.|||
|Seaweed||H2SO4C6H11ClN2||Pretreatment: (1) the powdered seaweed samples were treated with NaOH under microwave irradiation for 30 min at 360 W; (2) to ensure complete delignification, the alkali-pretreated sample was bleached using H2O2 for 4 h at 55 °C; (3) the bleached sample was subjected to hydrolysis using H2SO4 and C6H11ClN2 for 30 min at 95 °C to remove the amorphous parts of the sample.||CNCs can be successfully isolated from Gelidiella aceroso via microwave irradiation, which is an alternative energy source for alkali treatment.|||
|Groundnut shells (GNS)||H2SO4||Pretreatment: (1) GNS were cleaned by washing in dH2O, dried and milled; (2) powdered shells were submitted to soxhlet extraction for 8 h using benzene/methanol; (3) the dewaxed shells were bleached with NaClO2 to remove lignin at 70 °C for 2 h, and then filtered; (4) the holocellulose obtained was treated with 1 M NaOH solution at 65 °C for 2 h to remove hemicelluloses; (5) the extracted product was dried for 24 h at 100 °C;|
Isolation of cellulose nanocrystals: (1) a certain amount of cellulose was treated with H2SO4 for 75 min at 45 °C; (2) in the end the samples were washed.
|CNCs were successfully isolated from groundnut shells, after purification and acid hydrolysis treatment, reaching a yield of 12%.|||
|BC||Undyed cotton-based textile wastes||[AMIM]Cl||Pretreatment: (1) the waste cotton was cut into small pieces; (2) these were added to an IL solution at 90, 110 or 130 °C; (3) dH2O was used as an anti-solvent for regenerated cellulose;|
Enzymatic hydrolysis: (1) cellulose regenerated and untreated cotton were immersed in citrate buffer containing cellulase and incubated at 50 °C; (2) the amount of IL affecting the polymer yield was analyzed.
|Pretreatment with [AMIM]Cl is very efficient in increasing the hydrolytic rate of cotton cloth, since after 4 h the yields of the reduced sugar from pretreated and untreated cotton cloth were 22.4% and 4.0%, respectively;|
Higher BC yields (40–65%) were obtained in cotton enzymatic hydrolysate cultures;
BC production decreased at IL concentration of 0.001 g/mL.
|Potato peel waste (PPW)||HNO3; H2SO4; HCl; H3PO4||Production of PPW acid hydrolysate: (1) PPW was added to solutions of HNO3, H2SO4, HCl and H3PO4 at 100 °C for 2, 3, 4 and 6 h; (2) the pH of each mixture was neutralized to 6 with 1 M NaOH; |
PPW as alternative media for BC production: five factors were tested to optimize BC production, initial pH (7–11), media volume (mL), inoculum size (4–12%), temperature (25–45 °C), and incubation time (2–6 days);
BC purification: (1) the produced BC was collected, rinsed in dH2O, and immersed in 1 N NaOH at 60 °C for 90 min to remove attached cells and impurities; (2) pellicles were rinsed with methanol, washed with the dH2O and dried at 60 °C for 24 h.
|Maximum BC yield was achieved using PPW-nitric acid hydrolysate at 2.61 g/L followed by PPW-sulfuric acid hydrolysate at 2.18 g/L;|
Optimal BC production conditions were determined as pH 9 with 8% inoculum size and volume of 55 mL, at 35 °C and incubation of 6 days.
|Wheat straw (WS)||[AMIM]Cl||Pretreatment: (1) WS was mixed with IL; (2) the mixture was heated from 90 to 120 °C and incubated for different times under 500 rpm; (3) dH2O was added to straw/IL solution to regenerate the straw; |
Enzymatic hydrolysis: (1) WS regenerated was placed in acetate buffer (pH 5.0) containing cellulase and was incubated at 50 °C at 80 rpm.
|The hydrolytic efficiency of regenerated straw increased compared to untreated materials;|
The yield of the straw was 71.2% after pretreatment in [AMIM]Cl at 110 °C for 1.5 h, with a 3 wt.% straw dosage, which was 3.6 times higher than that of untreated straw (19.6%);
BC yield obtained from straw hydrolysates was higher than that from glucose-based media.
|Kitchen waste (KW)||α-amylase;|
|Pretreatment: (1) samples were subjected to a washing process using tap water to separate the KW into solid fraction (starch-rich solid) and liquid fraction (oil/water mixture); (2) the solid fraction was sterilized at 121 °C for 15 min;|
Enzymatic saccharification of the solid fraction: (1) samples were hydrolyzed using α-amylase and amylglucosidase at 55 °C for 24 h, at 150 rpm;
BC production: (1) the glucose concentration of the resultant hydrolysate was diluted to 50 g/L; (2) then 5 g/L peptone, 5 g/L yeast extract, 1.15 g/L citric acid and 2.7 g/L disodium hydrogen phosphate were added to prepare the BC production media; (3) the seed culture was incubated at 30 °C and 150 rpm for 2 days; (4) 10 mL of the cultured seed were inoculated in 100 mL of production media (pH of 5.0), which was cultivated at 30 °C under static conditions for 15 days; (5) at 1, 4, 8, 12 and 15 days the concentrations of glucose and glycerol were measured.
|The washing with dH2O during pretreatment removed oil and NaCl from samples, increasing the BC yield.|||
|Cellulose||Tetracycline hydrochloride (TH)|
Donepezil hydrochloride (DNP)
|Silver NPs (AgNPs)|
Zinc oxide NPs (ZnONPs)
Ferulic acid (FA)
Silver salt of sulfadiazine (SSD)
|Cinnamon (CN); Lemongrass (LG);|
|BC||Soy protein particles|
Graphene oxide (GO)
|Tragacanth gum (TG)||[190,191,192]|
|Drugs||Polymer(s) and solvent(s)||Processing conditions||Observations||Ref.|
|TH||3% w/v of TCMC in DMF;|
1% w/v of PEO in CHCl₃
|Single nozzle and core-shell electrospinning;|
Graft copolymerization: NaCMC was grafted with MA originating NaCMC-co-MA copolymer (TCMC);
Single nozzle: 5% w/w TH (in relation to methanol concentration) was added to TCMC/PEO and processed at 15 kV, distance of 20 cm and feed rate of 3 mL/h;
Core-shell: TCMC was used at the shell and 5% w/w TH/PEO was used at the core, fibers were produced using potential of 15 kV, distance of 18 cm and feed rate of 0.4 mL/h.
|Fibers produced from polymer blend were more uniform and bead free than those generated from core-shell;|
The TH release profile in core-shell nanofibers was more efficient, with an initial burst release of only 26% (first 30 min), and a 92% released within 72 h;
TH-loaded TCMC/PEO core-shell nanofibers revealed excellent antibacterial effects against Gram-positive bacteria.
|CIF||13% w/v of EC or PVP in HFIP||Single nozzle electrospinning;|
5% and 15% w/w of CIF (with respect to the polymer concentration) was added to PVP and to EC;
Fibers were produced using potential of 20 kV, distance of 16 cm and a feed rate of 0.8 mL/h. Fibers were collected from an aluminum foil and from a gauze covering the foil.
The following samples were produced:
S1: control with PVP; S2: PVP/CIF (5%) in foil; S2G: PVP/CIF (5%) in gauze; S3: PVP/CIF (15%) in foil; S3G: PVP/CIF (15%) in gauze; S4: control of EC; S5: EC/CIF (5%) in foil; S5G: EC/CIF (5%) in gauze; S6: EC/CIF (15%) in foil; S6G: EC/CIF (15%) in gauze.
|Neat PVP fibers generated the largest diameters (832 ± 241 nm), which decreased after CIF addition; |
Neat EC fibers displayed diameters of 597 ± 214 nm; while S5 and S6 attained diameters of 435 ± 137 nm and 368 ± 108 nm, respectively;
Drug release was slower on EC than on PVP fibers;
After 480 min, both sets of fibers had released 90% of their CIF loading;
Samples showed no toxicity towards cells;
Inhibition zones of the CIF-loaded PVP fibers (S2 and S3) for E. coli and S. aureus after 24 h contact were 5.30–5.71 cm and for CIF-loaded EC fibers were 4.29–4.72 cm.
|DNP||12.5% w/v of PU in DMF; |
1.2, 2.5, 5.0, and 10.0% w/v of HPC in DMF
|Single nozzle electrospinning;|
PU was blended with various concentrations of HPC and DNP at 1.25% w/v (RT);
Fibers were produced using potential of 15 kV, distance of 15 cm and a feed rates of 1.0 mL/h.
|Mats presented a uniform, non-beaded, and smooth morphology, with diameters ranging from 464 ± 24 to 995 ± 14 nm;|
PU/HPC/DNP mats portrayed generally smooth nanofibers, with the exception of ratios 10/4/1 and 10/8/1 which displayed some beads;
Nanofibers composed of PU/HPC/DNP at ratios 10/0/1, 10/1/1, 10/2/1, and 10/4/1 revealed an initial burst release of 66, 66, 61, and 71%, respectively;
The total amount of DNP on the fibers ranged 85–90%;In vitro cytotoxicity analysis indicated that PU/HPC mats were well tolerated by the skin and the DNP was not irritant.
|TH||18% w/w CA in acetone/ DMAc at 2/1 v/v;|
10% w/w PCL in DMF/ THF at 1/1 v/v;
CA/PCL were mixed at 1/1, 2/1 and 3/1 v/v;
1% w/w dextran was added to CA/PCL
|Single nozzle electrospinning;|
1% w/w THC was added to CA/PCL/dextran;
Fibers were produced using potential of 15 kV, distance of 15 cm and feed rate of 1.0 mL/h.
|Fiber diameters varied from 0.28 to 2.20 µm;|
The CA/PCL/Dextran/THF were very smooth;
Higher amounts of PCL produced more uniform fibers;
Fibers modified with dextran were dense, uniform and revealed smaller diameters;
THC loaded nanofibers were very biocompatibility, accelerating 3T3 fibroblasts proliferation and differentiation;
Drug loaded mats were effective against S. aureus and E. coli bacteria.
|FA||Core: 16% w/v of gliadin in HFIP/TFA at 8/2 v/v;|
Middle layer: 6% w/v CA in acetone/acetic acid at 2/1 v/v;
Outer layer: acetone and acetate acid at 2/1 v/v
FA: 4% w/v in 8/2 v/v HFIP/TFA and mixture with the 16% w/v gliadin (core);
Four different fibers were produced using potential of 15 kV, distance of 20 cm and feed rates of 0.3 outer, 0.1–0.5 middle and 2 inner.
|Fibers were linear, cylindrical and with a smooth surface;|
As feed rates increased diameters decreased and the sheath thickness decreased;
Thicker CA coatings increased the release time;
The sheath prevented the initial burst release;
After the first hour, continued drug release was still observed.
|IBU||Core: 16% w/v of gliadin in HFIP/TFA at 8/2 v/v;|
Middle layer: 0, 1, 3 and 5% w/v CA in acetone/acetic acid at 2/1 v/v;
Outer layer: acetone and acetate acid at 2/1 v/v
IBU: 4% w/v in 8/2 v/v HFIP/TFA and mixture with the 16% w/v gliadin (core);
Four different fibers were produced using potential of 15 kV, distance of 20 cm and feed rates of 0.3 outer, 0.3 middle and 2 inner.
|Fibers were linear, cylindrical and with a smooth surface;|
Diameters increased with the increased content of CA in the middle layer: 540 (0%), 660 (1%), 720 (3%), and 870 (5%) nm;
Higher CA concentrations also increased the sheath thickness to 1.82 (1%), 5.85 (3%), and 11.60 (5%) nm;
Time for IBU complete release increases with the fiber sheath thickness;
In the first hour, release of IBU was determined at 34.2 ± 4.5% (0%), 8.3 ± 4.6% (1%), 5.4 ± 4.1% (3%), and 2.7 ± 3.1% (5%).
|KET||Core and Sheath: 11% w/v CA in acetone/DMAc/ethanol at 4/1/1 v/v||Coaxial electrospinning;|
KET: 2% w/v (in relation to the polymers mass) was mixture with 11% w/v CA;
Fibers were produced using potential of 15 kV, distance of 15 cm and a feed rate at the core of 1.0 mL/h and at the sheath at 0.0, 0.2 and 0.4 mL/h.
|As the feed rate at the sheath increased the diameters decreased and the fibers became smoother and uniform;|
Fiber produced with a 0.2 mL/h feeding rate averaged 240 nm and were capable of sustaining a more controlled release profile of KET.
|Amoxicillin||8% w/v CA in acetone/water at 80/20 v/v|
8% w/v PVP in ethanol/water at 85/15 v/v.
Two different nanofibers were produced: CA/PVP/CA: PVP-core and PVP/CA/PVP: CA-core;
Fibers were produced using potential of 15 kV, distance of 15 cm and a feed rates between 0.3 and 1.0 mL/h;
After electrospinning, dried rectangular-shaped samples were immersed in a 1 M aqueous solution of amoxicillin for 90 min.
|CA/PVP/CA after being washed in water showed the existence of cylindrical fibers;|
PVP/CA/PVP washed with water showed lower diameters (due to dissolution of PVP);
Fibers diameters ranged from 0.5 to 2.0 μm;
Young’s Modulus and the strain at break of CA/PVP/CA are slightly higher than PVP/CA/PVA;
Drug release kinetics was dependent on the media pH;
Time release of amoxicillin was of ≈ 15 days and was accelerated at basic pHs (pH = 7.2).
|TQ||6% w/v PLA/CA in DCM/DMF at 7/3 v/v, at ratios 9/1 and 7/3 w/w||Single nozzle electrospinning;|
3% w/w TQ (in relation to the polymers mass) was mixture with PLA/CA;
Fibers were produced using potentials of 20–24 kV and feed rates of 1.5–3.0 mL/h.
|Fiber diameters reduced with increased CA content;|
Presence of TQ reduced even more the diameters;
7/3 PLA/CA loaded with TQ revealed the most porous structure, with an initial burst of TQ that lasted 24 h, followed by a more sustained release of the drug for 9 successive days;
7/3 PLA/CA loaded with TQ promoted the most fibroblasts proliferation and collagen deposition and was the most effective against bacteria.
|SSD||24% w/w CA in DMF/acetone at 6/4 v/v||Single nozzle electrospinning;|
SSD was mixed with CA solution at 0.125, 0.25, 0.37 and 0.50% w/w;
Fibers were produced using potential of 12 kV and distance of 15 cm.
|SSD was uniformly distributed along the fibers;|
The average fiber diameters decreased with the increasing loading of SSD, from ≈ 292 nm to ≈ 286 nm;
0.5% w/w SSD was the most effective concentration against bacteria.
|TH||10% w/v PHBV in chloroform/DMF at 9/1 w/w||Single nozzle electrospinning;|
1, 3, 6, 9 and 10% w/w CNCs were added to the PHBV solution;
5, 15, and 25% w/w TH were added to the PHBV/CNCs solutions;
Fibers were produced using potential of 15 kV with a distance of 18 cm and a feed rate of 1.0 mL/h (during 6 h).
|Addition of 3 to 6% w/w CNCs to the PHBV nanofibers (1025 ± 96 nm) decreased the fibers from 748 ± 62 to 620 ± 33 nm, respectively;|
The tensile strength and Young’s modulus increased with the increased CNCs content, and reached a maximum with 6% w/w CNCs;
The higher CNCs content improved the hydrophilicity of PHBV nanocomposite;
The percentage of drug loaded and the loading efficiency were 25.0 and 98.8%, respectively (≈ 86% HF was delivered within 540 h for nanofibrous containing 6% w/w CNCs).
|16% w/w PCL in acetic acid/dH2O 90/10 v/v||Single nozzle electrospinning;|
Synthesis of CNC: (1) high molecular weight cellulose was extracted from cotton waste; (2) cellulose was hydrolyzed in H2SO4;
1% w/w TH was dissolved in 90% acetic acid;
0, 0.5, 1.0, 1.5, 2.5, 4% CNCs were added to the TH solution and then mixed with PCL;
Fibers were produced using potential of 17 kV with a distance of 16 cm and a feed rate of 0.9 mL/h.
|The lowest fiber diameters were obtained with 4% CNCs; |
The highest tensile stress was obtained was with 1.5% CNCs;
During biodegradation studies the weight loss of CNCs-incorporated samples was much higher than for pure PCL nanofibers;
Drug release was slower with increasing amounts of CNCs in the PCL nanofibers.
|10% w/w PLA in chloroform/DMF at 9/1 w/w||Single nozzle electrospinning;|
Synthesis of CNC: MCC was hydrolyzed in H2SO4;
PEG/CNCs were mixed at 1/1;
PLA was mixed with PEG/CNCs at 1–10% w/w;
3, 10, 15, 20 and 30% w/w TH were added to the polymeric blend;
Fibers were produced using potential of 18 kV with a distance of 15 cm and a feed rate of 1 mL/h.
|The diameter of the PLA nanofibers was 2.5 ± 0.1 µm and decreased to 1.2 ± 0.1 µm with the addition of 10% w/w PEG/CNCs; |
Increased drug loading reduced the fibers diameters;
The water contact angle was significantly reduced with the incorporation of 10% w/w PEG/CNCs;
Composite nanofibers containing 15–30% TH delivered more than 95.7% of their content within 1032 h, while neat PLA nanofibers only released 13% of the drug;
Composite nanofibers showed good biocompatibility with MG63 cells.
|Nanoparticles||Polymer(s) and solvent(s)||Processing conditions||Results||Ref.|
|AgNPs||4% w/v CMC and 4% PEO w/v in water||Single nozzle electrospinning;|
Fibers were produced using potential of 22 kV, with distance of 15 cm and feed rate of 2 mL/h;
After, electrospinning CMC/PEO mats were carefully immersed in AgNO3 solution (0.1 mol/L, to substitute Na+ with Ag+) and irradiated with UV-light.
|The average diameter of CMC/AgNPs fibers (89 ± 23 nm) was smaller than that of CMC/PEO fibers (103 ± 30 nm);|
CMC/AgNPs nanofiber mats were 100% effective against S. aureus and E. coli.
|17% w/w CA in DMF/acetone at 1/2 v/v||Single nozzle electrospinning;|
Cellulose nanofibers were prepared from CA nanofibrous mats by a simple alkaline treatment with NaOH and coated with silver by immersion in AgNO3, forming CEAgNP;
Fibers were produced using potential of 15 kV, with distance of 15 cm and feed rate of 0.06 mL/h.
|CA nanofibers showed a smooth and regular morphology with an average diameter of 291 nm, and cellulose displayed diameters averaging 289 nm;|
All CEAgNP samples were 100% bactericidal, being effective in preventing growth of E. coli and S. aureus strains.
|ZnO NPs||2% w/v CMC and 10% w/v PVA/dH2O||Single nozzle electrospinning;|
1/1 w/w PVA/CMC was combined with 3% w/w of ZnO NPs (relative to PVA/CMC blend) and then with EM at 5% w/w (relative to PVA/CMC blend) and mixed until a homogenous mixture was obtained;
Fibers were produced using potential of 16 kV, with distance of 20 cm and feed rate of 0.3 mL/h;
- Crosslinking was performed with 2% glutaraldehyde vapor in a desiccator for 48 h and then dipped in 3% AlCl3 in ethanol.
|PVA/CMC nanofibers ranged 214.5 ± 26.0 nm, while PVA/CMC/EM averaged 238.9 ± 18.0 nm;|
The average size of the fibers was determined in 193.5 ± 20.0 nm and 234.9 ± 28.0 nm for PVA/CMC/ZnO and EM-loaded PVA/CMC/ZnO nanocomposites, respectively;
The PVA/CMC/EM nanofibrous mat showed a high initial burst release of EM (58%)
Incorporation of 3% w/w ZnO NPs decreased the initial burst release of EM; EM-loaded PVA/CMC/ZnO nanocomposites were effective against S. aureus and E. coli.
|AgNPs||10% w/w CA in acetone/water at 4/1 v/v||Single nozzle electrospinning;|
AgNPs were added to CA solution at 0.0, 0.75 and 1.50% w/w;
Fibers were produced using potential of 15 kV, distance of 10 cm and a feed rate of 3.0 mL/h;
|Fiber diameters increased with increasing content of AgNPs, from ≈ 568 nm (pure CA) to ≈ 614 nm (1.50% w/w).|||
|Titanium dioxide (TiO2)/AgNPs||17% w/v CA in DMF/acetone at 1/2 v/v||Single nozzle electrospinning;|
TiO2/AgNPs production: (1) 2/1% w/v DOPA in 1M Tris HCl buffer were used to coat TiO2 NPs; (2) DOPA-coated TiO2 were then added to 0.2 M AgNO3 and stirred for 18 h; (3) TiO2/AgNPs nanocomposite particles were centrifuged and dried at 60 °C for 12 h;
5% and 10% w/w TiO2/AgNPs were added to CA;
Fibers were produced using potential of 15 kV and distance of 15 cm.
|TiO2/AgNPs nanocomposite particles had spherical and rod-like shapes and sizes between 20 and 100 nm (average of ≈ 36.12 nm);|
As the NPs content increased so did the fibers diameters;
Both studied NPs concentrations showed good antibacterial activities against E. coli and S. aureus.
|ZnO/AgNPs||17% w/w CA in DMF/acetone at 1/2w/w||Single nozzle electrospinning;|
5% and 10% w/w ZnO/AgNPs were mixed with CA;
Fibers were produced using potential of 15 kV and distance of 15 cm.
|CA, CA/ZnO and CA/ZnO/AgNP nanofibers were regular and bead free;|
Addition of AgNPs to CA/ZnO reduced the fibers diameters;
CA/ZnO/AgNPs nanofibers were effective against E. coli and S. aureus bacteria;
Nanocomposites containing 10% w/w ZnO/AgNPs yielded 0% viable bacteria cells in relative cell viability experiments.
|Ag/Cupper (Cu) loaded onto sepiolite (SEP) and mesoporous silica||9% w/w CA in acetone/dH2O at 80/20 v/v||Single nozzle electrospinning;|
Two NPs were produced: NPs of silica SBA-15 contained 8.9% w/w Cu and 3.5% w/w Ag, and raw SEP NPs containing 24.4% w/w Ag and 18.5% w/w Cu;
5% w/w particles (in relation to the polymer and NPs mass) were added to CA;
Fibers were produced using potential of 23 kV, distance of 15 cm and feed rate of 0.8 mL/h.
|NPs became entrapped within the fibers during production; |
NPs were found well dispersed with occasional aggregates randomly distributed along the fibers;
Diameters varied between 400 and 500 nm;
All metal-loaded CA nanocomposites impaired significantly the growth of Aspergillus niger;
The amount of metal NPs released daily by the nanocomposite represented ≈ 1% of the total amount of Ag or Cu.
|Ag ions/AgNPs||10% w/w CA in acetone/water at 80/20 w/w||Single nozzle electrospinning;|
0.0, 0.05, 0.30 and 0.50% w/w AgNO3 were added to CA; Fibers were produced using potential of 17 kV, distance of 10 cm and feed rate of 3 mL/h;
Silver ions on the electrospun CA fibers were submitted to UV irradiation (photoreduction).
|Fiber diameters decreased with AgNO3 increased content; |
Silver ions in ultrafine CA fibers were successfully photoreduced into AgNPs;
The average diameters of the AgNPs were in the range of 3–16 nm;
Both AgNO3 (non-reduced) and AgNPs (photoreduced) ultrafine CA fibers showed very strong antimicrobial activity.
|ZnO||10 % w/v PHBV in chloroform/DMF at 90/10 v/v||Single nozzle electrospinning;|
CNCs were prepared by acid hydrolysis in 9/1 v/v C6H8O7/ HCl at 80 °C for 6 h;
Zn (NO3)26H2O were added at ½ into CNCs;
NaOH was added drop-wise to precipitate Zn2+;
0, 3, 5, 10 and 15 w/w% CNC/ZnO to PHBV and mixed for 24 h prior to spinning;
Fibers were produced using potential of 18 kV, distance of 16 cm and feed rate of 1 mL/h.
|Fiber diameters became narrower with higher loads of CNC/ZnO;|
The uniformity and porosity of the mats also increased with the higher incorporation of CNC/ZnO;
The tensile strength and Young’s modulus were the most important with 5 w/w% CNC/ZnO;
Mats with 5 w/w% CNC/ZnO had the highest water absorbency and exhibited the best antibacterial activity.
|AgNPs||6% w/v PVA in dH2O||Single nozzle electrospinning;|
Synthesis of CNCs: (1) cellulose-rich cotton fibers were immersed in a NaOH solution (2% w/v) to remove impurities; (2) samples were hydrolyzed in HCl;
CNCs were surface modified with succinic anhydride (SA) for 24 h;
Modified CNCs (0.5 g) and AgNO3 at 0.05 M were mixed for 15 h, filtered and washed, and finally added to PVA;
Fibers were produced using potential of 15 kV, distance of 15 cm and feed rate of 0.3 mL/h.
|Films were smooth, highly flexible and displayed a highly homogeneous appearance;|
AgNPs coupled to the CNC were more effective against P. aeruginosa.
|16.6% w/w PVP in DMF||Single nozzle electrospinning;|
Synthesis of CNCs: CNCs were isolated from corn stalk using 60 w/w% sulfuric acid hydrolysis and mechanical treatments;
AgNO3 and freeze-dried CNCs were dispersed in PVP at continuous stirring for 24 h at RT;
Prepared samples: pure PVP, PVP/CNC-2%, PVP/CNC-4%, PVP/AgNO3-0.17%, PVP/AgNO3-0.34%, PVP/CNC-2%/AgNO3-0.17%, and PVP/CNC-2%/AgNO3-0.34% suspensions;
Fibers were produced using potential of 18 kV, distance of 20 cm and feed rate of 1 mL/h.
|Fiber diameters were the smallest for PVP/CNC-4%/AgNO3-0.34% (131 ± 46 nm);|
Upon addition of 4 w/w% CNCs, the ultimate tensile strength of pure PVP increased 0.8 MPa;
PVP/CNC-4%/AgNO3-0.34% composites acted as excellent antimicrobial agents against both E. coli and S. aureus.
|Bacterial Cellulose (BC)|
|Soy protein NPs||5% w/v BC in TFA||Single nozzle electrospinning;|
Fibers were produced using potential of 30 kV, distance of 20 cm and feed rate of 0.2 mL/h;
Surface functionalization: (1) 2.5% w/v of soy protein was dispersed in dH2O; (2) BC electrospun nanofiber scaffolds were immersed in soy protein solution and ultrasonicated for 1 h at 300 W for ultrasound-induced self-assembly process; (3) nanofibers were washed three times with ethanol/water mixture (70/30, v/v) to remove free soy protein molecules.
|Nanofibers had a multi-size distribution with diameters ranging from 80 to 360 nm; |
After soy protein surface modification, nanofibers became more stretchable, increasing the elongation at break;
Nanofibrous with soy protein NPs showed superior biocompatibility compared to pure BC electrospun nanofibers.
|GO||3% w/v chitosan (CS) in acetic acid solution and 5% w/v BC prepared at 1/1, 4.5/1 and 8/1;|
5% w/v PEO was added to the mixtures at different amounts
|Single nozzle electrospinning;|
0, 3, 6 and 10 v/v% PEO were added to CS/BC;
PEO/CS/BC fibers were produced using potential of 20 kV, distance of 12 cm and feed rate of 0.3 mL/h;
0, 0.5, 1, 1.5 and 2 w/w% GO were added to CS/BC;
GO/CS/BC fibers were produced using potential of 22 kV, distance of 10.
|Mats with uniform morphologies were attained with 1.5% GO, however with 2% GO smaller diameters were generated;|
High amounts of GO increased the scaffold mechanical strength;
A reduction in the hydrophilicity of the electrospun nanofibers and their water vapor permeability with the addition of GO was also reported.
|Natural Extracts||Polymer Concentration/Ratio/Solvent||Incorporation of Agent and Production Conditions||Results||Ref.|
|Bromelain||15% w/w CA in acetone/DMF at 85/15 w/w|
15% w/w CTAc in acetone/DMF at 85/15 w/w
15% w/w 70%CA + 30%CTAB in acetone/DMF at 85/15 w/w
|Single nozzle electrospinning;|
CTA was produced from CTAc and CTAB through traditional acetylation process with H2SO4 and C4H6O3;
0.0264 g of bromelain were added to 15% w/w 70%CA + 30%CTAB in acetone/DMF;
Fibers were produced using potential of 25 kV, distance of 10 cm and feed rate of 4 mL/h;
Bromelain was also immobilized via crosslinking on control fibers by immersion in 3-aminopropyl triethoxysilane and 1% v/v glutaraldehyde.
|The acetyl content of CA was 41.9%, which corresponded to a D of 2.8; |
CTAC and CTAB solutions could not be electrospun because of their improper molar mass;
CA fibers reached diameters of 470–755 nm and the CA+CTAB of 93–206 nm;
Nanofibers immersed in a solution mimicking basic sweat had the lowest mass loss rate, not exceeding 9%, while in acid solutions they had the highest, ≈28%;
In vitro controlled release tests were performed to semi-quantitatively evaluate the release profile of bromelain, which was completed in 3 days;
Crosslinking was more effective than pos-electrospinning immobilization.
|15% w/v CA in acetone||Single nozzle electrospinning;|
5% v/v of selected EO in CA solution;
Fibers were produced using potential of 15 kV, distance of 15 cm (maintained for all combinations) and feed rate of 5 mL/h for pristine CA, 25 kV and 3 mL/h for CA/CN, and 20 kV and 5 mL/h for both CA/LG and CA/PM.
|The produced fibers were smooth, with diameters averaging ≈ 4.2 μm for CA, ≈ 0.9 μm for CA/CN, ≈ 2.8 μm for CA/LG and ≈ 2.3 μm for CA/PM; |
Fibers encapsulating 6.2 to 25.0% w/w of EOs were able to effectively stop proliferation of E. coli;
EOs loaded mats were only effective against C. albicans with concentrations above 40% w/w;
No cytotoxic effects were observed against fibroblasts and human keratinocyte cell lines.
|15% w/v of CA in acetone||Single nozzle electrospinning;|
5% v/v of selected EO in CA solution;
Fibers were produced using potential of −120 kV, distance of 15 cm and feed rate of 2 mL/h.
|Fibers loaded with EOs revealed larger diameters because of the solution increased viscosity; |
Oregano oil was more effective than rosemary oil against bacteria;
Rosemary oil was more efficient against the yeasts C. albicans than oregano oil.
|Thymol (THY)||Porous mats:|
5.75% w/v CA in acetone/DCM at 1/4 v/v;
15% w/w CA in acetone/DMAc at 3/2 v/v
|Single nozzle electrospinning;|
Porous and nonporous mats: 0, 5, 10 and 15% w/w of THY (in relation to the polymer mass) mixed in the CA solution;
Fibers were produced using potential of 18 kV, distance of 15 cm and feed rate of 2 mL/h.
|Fibers from porous CA mats attained diameters of 2.95–4.66 μm;|
Fibers from nonporous CA mats exhibited smooth surface morphologies with diameters ranging 450–850 nm;
Porous THY-loaded mats had a slower initial EO release, prolonging it over time, and reveling a superior antibacterial activity and cytocompatibility compared with the nonporous THY-loaded mats.
|15% w/w CA and 10% w/w polyurethane (PU), at 1/1, 2/1 and 3/1 v/v, in DMF/MEK at 50/50 w/w||Single nozzle electrospinning;|
2% w/w of zein and 1% w/w of streptomycin sulfate were added to the CA/PU solutions;
Fibers were produced using potential of 18 kV, distance of 15 cm and feed rate of 0.5 mL/h.
|1/1 and 2/1 CA/Pu ratios registered bead formations on the surface; At 3/1 CA/PU fibers were more uniform exhibiting diameters of 400–700 nm; Loaded CA/PU accelerated blood clotting and enhanced fibroblasts growth, while displayed excellent bactericidal activity against Bacillus subtilis and E. coli bacteria.|||
|Asiaticoside in the form of pure substance (PAC) and crude extract (CACE)||17% w/v CA in acetone/DMAc at 2/1 v/v;|
For comparison purposes, films were also produced by solvent-casting at 4% w/v CA in acetone/DMAc at 2/1 v/v
|Single nozzle electrospinning;|
40% w/w of PAC or CACE (in relation to the polymer mass) were added to the CA solutions, both for electrospinning or solvent-casting;
Fibers were produced using potential of 17.5 kV, distance of 15 cm and feed rate of 1 mL/h.
|Produced fibers were smooth even with the addition of the plant extracts; |
The average fiber diameter increased from 485 nm for PAC loaded to 545 nm for CACE loaded spun mats;
Loaded electrospun mats showed higher capacity to retain water and resist weight loss than those films produced by solvent casting;
All extract-loaded films were nontoxic to cells, the only exception being the highest concentration of CACE which was seen to lower cell viability.
|Curc||17% w/v CA in acetone/DMAc at 2/1 v/v;|
For comparison purposes, films were also produced by solvent-casting at 4% w/v CA in acetone/DMAc at 2/1 v/v.
|Single nozzle electrospinning;|
5, 10, 15 and 20% w/w of Curc (in relation to the polymer mass) were added to the CA solutions, both for electrospinning and solvent-casting;
Fibers were produced using potential of 17.5 kV, distance of 15 cm and feed rate of 1 mL/h.
|Curc loading did not affect the electrospun mats morphology;|
The fiber diameter of Curc loaded CA fibers averaged 314–340 nm;
The Curc loaded nanostructured mats antioxidant activity was superior to the casted films;
Presence of Curc decreased cell viability but was not significant to pose any threats to the normal function of the human dermal fibroblast.
|10% w/w CA in acetone/water at 80/20 v/v;|
10% w/w polyvinylpyrrolidone (PVP) in acetone/water at 50/50 v/v;
10% w/w CA/ PVP in acetone/water at 70/30 v/v.
|One-pot electrospinning using the dual spinneret technique;|
10% w/w of Curc (in relation to the polymer mass) were added to the CA, PVP or CA/PVP solutions;
Fibers were produced using potential of 25 kV, distance of 15 cm and feed rate of 3 mL/h.
|Diverse fiber diameters were obtained: ≈ 780 nm for neat CA, ≈ 495 for neat PVP, ≈ 1150 for Curc/CA, ≈ 570 for Curc/PVP, and ≈ 1560 for Curc/CA/PVP;|
Incorporation of PVP increased the fibers hydrophilicity and accelerated Curc release;
Mats prepared by dual-spinneret electrospinning, namely Curc/CA+Curc/PVP, exhibited the highest antibacterial activity against S. aureus.
|Asiaticoside in form of PAC and CACE;|
|17% w/v CA in acetone/DMAc at 2/1 v/v.||Single nozzle electrospinning;|
5, 10, 15 and 20% w/w of Curc (in relation to the polymer mass) were added to the CA solutions;
2, 40% w/w of PAC or CACE (in relation to the polymer mass) were added to the CA solutions;
Fibers were produced using potential of 17.5 kV, distance of 15 cm and feed rate of 1 mL/h.
|As-loaded herbal mats remain stable up to 4 months of storage, either at RT or 40 °C;|
Curc loaded mats showed superior antioxidant capacity compared to PAC or CACE containing mats;
PAC and CACE loaded structures were more biocompatible the Curc loaded counterparts;
40% w/w PAC loaded surfaces supported the most attachment and proliferation of fibroblasts;
Higher syntheses of collagen was observed for cells cultured on CA fibers that containing either 2% w/w CACE or 40% w/w PAC.
|Gallic acid (GA)||17% w/v CA in acetone/DMAc at 2/1 v/v||Single nozzle electrospinning;|
2.5–10% w/w of GA (in relation to the polymer mass) were added to the CA solutions;
Fibers were produced using potential of 12 kV, distance of 12.5 cm and feed rate of 0.1 mL/h.
|Fiber diameters increased linearly with the amount of GA;|
GA aggregation of GA was observed on surfaces loaded with 7.5–10% v/v GA;
GA was successfully released from the electrospun mats.
|Gingerol||12% w/v CA in acetone for 2 h at 25 °C;|
For comparison purposes, films were also produced by solvent-casting at 12% w/v CA in acetone
|Single nozzle electrospinning;|
6% w/w of gingerol were added to the CA solutions, both for electrospinning and solvent-casting;
Fibers were produced using potential of 7.5 kV, distance of 10 cm and feed rate of 0.7 mL/h.
|Fibers were smooth, varying from ≈ 475 nm (pristine) to 375 nm (loaded) in diameter, and with a very small number of beads being detected;|
≈ 97% of the loaded gingerol could be released from the fibers at 37 °C;
The release rate of gingerol increased drastically in the first 4 h (≈ 92%) and remained constant after that period;
2,2-diphenyl-1-picrylhydrazyl (DPPH) scavenging assays and in vitro cytotoxicity tests showed the antioxidant activity of the prepared fibers and a viability above 60% for L-929 mouse fibroblast-like cells.
|Garlic extract||9.6% w/v CA and 9% w/v PVP in 98% acetic acid||Single nozzle electrospinning;|
Garlic extraction: (1) the garlic was crushed and macerated in ethanol at 1/1 w/w for two nights at 4 °C;
CA solution was mixed with PVP at 8:5, which made the ratio of the dry weight of PVP to CA of 3/2;
For every 13 g of PVP/CA 1 g of glycerine was added (PVP/CA/glycerine) or 1 g of garlic extract (PVP/CA/garlic); combinations of the two were also made;
Fibers were produced using potential of 15 kV and distance of 12 cm.
|The composite nanofibrous mats were uniform, bead-free with a size ranging from 350 nm to 900 nm; |
Release of garlic extract from PVP/CA/glycerine/garlic was the most important due to the large diameter of the fibers;
The antibacterial activity of the PVP/CA/garlic nanofibrous mat was effective against both S. aureus and P. aeruginosa;
PVP/CA/glycerine/garlic fibers were the most antimicrobial.
|Thymol||9% w/v PVA in dH2O||Single nozzle electrospinning;|
30% w/w CNCs (in regard to PVA concentration) were prepared in dH2O/H2SO4 and added to PVA;
Fibers were produced using potential of 10 kV, distance of 10 cm and feed rate of 0.25 mL/h.
Electrospun PVA/CNCs was mixed with PLA in CHCl3 to obtain blends with a final concentration of 1 % w/w;
nanocomposite films were impregnated with thymol dissolved in supercritical carbon dioxide (scCO2).
|PVA/CNCs nanofibers impregnated with thymol registered a yield of 20%, while the PLA films obtained 24%;|
The release rate of thymol was significantly slower when PVA/CNCs were incorporated within a PLA matrix.
|Tragacanth gum (TG)||7.7% w/w of keratin/PEO at 70/30 in dH2O;||0, 1, 3 and 5% w/w of BC were added to the keratin/PEO solution; |
Fibers were produced using potential of 22 kV, with distance of 10 cm and feeding rate of 0.1 mL/h;
TG was incorporated by electrospraying as the nanofibers were being electrospun.
|The mean fiber diameter of the mats composed by keratin/PEO was 243 ± 57 nm and reduced to 150 ± 43 nm with the addition of 1% or higher % of BC; |
BC (1%) significantly reduced the hydrophobicity of the mat;
TG and BC modified mats promoted cell attachment and proliferation on the surface of the nanofibers.
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