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64 protocols using n n dimethylformamide (dmf)

1

Electrospun PLLA Membrane Fabrication

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The generation of electrospun membranes consisting of PLLA fibres by use of the Nanospider device (NS 1WS500U, Elmarco) is described thoroughly elsewhere [60] . In brief, dichloromethane (DCM, Macron fine chemicals, Avantor, USA) was mixed with dimethylformamide (DMF, VWR chemicals, USA) by a 98 to 2 weight ratio (98/2 w DCM /w DMF ) to increase the solution conductivity and relative permittivity. Two different electrospinning solutions were prepared by dissolving PLLA in form of pellets (3100HP Ingeo, Natureworks, USA) by a weight ratio of 10% (w PLLA /w Solvent ) (sample I) and 8% (w PLLA /w Solvent ) (sample II), respectively, in the blend solvents. Furthermore, a third sample with a weight ratio of 12% (w PLLA /w Solvent ) was produced (sample III) for CT scanning. Tetraethylammonium bromide (TEAB, Sigma Aldrich, USA) was added by a weight ratio of 0.015%w/w Solvent to increase electrical conductivity. The solution was filled in the reservoir of the Nanospider device equipped with a spinning carriage module and spinning was performed with an applied voltage of +20 / -17 kV and a distance of 220 mm of the source to the substrate. Furthermore, a relative humidity of 20% and a reservoir speed of 480 mm/s were applied.
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2

Mimosa Tannin Extract Characterization

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The commercially available mimosa tannin “Weibull” extract was supplied by the Tanac company (Montenegro, Brazil). The 5-(hydroxymethyl)furfural (5-HMF, ≥ 95%) was acquired from AVA Biochem (Zug, Switzerland). Technical grade acetone (>99%), sodium hydroxide pellets (NaOH) and N,N-Dimethylformamide (DMF, 99.9%) were provided by VWR. Ammonium hydroxide (25% in H2O), zinc sulfate heptahydrate, Eriochrome® Black T, ammonium chloride, Murexide, and methyl orange (MO) were obtained from Sigma Aldrich (St. Louis, MO, USA). Copper(II)sulfate (anhydrous) and acetic acid (glacial, 100%) were acquired from Merck (Darmstadt, Germany). Rhodamine B (RB) was provided by Alfa Aesar (Haverhill, MA, USA). Ethylenediaminetetraacetic acid disodium salt solution (0.1 M) was purchased from Fischer Scientific (Hampton, VA, USA). Ethylenediaminetetraacetic dianhydride (EDTAD, 98%) was supplied by ABCR (Karlsruhe, Germany).
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3

Tilapia Skin Preparation for Analysis

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Fish skins were peeled off Tilapia specimens bred in the pilot aquaponics plant of the “Urban Farming Lab” of the Dept. of Innovation Engineering (University of Salento, Lecce, Italy), where they were distributed in glass aquaria filled with dechlorinated water and supported with two oxygen pumps. Skins were harvested when the small (length: 25.0 ± 1.1 cm, height: 9.4 ± 0.9 cm, weight: 320.8 ± 35.8 g, ST) and the big (length: 31.6 ± 0.6 cm, height: 10.9 ± 0.9 cm, weight: 606.7 ± 19.7 g, BT) adult size were reached. Non-fish-skin components (i.e., scales, fillet) were immediately eliminated with a knife. Then, fish skins were rinsed three times with distilled water and stored at −20 °C in polyethylene bag. Prior to use, samples were thawed at 4 °C.
Distilled water was obtained from Millipore Milli–U10 water purification facility from Merck KGaA (Darmstadt, Germany). N, N–dimethylformamide was provided by VWR International PBI S.r.l. (Milan, Italy). Acetic acid, chloroform, methanol, and CaCl2, norleucine, and N–tert–butyldimethylsilyl–N–methyltrifluoroacetamide (MTBSTFA) were purchased from Sigma–Aldrich (Milan, Italy). If not otherwise stated, all other chemicals used were of analytical grade and purchased from Sigma–Aldrich (Milan, Italy).
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4

Solid-Phase Peptide Synthesis Protocol

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All Fmoc amino acids, Rink amide AM 200–400, 1-hydroxybenzotriazole (HOBt·H2O) and O-Benzotriazole-N,N,N’,N’-tetramethyluronium hexafluorophosphate (HBTU) were purchased and used as received from Iris Biotech GmbH (Marktredwitz, Germany). Triisopropylsilane (TIS), ethane-1,2-dithiol (EDT), trifluoroacetic acid (TFA), sodium trifluoroacetate (NaTFA), acryloyl chloride (99 %), diisopropylethylamine (DIEA, 98 %), dicyclohexylcarbodiimide (DCC, 99 %) cesium hydroxide monohydrate (99.95 %), ethyl vinyl ether (98 %), palladium on activated charcoal (10 % Pd), phosphate buffered saline sachets and α-cyanohydroxycinnamic acid were purchased from Sigma-Aldrich (Buchs, Switzerland). N,N-dimethylformamide was obtained from VWR, (Nyon, Switzerland) and N-methylpyrrolidone was obtained from Schweizerhall (Basel, Switzerland). Glycidol (96 %), ethanolamine (99 %), serinol (98 %), p-methoxybenzylalcohol (98 %), phosphorus tribromide (1.0 M solution in dichloromethane, AcroSeal®), potassium carbonate (99+ %), maleic anhydride (99 %), β-alanine (99 %), pentafluorophenol (99 %) and benzene (99 %) were obtained from Acros (Germany).
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5

Cobalt Phthalocyanine Microparticle Synthesis

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Cobalt(II) phthalocyanine microparticles (CoPCMPs) and Pluronic® F-127 (Pluronic) were purchased from Sigma-Aldrich. N,N-dimethylformamide (DMF) was purchased from VWR (Radnor, PA, USA). Matrimid® 5218 (Matrimid) was purchased from Huntsman Corporation (Conroe, TX, USA). All chemicals were used as received without further purifications. Chemical structures of CoPCMPs and commercial polymers are illustrated in Figure 1.
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6

Synthesis of Redox-Responsive Polymers

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N-Cyanomethylacrylamide and ethyl 2-(butylthiocarbonothioylthio)propanoate (CTA-1) were synthesized according to previously described protocols [11 (link)]. 2,2′-Azobis(isobutyronitrile) (AIBN, ≥98%, Aldrich, France), 2,2′-azobis[2-(2-imidazolin-2-yl)propane]dihydrochloride (VA-044) (Aldrich, 98%), 1,3,5-trioxane (Aldrich, ≥99%) and N,N-dimethylformamide (DMF, Normapur, VWR, France) were used as received. N,N-Dimethylacrylamide (DMAm) (Aldrich, ≥99%) was distilled under reduced pressure before use. Deionized water was used for all aqueous polymerizations.
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7

Carvedilol-Loaded Polymer Microparticles

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Carvedilol (CVD) was obtained from Inke (Castellbisbal, Spain). Poly-ε-caprolactone (PCL, Mw 80,000 Da) was supplied by Perstorp Caprolactones Ltd. (Warrington, UK), Poly(DL-lactide) (PDLA, viscosity midpoint 2.0 dl/g) was supplied by Corbion polymers® (Amsterdam, The Netherlands) and poly(3-hydroxybutyrate) (PHB, under the trade name P226, Mw 426,000 Da) was purchased from by Biomer (Krailling, Germany). For the hydrophilic layer, Polyethylene oxide (PEO, Mw 200,000 Da) was purchased from the Dow Chemical Company (Montomeryville, PA, USA), polyvinylpyrrolidone (PVP, under the trade name Kollidon 90F, Mw 1,250,000 Da) was purchased from BASF (Ludwigshafen, Germany) and ethyl cellulose (EC, viscosity 22 cP, 5% in toluene/ethanol 80:20) was purchased from Sigma-Aldrich (Madrid, Spain). Chloroform (ACS reagent, ≥99.8%) was supplied by Sigma-Aldrich (Madrid, Spain), whilst methanol, ethanol (≥99%), and acetone (≥98%) were supplied by Panreac Química S.L.U. (Castellar del Vallès, Barcelona). The solvent 2,2,2-trifluoroethanol (TFE, ≥99%) was purchased from Alfa AesarTM (Karlsruhe, Germany) and N,N,-dimethylformamide (DMF, ≥99.8%) was purchased from VWR Chemicals (Leuven, Belgium). All the polymers and reagents were used as received without further purification.
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8

Synthesis and Characterization of Block Copolymers

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Poly(styrene-random-2-vinyl pyridine) with Mn value of 130k and a PDI of 1.69 was acquired from Sigma-Aldrich. Poly(styrene-block-2-vinyl pyridine) (PSbP2VP) and poly(2-vinyl pyridine-block-styrene-block-2-vinyl pyridine) (P2VPbPSbP2VP) with Mn values of 102–97k (PDI: 1.12), 40–44k (PDI: 1.10) and 12–23–12k (PDI: 1.25), respectively, were purchased from Polymer Source Inc. and were used as is. Silicon wafers with and without thermally grown oxide layers of 1 μm were acquired from WRS Materials. The silicon wafers used for atomic force microscopy, ion sorption, and GI-SAXS were p-type and doped with boron (resistivity of 1 to 20 Ω cm). The silicon wafers with 1 μm SiOx were used for fabricating interdigitated electrodes (IDEs). Gold quartz crystals (5 MHz) were supplied from Gamry. 99.9% gold pellets were purchased from ACI Alloys for making IDEs. Iodomethane (CH3I), potassium iodide (KI), toluene, N,N-dimethylformamide (DMF) were acquired from VWR or Sigma-Aldrich and used as is. S1813 photoresist and MF-319 developer were purchased from MicroChemicals.
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9

Mucoadhesive Ciprofloxacin Drug Delivery

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Ciprofloxacin hydrochloride monohydrate (CPX) was obtained from Uquifa (Castellbisbal, Spain). Poly-ε-caprolactone (PCL, Mw 80000 Da) was supplied by Perstorp Caprolactones Ltd (Warrington, United Kingdom), and poly(lactic acid) (PLA viscosity midpoint 2.0 dL/g) was supplied by Natureworks® (Naarden, Netherlands). For the mucoadhesive layer, polyethylene oxide (PEO, Mw 200000 Da) was purchased from the Dow Chemical Company (Montomeryville, PA, USA), and Eudragit RS100 (PAC, copolymer of ethylacrylate, methyl methacrylate and trimethylammonioethyl meth-acrylate chloride) was purchased from Evonik Industries (Essen, Germany). Chloroform (ACS reagent, ≥99.8%) was supplied by Sigma-Aldrich (Madrid, Spain), whilst methanol (≥99%) was supplied by Panreac Química S.L.U. (Castellar del Vallès, Barcelona). The solvent 1,1,1,3,3,3-hexafluoro-2-propanol (HFIP) was supplied by Fluorochem (Hadfield, United Kingdom) and N,N,-dimethylformamide (DMF, ≥99.8%) was purchased from VWR Chemicals (Leuven, Belgium). All the polymers and reagents were used as received without further purification.
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10

Synthesis of Aromatic Polyimides

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Terephthaloyl chloride (TC, >99%), 1-(3-aminopropyl)imidazole) (API, >97), benzene-1,3,5-tricarbonyl trichloride (>98%) and 4-(chloromethyl)benzoyl chloride (>98%) were purchased from TCI (Tokyo, Japan). 1,4-phenylenediamine (>97%) was purchased from Alfa Aesar (Haverhill, MA, USA). Potassium carbonate (K2CO3, 99% anhydrous) and iodomethane (99.5% stabilized) were purchased from BeanTown Chemical (Hudson, NH, USA). Lithium bistriflimide (LiTf2N, 99%) was purchased from 3M (Minneapolis, MN, USA). N-methylpyrrolidone (NMP, ACS grade), N,N-dimethylacetamide (DMAc, ACS grade), N,N-dimethylformamide (DMF, anhydrous), toluene (anhydrous), dichloromethane (DCM, anhydrous), triethylamine (Et3N), and acetonitrile (CH3CN, ACS grade) were purchased from VWR (Atlanta, GA, USA). 4,4′-(hexafluoroisopropylidene)diphthalic anhydride (6FDA, 99%) and pyromellitic dianhydride (PMDA, 99%) were purchased from Akron Polymer Systems (Akron, OH, USA). All reagents and solvents were utilized as obtained, without further purification.
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