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5 protocols using tmpta

1

Fluorescent Dyes and Monomers for Photopolymerization

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The fluorescent dyes [4-phenyl-2,6-bis(2-pyridyl)pyridine]tris [4,4,4-trifluoro-1-(4-nitrophenyl)butane-1,3-dione]europium(III) (Eu1), 7-diethylamino-4-methylcoumarin (Coumarin 1, Alfa Aesar), and 4,4-difluoro1,3,5,7,8-pentamethyl-4-bora-3a,4a-diaza-s-indecene (BODIPY, B1) were used. The synthesis of the compound 4,4-difluoro1,3,5,7,8-pentamethyl-4-bora-3a,4a-diaza-s-indecene (BODIPY, B1) was described in a previous article [41 (link)]. Monomers used for the compositions were isobornyl acrylate (IBOA, IGM RESINS), bisphenol A ethoxylate diacrylate (BEDA, Sigma Aldrich, St. Louis, MO, USA), and trimethylolpropane triacrylate (TMPTA, Sigma Aldrich). The initiator diphenyl(2,4,6-trimethylbenzoyl)phosphine oxide (TPO, Sigma Aldrich) was used. The structures of the molecular fluorescent dyes, monomers, and initiator are presented in Figure 9.
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2

3D Printing of Arteriovenous Grafts

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The 3D printing resin formulation used for the arteriovenous ACMO-based graft (ACMO-AVG) was comprised of 4 mL of 4-acryloylmorpholine (ACMO, Sigma Aldrich, CAS# 5117-12-4), 0.5 mL of trimethylolpropane triacrylate (TMPTA, Sigma Aldrich, CAS# 15625-89-5) and 0.5 mL of trimethylolpropane ethoxylate triacrylate (TMETA, Sigma Aldrich, CAS# 28961-43-5) in 1 mL of ethanol. Likewise, the 3D printing ink formulation of the arteriovenous PEGDA graft (PEGDA-AVG) was comprised of 60% PEGDA-575, 30% PEGDA-250 (Sigma Aldrich, CAS# 26570-48-9) and 10% ethanol. Bis(2,4,6-trimethylbenzoyl)-phenylphosphine oxide was used to as the photoinitiator in the printing process. Computer assisted design (CAD) models were first drawn and the different structural features were specified. The models were then sliced into multiple images using the manufacturers provided software. All the 3D printing processes were conducted using a DLP 3D printer. For the purpose of this study, the curing time for both the ACMO-AVG and PEGDA-AVG were kept the same and after the printing process, the grafts were first rinsed with ethanol before being subjected to a post-curing exposure to 365 nm UV light for 2 min to ensure the full extent of polymerization.
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3

Synthesis of Photocrosslinkable Hydrogels

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FeCl3·6H2O (Acros
Organics, 99%), fumaric acid (Acros Organics, 99%), Pluronic F127
(Sigma-Aldrich, average Mw = 12,600 g/mol, Aldrich), acetic acid (Thermo
Scientific, 99.7%), poly(ethylene glycol) diacrylate (Sigma-Aldrich,
average Mn = 250), PEGDA250, poly(ethylene glycol) diacrylate
(Sigma-Aldrich, average Mn = 700) PEGDA700, TMPTA (Sigma
Aldrich), and diphenyl(2,4,6-trimethylbenzoyl)phosphine oxide (Sigma-Aldrich,
97%) were purchased and used without further purification.
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4

HIPE Synthesis with Monomer Variation

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HIPEs were synthesised with monomer proportions ranging from 100% EHA (Sigma Aldrich, UK) to 100% IBOA (Sigma Aldrich, UK) at 25% intervals. The organic component of the continuous phase was formed from the monomers and a crosslinker (trimethylolpropane triacrylate (TMPTA) Sigma Aldrich, UK) at 26.96 wt% of the monomers. A surfactant (Hypermer B246-SO-(MV), Croda, UK) was added at 3 wt% of the organic mass and left to dissolve in a sonic water bath. Finally, a photoinitiator (2,4,6-trimethylbenzoyl)-phosphine oxide/2-hydroxy-2-methylpropiophenone, 50/50, Sigma Aldrich, UK) was added at 5 wt% of the organic mass. The internal phase, distilled water, was added at 0.75, 0.80, 0.85 and 0.90 ϕ to each continuous phase, to produce twenty HIPE compositions. These are referred to by their wt% EHA and nominal porosity. For example, EHA50P85 is a HIPE consisting of 50 wt% EHA and 50 wt% IBOA with a ϕ of 0.85, and EHA0P75 is a HIPE formed from 100% IBOA with a ϕ of 0.75.
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5

Photopolymerized Amphiphilic Copolymer Nanoparticles

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2-ethylhexyl acrylate (EHA, 98.0%, Sigma-Aldrich), isobornyl acrylate (IBOA, 85.0% Sigma-Aldrich), trimethylolpropane triacrylate (TMPTA, 80.0 %, Sigma-Aldrich) were used as monomers. Poly (ethylene glycol)-block-poly (propylene glycol)-block-poly (ethylene glycol)
[PEG-PPG-PEG, Pluronic L-81, average Mw ~ 2800 g mol -1 , and HLB ~ 2] and Irgacure 907 (BASF) were used as surfactant and photoinitiator, respectively, in the middle (monomer) phase. Poly (ethylene glycol)-block-poly (propylene glycol)-block-poly (ethylene glycol)
[Pluronic F-127, average Mw ~12,500 g mol -1 , and HLB ~ 22] was used as surfactant in the inner and outer aqueous phase.
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