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Poly[(N-isopropylacrylamide-co-acrylamide-co-(hydroxyethylmethacrylate))] thermoresponsive microspheres: An accurate method based on solute exclusion technique to determine the volume phase transition temperature
Authors:G. Fundueanu  M. Constantin  R. Cortesi  P. Ascenzi
Affiliation:a Department of Pharmaceutical Sciences, University of Ferrara, I-44100 Ferrara, Italy
b Department of Bioactive and Biocompatible Polymers, “Petru Poni” Institute of Macromolecular Chemistry, 700487 Iassy, Romania
c Department of Biology and Interdepartmental Laboratory for Electron Microscopy, University “Roma Tre”, I-00146 Rome, Italy
Abstract:Poly[(N-isopropylacrylamide-co-acrylamide-co-(hydroxyethylmethacrylate))] [poly(NIPAAm-co-AAm-co-HEMA)] copolymer was synthesized as a new thermoresponsive material possessing a lower critical solution temperature (LCST) around 37 °C in phosphate buffer, pH 7.4, at a solution concentration of 1%, w/v. The influence of polymer concentration on LCST was determined by cloud point measurements and by microcalorimetric analysis. The copolymer was transformed in hydrogel microspheres by suspension reticulation of single bondOH groups with glutaraldehyde. The volume phase transition temperature (VPTT) of microspheres was determined by a new approach, which involves measurement of the increase in concentration of a blue dextran (BD) solution at different temperatures in the presence of dry microspheres. The minimum BD concentration that gives reliable and reproducible results was determined to be 1 mg/ml. However, the higher is the concentration of BD in solution the smaller is the error. Contrary to solution of the linear polymer which displays a sharp phase transition temperature, the dependence of water regain of the hydrogel with temperature lasts from 4 °C to 50 °C.
Keywords:AAm, acrylamide   AIBN, N,N&prime  -azobisisobutyronitrile   BD, blue dextran   CP, cloud point   D2O, deuterated water   GA, glutaraldehyde   HEMA, 2-hydroxyethyl methacrylate   ISEC, inverse size exclusion chromatography   LCST, lower critical solution temperature   NIPAAm, N-isopropylacrylamide   VPTT, volume phase transition temperature
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