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Hollow-structured nano- and microspheres with diameters ranging from 24 μm to 160 nm were successfully produced from chemically modified pectin (Ma-Pec) through a two-step synthesis. In a first step, the Pec was modified with glycidyl methacrylate (GMA) in a heterogeneous phase system, indeed consisting of water-soluble Pec and water-insoluble GMA, via an interfacial reaction at the interface of the GMA−water phase system after 12 h under continuous stirring of 1000 rpm at 60 °C. In a second step, the spheres were prepared in a water-in-benzyl alcohol nanodroplet emulsion at 12000 rpm under a bubbling stream of nitrogen in the presence of sodium persulfate, as initiator, and TEMED, as catalytic agent. FT-IR spectra revealed that the vinyl groups (CC) coming from the GMA were attached onto backbone of the polysaccharide. 13C-CP/MAS NMR spectra demonstrated that the spheres were formed via carbon−carbon π-bonds on Ma-Pec in the water phase, for the duration of the dispersion stage. The dark center (an empty core) and edge of the hollow spheres could be easily identified by SEM micrographs. This type of polymer structure represents a class of unique material with particular importance in terms of state-of the-art applications in both nano- and microencapsulation of drugs, for example, protection shields of biologically active agents. [ABSTRACT FROM AUTHOR]

Polysaccharide-structured copolymer hydrogel having excellent pH-sensitivity was developed from N,N-dimethylacrylamide (DMAc) and vinyl-functionalized Pectin (Pec). The Pec was vinyl-functionalized by way of chemical reaction with glycidyl metacrylate (GMA) in water under acidic and thermal stimuli. 13C NMR, 1H NMR, and FT-IR spectra revealed that the vinyl groups coming from the GMA were attached onto backbone of the polysaccharide. The hydrogels were obtained by polymerization of the Pec-vinyl with the DMAc. 13C-CP/MAS NMR and FTIR spectra confirmed that the gelling process occurred by way of the vinyl groups attached on Pec-vinyl backbone. The values of apparent swelling rate constant (k) decreased appreciably for pH greater than 6, demonstrating the swelling process of the hydrogel becomes slower at more alkaline conditions. There was an increase of diffusional exponent (n) with increasing pH of the surrounding liquid. This means the water absorption profile becomes more dependent on the polymer relaxation in basified swelling media. In this condition, a longer water absorption half-time (t1/2) was verified, suggesting the polymer relaxation mechanism of the hydrogel would have a considerable effect on the t1/2. [ABSTRACT FROM AUTHOR]