pectins and glycidyl-methacrylate

Polysaccharide acid (PSA) based devices (consisting of alginic acid and polygalacturonic acid) were investigated for the detection of contaminating microorganisms. PSA-CaCl(2) hydrogel systems were compared to systems involving covalent cross-linking of PSA with glycidylmethacrylate (PSA-GMA) which was confirmed with Fourier Transformed Infrared (FTIR) analysis. Incubation of PSA-CaCl(2) and PSA-GMA beads loaded with Alizarin as a model ingredient with trigger enzymes (polygalacturonases or pectate lyases) or bacteria lead to a smoothening of the surface and exposure of Alizarin according to Environmental Scanning Electron Microscopy (ESEM) analysis. Enzyme triggered release of Alizarin was demonstrated for a commercial enzyme preparation from Aspergillus niger and with purified polygalacturonase and pectate lyase from S. rolfsii and B. pumilus, respectively. In contrast to the PSA-CaCl(2) beads, cross-linking (PSA-GMA beads) restricted the release of Alizarin in absence of enzymes. There was a linear relation between release of Alizarin (5-348 μM) and enzyme activity in a range of 0-300 U ml(-1) dosed. In addition to enzymes, both PSA-CaCl(2) and PSA-GMA beads were incubated with Bacillus subtilis and Yersinia entercolitica as model contaminating microorganism. After 72 h, a release between 10 μM and 57 μM Alizarin was detected. For protection of the hydrogels, an enzymatically modified PET membrane was covalently attached onto the surface. This lead to a slower release and improve long term storage stability based on less than 1% release of dye after 21 days. Additionally, this allowed simple detection by visual inspection of the device due to a colour change of the white membrane to orange upon enzyme triggered release of the dye.

Topics: Anthraquinones; Aspergillus niger; Bacillus subtilis; Biosensing Techniques; Biotechnology; Calcium Chloride; Culture Media; Epoxy Compounds; Hydrogels; Methacrylates; Microscopy, Electron, Scanning; Microspheres; Pectins; Polygalacturonase; Polysaccharide-Lyases; Yersinia enterocolitica

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.

Topics: Acrylamides; Epoxy Compounds; Hydrogel, Polyethylene Glycol Dimethacrylate; Hydrogen-Ion Concentration; Macromolecular Substances; Magnetic Resonance Spectroscopy; Methacrylates; Molecular Structure; Pectins; Phase Transition; Spectroscopy, Fourier Transform Infrared; Time Factors; Water

In this work, low-methoxyl pectin was chemically modified by reaction with glycidyl methacrylate (GMA) to give a material with low hydrosolubility. After physio-chemical characterization by FT-IR, DSC, and TGA analyses, the methacrylated/modified pectin (Pect-GMA) was crosslinked after the addition of sodium persulfate (SP), that actuates as initiator, at 50 degrees C for 24 and 48h either in the presence or not of aqueous polymethacrylate dispersion (Eudragit RS 30 D) to obtain free films by Teflon plate "casting" process. Different Pect-GMA/Eudragit RS 30 D ratios and SP concentrations were used. The free films were characterized by the determination of water vapor transmission (WVT), the swelling index (Ieq%) in simulated gastric (SGF) and intestinal (SIF) fluids, and by scanning electron microscopy (SEM). The presence of ionized groups in Pect-GMA turned the films pH-dependent because Ieq% of swollen crosslinked Pect-GMA films was larger at pH 6.8 than at pH 1.2. This was confirmed by the large pore size observed in the micrographs of SIF-swollen lyophilized films. In this way, films containing Pect-GMA and Eudragit RS 30 D, a time-dependent polymer, may present a synergistic action that favors specific biodegradation of the film in distal end of the gastrointestinal tract (GIT) by enzymes produced by the colonic microflora, enabling the modification of the release kinetics of drugs.

Topics: Bacteria; Calorimetry, Differential Scanning; Chemical Phenomena; Chemistry, Physical; Colon; Epoxy Compounds; Excipients; Hydrogen-Ion Concentration; Membranes, Artificial; Methacrylates; Microscopy, Electron, Scanning; Pectins; Permeability; Polysaccharides; Solubility; Spectroscopy, Fourier Transform Infrared; Thermogravimetry; Water