Synthesis, spectroscopic and structural characterization of Co(II)-pullulan complexes by UV-Vis, ATR-FTIR, MALDI-TOF/TOF MS and XRD

2018 
Abstract Complexes of Co(II) ion with reduced low-molar pullulan (RLMP) ( M w 6000 g/mol) were synthesized in aqueous solutions at boiling temperature in the pH range from 7.5 to 13.5. Obtained Co(II)-RLMP complexes, with cobalt content ∼2–8% (AAS), were characterized by UV-Vis spectrophotometry, FTIR spectroscopy (ATR-FTIR, FT-IRIS), MALDI-TOF/TOF MS, and XRD. Tetragonally distorted O h coordination of Co(II) ions with O ligand atoms in synthesized complexes is suggested based on the spectrophotometric data. No influence of complexation process on the 4 C 1 chair conformation of the d -glucopyranose units of pullulan was detected by ATR-FTIR measurements and FT-IRIS showed high homogeneity of synthesized complexes. Some additional depolymerization of pullulan during complex synthesis was indicated by MALDI-TOF/TOF MS but it also revealed good stability of complexes with much weaker binding of Co(II) ion in low molar mass fragments. Even in complexes with highest Co(II) ion content a low degree of crystallinity was detected by XRD analysis.
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