TY - JOUR
T1 - Towards a less biased dissolution of chitosan
AU - Thevarajah, Joel J.
AU - Bulanadi, Jerikho C.
AU - Wagner, Manfred
AU - Gaborieau, Marianne
AU - Castignolles, Patrice
PY - 2016
Y1 - 2016
N2 - The dissolution of polysaccharides is notoriously challenging, especially when one needs a “true” solution. Factors influencing chitosan’s solubility include composition, also known as degree of acetylation (DA). The dissolution of chitosan was investigated by visual observation, size-exclusion chromatography (SEC), pressure mobilization (PM), free-solution capillary electrophoresis (CE) and real-time solution-state NMR spectroscopy. Aqueous HCl dissolves around 15 % more chitosan than the commonly used aqueous acetic acid (AcOH), however aggregates were detected in SEC suggesting incomplete dissolution. Significant deacetylation of chitosan over the period needed for dissolution at high temperature occurred in DCl (NMR) by about 20 % of the initial DA value. Accurate DA determination by NMR spectroscopy may thus be possible only in the solid state (with a precision within 1 % on the DA % scale above a DA of 10 %). Overall a compromise between maximum solubilization and minimum degradation is required in attempting to obtain a “true” solution of chitosan. The completeness of the dissolution may be more influenced by the average DA than by molar mass.
AB - The dissolution of polysaccharides is notoriously challenging, especially when one needs a “true” solution. Factors influencing chitosan’s solubility include composition, also known as degree of acetylation (DA). The dissolution of chitosan was investigated by visual observation, size-exclusion chromatography (SEC), pressure mobilization (PM), free-solution capillary electrophoresis (CE) and real-time solution-state NMR spectroscopy. Aqueous HCl dissolves around 15 % more chitosan than the commonly used aqueous acetic acid (AcOH), however aggregates were detected in SEC suggesting incomplete dissolution. Significant deacetylation of chitosan over the period needed for dissolution at high temperature occurred in DCl (NMR) by about 20 % of the initial DA value. Accurate DA determination by NMR spectroscopy may thus be possible only in the solid state (with a precision within 1 % on the DA % scale above a DA of 10 %). Overall a compromise between maximum solubilization and minimum degradation is required in attempting to obtain a “true” solution of chitosan. The completeness of the dissolution may be more influenced by the average DA than by molar mass.
KW - chitosan
KW - dissolution (chemistry)
UR - http://handle.uws.edu.au:8081/1959.7/uws:36084
U2 - 10.1016/j.aca.2016.06.021
DO - 10.1016/j.aca.2016.06.021
M3 - Article
VL - 935
SP - 258
EP - 268
JO - Analytica Chimica Acta
JF - Analytica Chimica Acta
ER -