Detailed investigation on the molecular structure of carboxymethyl cellulose with unusual substitution pattern by means of an enzyme-supported analysis
B. Saake et al., Detailed investigation on the molecular structure of carboxymethyl cellulose with unusual substitution pattern by means of an enzyme-supported analysis, MACRO CH P, 201(15), 2000, pp. 1996-2002
Four carboxymethyl cellulose samples derived from the synthesis concept of
"reaction in reactive microstructures" were characterised in detail by comb
ination of different analytical techniques. Fractionation of one of the sam
ples according to water-solubility into four fractions revealed that a non-
statistical distribution of the substituents occurred for all fractions. En
doglucanase fragmentation of three samples was performed followed by analyt
ical and preparative SEC. The multi-detected analytical SEC proved samples
of high degree of substitution up to 1.9 to be intensively degraded, suppor
ting the proposed block-like substitution pattern. The detailed investigati
on of soluble fragmentation products by preparative SEC, hydrolysis and ani
on exchange chromatography pulsed amperometric detection revealed that all
samples contain fragments of much higher DS values than the average DS of t
he starting material. On the other hand, high quantities of degradation pro
ducts of low DS or almost no substitution occurred. Therefore, a structure
can be proposed with segments of very high DS alternating with areas of lim
ited substitution. The result clearly showed that the high substituted frag
ments were dominated by 2,3,6-tri-O-CMG.