am hydrolysing corncob powder with 1% sulphric acid (autoclaved) then the solid and liquid portion were separated by filtration process. in liquid portion i calculated the total sugars but am not found suitable method for estimation of remaining sugar is present in filtered solid hydrolysed matter.
I'd rehydrolyse using more concentrated sulfuric acid, namely the classical Saeman hydrolysis with 72% sulfuric acid room temp (30 min - 2h depending on sample) then dilution to 1M and 3h 100°C.
The original reference may not be easy to find
Saeman, J. F., W. E. Moore, et al. (1954). "Techniques for the determination of pulp constituents by quantitative paper chromatography." Tappi, The Journal of the Technical Association of the Pulp and Paper Industry 37(8): 336-343.
but it is described in many more recent papers like DOI:10.1016/j.foodchem.2008.10.073 or DOI:10.1016/j.lwt.2009.06.016
Yes indeed, swelling the material in concentrated sulphuric acid followed by dilution and then standard hydrolysis assists with accessing the crystalline cellulose microbrils, in corn Zea mays you will also find xylans and mannans encrusted. You should also consider milling the material to improve accessibility and consistency of your quantitation. best wishes.
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