The present study employed alkaline hydrogen peroxide pretreatment coupled with cold plasma for corn stalk’s complex biopolymers fractionation and valorization through enzymatic hydrolysis. This hurdle approach enables the prolonged generation of reactive oxidative species, initiating chemical reactions otherwise hardly possible under ambient conditions. A delignification rate between 76±1 and 86±2 % was obtained under different process parameters in a significantly shorter time compared to conventional alkaline pretreatment. Up to 94±4 % of cellulose in treated biomass was converted to glucose after enzymatic hydrolysis, achieving around 3.5 times higher glucose yield than the raw biomass. Different spectroscopic analyses confirmed specific alterations in the structure of the lignin-rich fraction caused by cold plasma. Micro- and nanoscale lignin particles obtained were rich in total phenolic content, reaching up to 140±20 and 107±12 µg gallic acid equivalents (GAE) per mg of lignin, respectively. The proposed concept of corn stalk fractionation through biorefinery can open new opportunities for valorizing different agricultural waste types.
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