<p>The present work focusses on eco-friendly method of aqueous extraction of biologically active compounds from corn silk, a by-product of maize production, collected at dough stage of maturity. Three methods, namely, conventional, ultrasonication and microwave, were evaluated for efficient extraction of corn silk, on the basis of total phenol content and polysaccharide yield. Chemical characterization of corn silk powder was done prior to extraction using fourier infrared transform spectrometry (FTIR) and gas chromatography/mass spectrometry (GC/MS). Among the methods tested, conventional extraction method proved most efficient for extraction of corn silk and high performance liquid chromatography (HPLC) of the extract revealed the presence of chlorogenic acid, rosmarimic acid, ferulic acid, rutin, caffeic and quercetin as major phenolic compounds. Polysaccharides isolated from the extract were evaluated for morphological characteristics using field-emission scanning electron microscopy (FE-SEM). The in vitro anti-diabetic activity studies of corn silk extract revealed high activity (&gt; 80% at the concentration of 400&#xa0;µg/mL) against digestive enzymes used in this study, however, activity was still lower than standard acarbose. Therefore, valorization of corn silk may serve as multifaceted opportunity that addresses environmental, economic and health needs. </p> Graphical Abstract <p></p>