Abstract:　During　the　processing　of　maize,　Stigma　maydis,　also　known　as　corn　silk,　is　normally　discarded　as　waste.　Phytochemical　research　was　carried　out　on　the　S.　maydis　to　use　it　as　a　valuable　source　of　bioactive　components.　This　research　aimed　to　maximize　the　recovery　of　free　and　bound　phenolic　compounds　from　corn　silk　under　optimal　experimental　conditions.　Response　surface　design　was　operated　to　optimize　the　alkaline　hydrolysis　extraction　of　bound　phytochemicals　from　corn　silk　based　on　total　phenolic　content　and　DPPH　radical　scavenging　activity.　The　optimum　conditions　(i.e.,　NaOH　concentration　2 M,　digestion　time　135 min,　digestion　temperature　of　37.5°C,　the　solid-to-solvent　ratio　of　1:17.5,　and　acetone)　were　obtained.　The　optimum　parameters　were　used　to　extract　the　corn　silk.　The　structures　of　two　compounds　isolated　from　ethyl　acetate　extracts　were　then　identified　as　friedelin　(1)　and　(E)-4-(4-hydroxy-3-methoxyphenyl)　but-3-en-2-one　(2).　The　DPPH,　H2O2,　and　ABTS　%　inhibition　of　the　compounds　is　as　follows:　compound　(1)　74.81%,　76.8%,　70.33%　and　compound　(2)　70.37%,　56.70%　and　57.46%,　respectively.　The　current　study　has　opened　previously　unexplored　perspectives　of　the　composition　of　bound　compounds　in　corn　silk　and　established　the　foundations　for　more　effective　processing　and　utilization　of　corn　waste.　Practical　Application:　Bound　phenolic　compounds　from　corn　silk　under　optimal　experimental　conditions　were　obtained.　Corn　silk　can　be　utilized　as　a　type　of　medicinal　herb　as　well　as　a　source　of　inexpensive　natural　antioxidants.　©　2023　Institute　of　Food　Technologists.