A biogenic approach, particularly plant-mediated synthesis, is currently regarded as the sustainable approach for
synthesizing nanomaterials (NMs). The present investigation concentrates on the green fabrication of Ag/Ag2O
nanoparticles (NPs), ZnO NPs, and Ag/Ag2O/ZnO nanocomposites (NCs) via microwave irradiation using Murusi
peel (MP) and Kew peel (KP) aqueous extracts and comparatively determine their antioxidant potentials. The
synthesis parameters of Ag/Ag2O NPs, ZnO NPs, and Ag/Ag2O/ZnO NCs were optimized and characterized using
different analytical techniques. Surface plasmon resonance peaks appeared at 448–450 nm, 350–370 nm, and
400–500 nm for Ag/Ag2O NPs, ZnO NPs, and Ag/Ag2O/ZnO NCs, respectively. The scanning electron microscopic
images of both peel-mediated Ag/Ag2O NPs depicted quasi-spherical shapes aggregating on the flakeshaped
ZnO surface, leading to the Ag/Ag2O/ZnO NCs formation. Transition electron microscopic analysis
revealed the average particle sizes of MP and KP-mediated Ag/Ag2O NPs, ZnO NPs, and Ag/Ag2O/ZnO NCs as
13.58±1.32 nm, and 36.79±1.24 nm, 13.00±1.26 nm, and 10.28±1.25 nm, 28.37±1.39 nm, and 11.21±1.06
nm, respectively. X-ray diffraction analysis confirmed the synthesis of pure crystalline structures with a hexagonal
wurtzite structure for ZnO and a face-centered structure for Ag and Ag2O during the formation of Ag/
Ag2O/ZnO NCs. According to the research findings, MP and KP-mediated Ag/Ag2O/ZnO NCs displayed an
enhanced free radical scavenging effect for DPPH (2,2-diphenyl-1-picrylhydrazyl) assay with IC50 values of 54.13
±0.53 ppm and 51.41±1.27 ppm, respectively. At higher concentrations, the NCs exhibited a greater radical
scavenging potential for ABTS (2,2′-azino-bis (3-ethylbenzothiazoline-6-sulfonic acid) assay, with the IC50 values
for MP and KP-mediated as 72.28±0.83 ppm and 65.78±1.29 ppm, respectively. Similarly, for the FRAP (Ferric
reducing antioxidant power) assay, MP and KP-mediated Ag/Ag2O/ZnO NCs demonstrated a higher antioxidant
potential, expressed in terms of ascorbic acid equivalents (AE), which were 46±0.7 (AE) mg/1 g and 50±1.1 (AE)
mg/1 g, respectively. To the best of our knowledge, this study remains the first comparative analysis of synergistically
enhanced antioxidant potential of the agro-waste mediated Ag/Ag2O/ZnO NCs with their respective
NPs counterparts, Ag/Ag2O NPs and ZnO NPs. These research findings pave the path for sustainably utilizing
these NMs in biomedical applications.