The application of electrochemically prepared Ag nanostructures (NSs) for fast monitoring of sulfur containing organophosphonates, ethion, malathion and fenthion, in real two natural matrices, tap-water and apple juice, has been investigated using localized surface plasmon resonance and electrochemical techniques. The results show a limit of detection of 10 μM for ethion and 100 μM for malathion and fenthion.