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A highly sensitive and selective method was developed for both UV-vis spectrophotometric and fluorimetric determination of organophosphorus pesticides (OPs). This method used silver nanoparticles (AgNPs) modified with graphitic carbon nitride (g-C3N4). The AgNPs reduced the fluorescence intensity of g-C3N4. Acetylthiocholine (ATCh) could be catalytically hydrolyzed by acetylcholinesterase (AChE) to form thiocholine, which induces aggregation of the AgNPs. This aggregation led to the recovery of the blue fluorescence of g-C3N4, with exc