A novel fluorescent probe was designed and synthesized from tetraphenylethene (TPE) and polyhedral oligomeric silsesquioxanes (POSS) via Heck‐palladium catalyzed cross‐coupling reaction. The as‐synthesized TPE functionalized probe performed good solvent stability and selectively preconcentration capability towards target analyte due to its stable structure and the adsorption property. The morphology as well as the physical and chemical properties of the POSS@TPE were carefully characterized. The POSS@TPE was employed to develop an effective fluorescent probe for trifluralin, with a response range of 0.1‐80 mg/kg and a detection limit of 0.102 mg/kg. The mixed mechanisms of inner‐filter effect (IFE) and photoinduced electron transfer (PET) explain the selectivity of POSS@TPE. Rapid detection for trifluralin in tomato and celery has been achieved with recoveries between 99.4–120.7% (RSD≤3.4%), and the results were verified compared with GC‐MS method.

Cyanide anion (CN-) in diet may cause serious health risk, asking for sensitivity, selective, and rapid detection method, especially in on-site test. In this work, a novel bisspiropyran (SP1) fluorescent...