Dual‐Responsive and Aggregation‐Induced‐Emission Probe for Selective Imaging of Infectious Urolithiasis

Abstract Identifying infected stones is crucial due to their rapid growth and high recurrence rate. Here, the calcium–magnesium dual‐responsive aggregation‐induced emission (AIE)‐active probe TCM‐5COOH (Tricyano‐methlene‐pyridine‐5COOH), distinctively engineered to distinguish high‐threat infection calculi from metabolic stones, is presented. Upon incorporation of flexible alkyl carboxyl group, TCM‐5COOH featuring five carboxyl moieties demonstrates excellent water solubility and enhanced penetration into porous infectious stones. The robust chelation of TCM‐5COOH with stone surface‐abundant Ca 2+ and Mg 2+ inhibits vibrational relaxation, thus triggering intense AIE signals. Remarkably, the resulting complex exhibits high insolubility, effectively anchoring within the porous structure of the infection calculi and offering prolonged illumination. Jobs’ plot method reveals similar response characteristics for Ca 2+ and Mg 2+ , with a 1:2 coordination number for both ions. Isothermal titration calorimetry (ITC) results demonstrate higher enthalpy change (Δ H ) and lower entropy change (Δ S ) for the reaction, indicating enhanced selectivity compared to TCM‐4COOH lacking the alkyl carboxyl group. Synchrotron X‐ray absorption fine spectroscopy (XAFS) validates TCM‐5COOH's interaction with Ca 2+ and Mg 2+ at the microlevel. This dual‐responsive probe excels in identifying infectious and metabolic calculi, compatible with endoscopic modalities and laser excitation, thereby prompting clinical visualization and diagnostic assessment.