Recent years, carbon nitride (C3N4) nanomaterials have engraved new insights into fluorescence spectrometry for the analysis of wide variety analytes (metal ions, organic and biomolecules). This review concentrates on the properties of C3N4 nanomaterials, synthetic routes for C3N4 nanomaterials and insights in fluorescence spectrometry for the detection of various chemical species. Firstly, this review summarizes the properties (photoluminescence, electrochemical, thermal and chemical stability) of C3N4 nanostructure materials. Secondly, the recent advances on the synthetic routes for the fabrication of C3N4 nanostructures including top‐down (hydrothermal, solvothermal and exfoliation) and bottom‐up (hard and soft templet, template‐free, solvothermal, hydrothermal and microwave) are discussed. Thirdly, we describe the new insights of C3N4 nanostructures as probes for assaying of metal ions, organic and biomolecules from complex samples via fluorescence spectrometry. Finally, we have summarized the future perspectives of carbon nitride nanostructures in analytical chemistry are described.