In biochemical sensing, substantial progress has been achieved in the design, development, and application of metallic nanoclusters (NCs) and metal-organic frameworks (MOFs) as distinct entities. Integration of these two nanostructured materials is a promising strategy to form innovative composites with improved properties. Some improvements include (i) supporting platform to minimize the aggregation of NCs and enhance the emission efficiency
(ii) dual-emitting NCs@MOFs from the fluorescent/non-fluorescent MOFs and/or fluorescent NCs
and (iii) stability enhancement. These improvements increase the sensitivity, signal-to-noise ratio, and color tonality, lower the limit of detection, and improve other analytical figures of merits. In this review, we outline the preparation methods of NCs@MOF composites with the improvements offered by them in the field of biochemical analysis. Analytical applications in different fields, such as bioanalysis, environmental monitoring and food safety, are presented. Finally, we address the challenges that remain in the development and application of these composites, such as ensuring stability, enhancing the fluorescence intensity, and improving selectivity and scalability. Furthermore, perspectives on future research directions in this rapidly evolving field are offered.