Several hybrid sensing materials, which are prepared by the covalent grafting of organic fluorescent molecules onto inorganic supports, have emerged as a novel and promising class of hybrid sensing probes and have attracted tremendous interest. In comparison to the organic fluorescent sensors, the hybrid sensing probes incorporate the beneficial chemical/physical properties of the organic molecules and inorganic materials, which accelerate the development of hybrid materials for ion recognition and removal. Hence, the novel hybrid sensing materials can selectively monitor and efficiently remove specific analytes, which can provide a novel opportunity to synthesize multifunctional hybrid materials. Considerable efforts have been devoted to developing effective and innovative approaches for the design and synthesis of hybrid sensing materials that can display highly desirable performance for ion detection and removal. This tutorial review firstly presents a brief description of the hybrid materials and mesoporous silica materials and then classifies the hybrid sensing materials into several categories, including mesoporous silica based hybrid sensors, magnetic core-shell particle based hybrid sensors, magnetic nanoparticle based hybrid sensors, polymer based hybrid sensors, surface-grafted composite based hybrid sensors, and host-guest interaction based hybrid sensors, followed by a detailed summary of the design and synthesis of hybrid sensing materials and their applications in environmental and biological fields. Hopefully, this review will provide perspectives and guidelines for the development and further research of hybrid sensing materials.