efforts have been devoted to remove the aforementioned limitations of the PNIPAM hydrogel sensors by incorporating nanomaterials. [17,18] Recently, low dimensional nanomaterials with a large specific surface area such as carbon nanotubes and graphene oxide have been incorporated to hydrophilic polymers such as PNIPAM, chitosan, and polyacrylic acid hydrogels to enhance the adsorption of substances and chemical storage capacity. [19][20][21] In this study, we demonstrate a composite hydrogel of MoS 2 nanosheets functionalized with 4-mercaptobenzoic acid (MBA) and PNIPAM (MBAMS-PNIPAM hydrogel) for the detection of water-soluble phenols. Herein, MoS 2 nanosheets have been shown to be promising candidate components for various fields, such as the detection of water-soluble substances, humidity, and gas species. [22][23][24][25][26] MBAMS was prepared via MoS 2 exfoliation processes and subsequent chemical functionalization process with 4-MBA for realizing the reactivity and selectivity toward the target substance. Here, 4-MBA, a small ligand molecule with a thiol and a carboxyl group, was used to modify the surface of MoS 2 nanosheets. We also verified that we can adjust the phenol detection range by controlling the adsorption and responsivity of the MBAMS-PNIPAM hydrogel through the amount of the incorporated MoS 2 . In addition, we demonstrate an in situ detection strategy of watersoluble phenols by developing an effective transduction strategy to convert the hydrogel volume change into electronic signals. The novel transduction strategy uses a liquid metal-based capacitive transduction method. Furthermore, combined with a handheld signal processor and home-built data-visualization software, we demonstrate a portable detection instrument for phenolic molecules. The instrument successfully detected resorcinol concentrations as low as 10 mg L −1 . As an example, compared to other sensors using optical or electrical mechanisms, [27][28][29] our hydrogel can be readily integrated with existing ducts, containers, or pipe systems without any additional process. Furthermore, above certain concentrations, the hydrogel color change will be large enough to enable detection with the naked eye. As this strategy enables the simple, one-step, and easy detection, it can be easily extended to detect water-soluble chemicals other than phenols in the future. Figure 1a depicts the molecular structure of MBAMS-PNIPAM hydrogels and the detection mechanism of phenols. The surface of MoS 2 was functionalized with 4-MBA molecules to enhance the reactivity and selectivity toward the target phenolic substance and stabilize the hydrogel structure. The target phenolic molecule A composite structure of molybdenum disulfide (MoS 2 ) nanosheets and poly(N-isopropylacrylamide) (PNIPAM) hydrogel is demonstrated for the selective detection of phenols. The incorporation of MoS 2 with a hydrogel system enhances its adsorption and its volume-change response to phenols. It is verified that the phenol detection range can be adjusted by controlling the ...