Recently, metal organic frameworks (MOFs) have received intensive research interest as an important family of functional materials. In particular, MOFs were widely used in electroanalysis and water splitting for their electrical conductivity and rich redox electrochemical activities. Prussian blue analogue (PBA), which owns hollow nanostructured MOFs with large surface area and unique structural features, offers great advantages for constructing advanced electrodes. Meanwhile, compared with platinum-based catalysts, molybdenum disulfide (MoS2) is increasingly becoming a research focus as an affordable alternative obtaining electrochemical hydrogen production from water. Here we synthesized the nano materials, MoS2-Co nanoboxes, using the facile hydrothermal method between cobalt Prussian blue analogue (Co PBA) nanocubes and ammonium thiomolybdate ((NH4)(2)MoS4). In acid and alkaline media, the MoS2-Co nanoboxes exhibit favorable catalytic performance for the hydrogen evolution reaction (HER). Furthermore, for researching the relationship of structural changes of MoS2 supported on Co PBA nanocubes and HER catalytic performance, we use the Raman spectroscopy to monitor nanostructured MoS2 which can promote the exposure of the most active sites. This new method applied in this study can be widely adopted for characterization of transition metal dichalcogenides with various compositions for a wide range of applications. (C) 2018 Elsevier Ltd. All rights reserved.