Nitrogen and sulfur codoped carbon-based dots (N,S-CDs) with strong blue light emission are encapsulated into red light-emitting europium metal-organic frameworks (Eu-MOFs) to form two color light-emitting nanohybrids (Eu-MOFs/N,S-CDs). In organic solvents, the encapsulated N,S-CDs are aggregated and confined in the cavities of the Eu-MOFs, exhibiting only a very weak photoluminescence (PL) signal. Therefore, the nanohybrids show red light emission of the Eu-MOFs. Contrarily, when the Eu-MOFs/N,S-CDs are dispersed in water, the encapsulated N,S-CDs are released into solution while the red light emission of the Eu-MOFs is quenched due to the effect of O-H oscillators. The nanohybrids are used as the probe for the water content in organic solvents. Take ethanol as an example; as the water content is increased from 0.2 to 30%, the nanoprobe provides distinguishable PL color change. The ratio of light intensity at 420 nm to that at 623 nm (I420/I623) increases linearly with increasing water content in the range from 0.05 to 4% with a low detection limit of 0.03%.