In situ characterization of minute amounts of fluids that rapidly change their rheological properties is a challenge. In this paper, the rheological properties of fluids were evaluated by examining the behavior of magnetic nanorods in a rotating magnetic field. We proposed a theory describing the rotation of a magnetic nanorod in a fluid when its viscosity increases with time exponentially fast. To confirm the theory, we studied the time-dependent rheology of microdroplets of 2-hydroxyethylmethacrylate (HEMA)/diethylene glycol dimethacylate (DEGDMA)-based hydrogel during photopolymerization synthesis. We demonstrated that magnetic rotational spectroscopy provides rich physicochemical information about the gelation process. The method allows one to completely specify the time-dependent viscosity by directly measuring characteristic viscosity and characteristic time. Remarkably, one can analyze not only the polymer solution, but also the suspension enriched with the gel domains being formed. Since the probing nanorods are measured in nanometers, this method can be used for the in vivo mapping of the rheological properties of biofluids and polymers on a microscopic level at short time intervals when other methods fall short.