The invention relates to a nuclear magnetic resonance method of detecting and monitoring the flocculation kinetics of high molecular weight fractions of a complex fluid. The inventive method applies the following to the fluid: a first static polarization magnetic field and, subsequently, at least a second oscillating pulsed magnetic field which generates a nuclear magnetic resonance for the nuclei considered and the acquisition of relaxation signals from the nuclei in the fluid. Moreover, the method detects, in the relaxation signals, a first part P1 which is representative of the relaxation of the flocculated fractions in the fluid and a second part P2 which is representative of the relaxation of the liquid fraction of the fluid; and determines the flocculation rate of the fractions by comparison with values Mx(t=0) and Mx1(t=0) which were extrapolated at the start of the acquisition times of the two parts. The invention is suitable, for example, for monitoring the flocculation kinetics of generally asphaltene polar fractions which are contained in the dissolved state and/or in the stable colloidal state in a liquid hydrocarbon fluid.