AbstractThe increased separation efficiency afforded by reducing the size of the separation column has resulted in ‘microseparations’ becoming an important component in many chemical and biochemical applications. The coupling of microseparations with NMR detection is an area of increasing interest owing to the high structural information of NMR. In order to couple efficiently with the separation, the NMR detector must be reduced in size to correspond to that of the separation peak. This paper summarizes some of the approaches used in coupling NMR detection with pressure‐driven and electrophoretic microseparations, the design of small NMR detectors and applications of this technology. Copyright © 2005 John Wiley & Sons, Ltd.