Structural characterization of active substances and their impurities is a common task during Discovery and Development of pesticides and fungicides in the Agrochemical industry. Nuclear magnetic resonance (NMR) spectroscopy and Liquid Chromatography-Mass spectrometry (LC-MS) are routinely used for the characterization of such chemicals. Isolation of low-level impurities in sufficient quantities is often necessary to obtain good NMR and MS data. Preparative and semi-preparative chromatography as well as solid-phase extraction (SPE) techniques are commonly used for the separation, fractionation and isolation of impurities. Our group has recently purchased and installed a hybrid LC-SPE system for isolation of relevant impurities. This talk will describe the hybrid LC-SPE system and its application to our structural characterization workflow.