Schematic diagram of the LC-MS-NMR platform, as applied to natural product discovery. The complex sample (bioactive fraction) is separated using high-resolution LC with UV and MS data acquired online. 98% of the eluent is directed to a UV-guided fraction collection. Fractions are concentrated by drying and may be stored. For NMR, fractions are resuspended in a small volume (2−5 μL) of deuterated solvent and loaded into a microcoil NMR probe, with an observed volume of 1−2 μL, using microplate automation. Samples are recovered after NMR analysis for additional analyses, archival or bioassay.