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Since its early beginnings, the science of chromatographic separations has seen a steady progression of technological advances. Improvements in both chromatographic instruments and stationary phases have led to leaps in separation performance. One of the most significant recent advances in stationary phases was the introduction of hybrid organic/ inorganic particles. Hybrid-based packing materials offer an extended usable pH range compared to that of silica-based packing materials, as well as excellent peak shape and high efficiency. In addition to advances in stationary phase chemistry, the availability of columns containing sub-two micron particles has allowed for dramatic improvements in the speed, sensitivity and resolution of LC separations. However, despite these advances, new challenges continue to emerge, particularly as the result of the increasing use of liquid chromatography/mass spectrometric (LC/MS) methods.