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In bioanalytical LC-MS/MS matrix effects influencing the ionization process are a major concern with respect to the quality of the results obtained.In general such matrix effects are directly related to an insufficient sample clean-up of the biofluids.In order to establish a MS-adequate clean-up procedure for basic analytes present in biofluids (e.g.urine, plasma) which is based on solid-phase extraction (SPE) principles a combination of tailor-made SPE column packings and automated column-switching was developed.This novel, multidimensional (MD) SPE platform relies on the combination of a SPE column packed with a restricted access material (RAM) allowing size-exclusion and reversed phase chromatography (SEC-RPC) and a second SPE column packed with a mixed-mode phase (MMP) allowing ion exchange and reversed phase chromatography (IEX-RPC).