Disclosed is a two-dimensional separation system, comprising a liquid chromatography column having an outlet port; a capillary electrophoresis capillary having an inlet end and an outlet end; buffer supply means for supplying buffer to the capillary; and valve means connecting the capillary inlet end to the chromatography column outlet port and to the buffer supply means, the valve means switchable between a first configuration providing fluid to the capillary inlet end from the buffer supply means and a second configuration providing fluid to the capillary inlet end from the chromatography column. Methods of carrying out two- dimensional separations employing the system are also disclosed.
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