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Abstract. Capillary zone electrophoresis (CZE) coupled with an on-line mass spectrometric (MS) detection system by an atmospheric pressure electrospray ionization (ESI) interface has been used successfully for separations of peptide and protein mixtures. For CZE-MS, ESI produces multiply charged molecular ions and thus allows m a s spectrometers with a limited mass-to-charge range to analyze proteins having molecular weights greater than 100,000. Various pH buffer systems have been investigated, including buffer systems in which pH > p1 (isoelectric point of analytes) and pH << pl are designed to reduce protein adsorption onto silica capillary surfaces and thus improve separation efficiencies. More than 125,000 theoretical plates have been obtained from a CZE-MS separation of less than 1 pmol per component of leucine enkephalin and horse heart myoglobin. CZE-MS of other large peptides and proteins are demonstrated.

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