The　objective　of　this　study　was　to　prepare　a　coated　capillary　to　achieve　rapid　analysis　of　peptides　and　amino　acids　(AAs)　by　CE-ESI-MS.　The　coated　capillary　was　prepared　by　chemical　modification　of　the　fused　silica　(FS)　capillary　with　2-acrylamido-2-methyl-1-propanesulfonic　acid　(AMPS)　via　a　silanization　reaction　followed　by　an　on-column　in　situ　graft　polymerization.　In　preparing　capillary　coating,　AMPS　was　introduced　for　the　following　two　purposes:　first,　to　achieve　strong　and　stable　EOF　in　a　wide　pH　range,　and　second,　to　obtain　good　repeatability　of　separations　of　peptides　and　AAs　by　reducing　their　adsorption　to　the　FS　capillary.　The　inner　wall　morphology,　the　characteristics　of　EOF,　and　the　performances　of　coated　capillary　including　separation　ability,　repeatability,　and　stability　were　investigated　in　detail　and　evaluated　by　analyses　of　four　peptides　(D-Ala-DAla,　Gly-Gly-L-Leu,　Gly-D-Phe,　and　L-Leu-D-Leu)　and　three　AAs　(glycine,　glutamic　acid,　and　phenylalanine),　respectively.　Under　the　optimized　conditions,　the　analysis　times　of　four　peptides　and　three　AAs　in　the　coated　capillary　were　5.6　and　6.0　min,　respectively,　i.e.　much　shorter　than　those　in　the　bare-FS　capillary,　20　and　26　min,　respectively.　These　coated　capillaries　were　shown　to　be　well　suitable　for　CE　coupling　with　ESI-MS　to　analyze　peptides　and　AAs　thanks　to　high　separation　power,　short　analysis　times,　good　repeatability　and　high　stability.　©　2009　Wiley-VCH　Verlag　GmbH　&　Co.　KGaA.