A　simple　and　sensitive　method　has　been　developed　for　the　simultaneous　determination　of　polar　nonsteroidal　pharmaceuticals　and　metabolites,　including　acetaminophen,　p-aminophenol　and　several　aspirin　metabolites　(salicylic　acid,　gentisic　acid,　salicyluric　acid　and　2,3-dihydroxybenzoic　acid),　by　capillary　liquid　chromatography　with　amperometric　detection.　Using　a　capillary　monolithic　column　with　mixed　mode　stationary　phases　and　a　mobile　phase　composed　of　acetonitrile　and　Tris　buffer,　rapid　separation　of　six　polar　analytes　was　achieved　within　8　min,　and　a　hydrophilic　interaction　and　strong　anion　exchange　separation　mechanism　were　exhibited.　Method　detection　limits　of　six　analytes　ranged　from　10　to　50　ng/mL.　In　terms　of　precision,　the　intra-　and　interday　relative　standard　deviation　values　in　all　analytes　never　exceeded　3.1%　for　migration　time　and　8.9%　for　peak　areas,　respectively.　This　method　provided　a　simple,　rapid　and　cost-effective　approach　for　the　analysis　of　polar　pharmaceuticals.　The　applicability　of　the　method　in　pharmacokinetics　was　verified　by　spiking　human　serum　samples　with　the　compounds　and　analyzing　the　recoveries.　Copyright　©　2011　WILEY-VCH　Verlag　GmbH　&　Co.　KGaA,　Weinheim.