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A rapid and sensitive LC MS/MS method for the simultaneous quantitation of lamivudine, zidovudine and nevirapine in human plasma using abacavir as internal standard has been developed and validated. The analytes and IS were extracted from plasma by solid phase extraction using Oasis HLB cartridges and separated on a Hypurity Advance C18 column using a mixture of acetonitrile:0.10/. formic acid (76:24, v/v) at a flow rate of 0.8 mL/min. Detection involved an API4000 LC MS/MS with electrospray ionization in the positive ion mode and multiplereaction monitoring for analysis. The method was validated according to FDA guidelines and shown to provide intra- and interday precision and accuracy within acceptable limits in a run time of only 3.5 min. The method was successfully applied to a pharmacokinetic study involving a single oral administration of a combination tablet to human male volunteers. (C) 2012 Institute of Materia Medica, Chinese Academy of Medical Sciences and Chinese Pharmaceutical Association. Production and hosting by Elsevier B.V. All rights reserved.