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Allopurinol is used widely for the treatment of gout,but its pharmacokinetics is complex and some patients show hypersensitivity,necessitating careful monitoring and improved detection methods.In this study,a sensitive and reliable liquid chromatography-tandem mass spectrometry method was developed to determine the concentrations of allopurinol and its active metabolite oxypurinol in human plasma and urine using 2,6-dichloropurine as the internal standard (IS).Analytes and the IS were extracted from 0.5 ml aliquots of plasma or urine using ethyl acetate and separated on an Agilent Eclipse Plus C18 column using methanol and ammonium formate – formic acid buffer containing 5 mM ammonium formate and 0.1 % formic acid (95:5,v/v) as the mobile phase (A) for allopurinol or methanol plus 5 mM ammonium formate aqueous solution (95:5,v/v) as the mobile phase (B) for oxypurinol.Allopurinol was detected in positive ion mode and the analysis time was about 7 min.