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Despite being considered ergolytic drugs, diuretics have been included on the lists of prohibited substances of the International Olympic Committee since 1986 due to their capacity of masking doping agents in urine. As diuretics are also prone to be misused regarding weight categories, screening procedures to check their presence in urine, whenever doping control is involved, are mandatory. A simple screening method using liquid‐liquid extraction was validated for the compounds: acetazolamide, amiloride, bumetanide, chlorthalidone, clopamide, furosemide, hydrochlorothiazide, piretamide, spironolactone, and triamterene. Urine samples were extracted in both acidic and basic media. HPLC analyses were performed with a Spherisorb ODS column and diode array UV detector, set at 260, 270, and 360 nm wavelengths. A gradient mobile phase was used. Limits of detection varied from 0.09 to 0.75 µg/mL. Recoveries ranged from 55.26 to 94.82%. Inter and intra‐assay precision tests showed good values.