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Background: A method for the measurement of five important serum and urinary corticoids on the syndrome of mineralcorticoid excess is reported. The methodology was combined gas chromatography-mass spectrometry (GC-MS) with selected ion-monitoring mode. Methods: After extraction with a solid-phase cartridge using an Oasis HLB copolymer, the residues were derivatized with a mixture of N-methyl-N-trimethylsilyltrifluoroacetamide/ammonium iodide/dithioerythritol (1000:4:5, v/w/w), and analyzed. Results: The linearity as the regression coefficients were >0.979 over a range of 1-500 ng/ml, and limit of detection ranged from 1 to 3 ng/ml while their analytical recoveries varied in the range of 75.7-94.9%. The overall precision (% CV) of the method were 3.2-7.2% and 3.6-6.3% for serum and urine, respectively. The accuracy expresses as % bias ranged from -4.1 to 6.4%. This assay was used on two patients with hypokalemic hypertension, and may be useful in ruling out mineralcorticoid excess (AME) type 1 or 2. Conclusions: The present GC-MS technique may be useful to differentiate between the syndrome of AME and other hypertensive diseases with clinical features suggestive of mineralcorticoid excess because of the assay’s reliability and precision. (C) 2002 Elsevier Science B.V. All rights reserved.