Abstract: | Complete GC–SIM/MS separation and identification of 19 steroids (including several steroid isomers) in a male urine sample, as their per-trimethylsilyl ethers, is described. Trimethylsilylation of their functional groups (hydroxyl and carbonyl) was achieved by a rapid, simplified and one-step derivatization method, using N -methyl- N -trimethylsilyl-2,2,2,-trifluoroacetamide as the silylating agent and the solvent as well, along with catalytic amounts of trimethylsilyl iodide and dithioerythritol. Furthermore, a GC/MS method for the analysis of a synthetic mixture of underivatized urinary steroids is proposed. © 1997 by John Wiley & Sons, Ltd. |