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RATIONALE The capabilities of modified non-spherical Doehlert-type experimental designs to optimize the performance of a hybrid mass spectrometer were investigated in this paper for the first time. The optimization process was completed in three successive steps with groups of variables avoiding any univariable approach. Glutathione (GSH, reduced) was selected as a very interesting analyte since it is considered to be one of the most abundant tripeptides in human organism and its action against xenobiotics and oxidative radicals is well known. METHODS In particular, a tandem technique based on sequential ion management by an ion trap followed by a time-of-flight mass analyzer (ITTOFMS) was introduced commercially in recent years and investigated for glutathione determination. Glutathione was injected in a stream of a typical mobile phase used in liquid chromatography (LC) and analyzed after electrospray ionization (ESI) in tandem MS. RESULTS The three main steps of the LC/MS system, namely the LC mobile phase, the ESI interface and the MS analyzer, were independently optimized in terms of maximum sensitivity. In this context quadratic models were found and their prediction power was evaluated. A calibration study was performed at default and optimum conditions in order to quantitatively estimate the sensitivity enhancement of the employed technique for this analyte. Satisfactory precision (RSD 5.7%) and detectability (LOD 0.07 µmol L-1) were achieved. CONCLUSIONS The results highlighted the possibilities offered by the employment of multifactorial optimization towards the improvement of performance of tandem mass spectrometry techniques. Copyright © 2012 John Wiley & Sons, Ltd. [ABSTRACT FROM AUTHOR]