Metal deactivator additives (MDAs) have been used for over 60 years to prevent metal catalyzed reactions in petroleum products; a commonly used metal deactivator is N,N'-disalicylidene-1,2-propanediamine. The quantitation of low MDA concentrations in fuels is challenging due to the complexity of the sample matrix. In this work, this difficulty was overcome using GC × GC hyphenated with a nitrogen chemiluminescence detector. The high resolution power of GC × GC avoided co-elution between the MDA and other sample matrix compounds; while the enhanced sensitivity of GC × GC and the use of a nitrogen chemiluminescence detector supplied a high sensitivity and specificity for nitrogen compounds. For the analysis, the MDA additive was derivatized with the silylation agent N,O-bis (trimethylsilyl)trifluoroacetamide at room temperature and its quantitation was based on an external calibration curve; good linear response was obtained in the 1.4-8.6 ppm range.