Simultaneous chemical and sensory analysis with multidimensional gas chromatography-mass spectrometry- olfactometry (mdGC-MS-O) combine classic chromatographic separations with sensory analyses. Trained panelist and human nose is used as a detector simultaneously recording olfactory responses (aromagrams) with chemical separations (chromatograms). Analysis of chromatograms and aromagrams enables separation of odor- (or aroma-) causing compounds in very complex matrixes. Multidimensional chromatography by heart-cutting with Dean’s switch enhances chromatographic separations. Combined with the sensory analyses, it allows for isolation and ultimately, identification of odor-causing compounds. Mass spectrometry detection allows for identification and quantification of specific target compounds. The objective of this paper is an introductory overview of simultaneous chemical and sensory analyses using multidimensional GC-MS-Olfactometry.