Important advances in chemical and flavor knowledge are possible through improved analytical separation and identification. Along with greater separation power, both a more robust analysis and an improved identified sample composition result. In this paper, a number of new integrated methods are explored that permit improved resolution and superior analyses for a range of studies. These methods focus on multidimensional gas chromatography (MDGC), comprehensive two-dimensional gas chromatography (GCxGC), olfactometry, mass spectrometry, and nuclear magnetic resonance (NMR) spectroscopy. The overriding objective is to provide technical solutions that employ the best possible separation of compounds, allowing tools such as olfactometry, mass spectrometry, NMR spectroscopy, and other detectors to provide much better characterization of separated chemical species. Various novel strategies are demonstrated that provide the necessary increased separation power, integrated with specific detection steps. Case studies presented include the sensory-directed identification of a woody odorant in hop essential oil, correlation of compound identifications in coriander leaf, and development of new preparative isolation capabilities using MDGC with NMR spectroscopy.