Delivery of lipophilic compounds in nano-encapsulated edible form has received growing attention both by research groups and industry. A novel multilayer oil-in-water (M-O/W) emulsion system was developed as a carrier for non-polar compounds, and has been shown to be stable over a wide range of environmental conditions. M-O/W emulsion systems offer an enhanced ability, over single-layer emulsions, to design interfacial layers according to required function. In this study, the role of low-fat (5% wt) M-O/W emulsions as a carrier for volatile organic compounds (VOCs) with controlled release using internal triggers (pH and salt) was investigated. The M-O/W emulsions consisted of β-lactoglobulin (βLG) and pectin layers which are known to bind VOCs. The release of VOCs with different physiochemical properties from aqueous solutions and emulsion systems was determined using static and dynamic headspace methods. The partition coefficients (K) between the aqueous and oil phases were calculated using the phase ratio variation (PRV) method, and showed different volatile release profiles for each emulsion type. An increase in the VOC release was found for the unstable primary emulsion at pH 5, whereas the M-O/W emulsion was stable at the same pH and retained, to a greater extent, the hydrophobic VOCs. Hydrophobic interactions and hydrogen bonds with a secondary dense layer of pectin facilitated this retention. An increase in the ionic strength acted as a release trigger to detach the pectin from the interface and diminish the hydrophobic barrier. The results of this study demonstrate the capability of using M-O/W emulsions for controlled release of VOCs, as well as an alternative system to create stable emulsions with similar VOC release profiles (Fig.1). To further explore this, we have developed a mechanical model mouth interfaced with proton transfer reaction mass spectrometry (PTR-MS) for rapid analysis of volatile release under swallowing conditions.