The use of on‐line mass spectrometry to measure aroma release from model systems, or from people consuming food or beverages, delivers time‐based aroma release curves that relate better to sensory perception. The technique allows the rapid analysis of the headspace above foods as well as the measurement of the performance of flavour systems in manufactured foods during consumption. The data obtained can give quick insights into the potential success of a flavouring and on‐line mass spectrometry is widely used in the food and flavour industries. The speed of data acquisition, sensitivity to a wide range of chemical compounds, and resolution of compounds with the same nominal mass are recurring issues for on‐line analysis. Here, we present a study of the performance of an atmospheric pressure chemical ionization (APCI) source connected to a triple quadrupole mass spectrometer. Fast data acquisition could be achieved with little loss of ion signal but with slightly increased noise. In ‘Multiple Reaction Monitoring’ mode, sensitivity increased appreciably for six out of the seven compounds tested, and changing the collision energy of the system produced different mass spectral patterns for six compounds with the same nominal mass. The application of some of these techniques to coffee analysis identified the challenges and approaches needed to provide an in‐depth analysis for real samples.
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