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A temperature controlled proton-transfer ionization(HFI)technique was developed for the mass spectrometric analysis of different polarities organic compounds.A stainless steel t-branch tube was used to control the differentiate flow rate of hydrogen gas and inert gas respectively,thus a series of temperatures of the flame are acquired for thermal desorption ionization of analytesin-situ.The ionization mechanism of HFI-MS was suggested to involve proton-transfer process,and then,analytes ions were formed throughion-molecule reactions between protonated water clusters and the desorption analytes.As a temperature-controlled,non-polluted and convenient ionization method,HFI-MS is mainly for analyzing polar and nonpolar organic compounds,such as trace vapor molecules,food additive,chemical dyes,polymers and olefins.Some of these compounds were ionized and detected in different temperature flame,but not be well-analyzed by electrospray ionization or atmospheric-pressure chemical ionization mass spectrometry.The HFI-MS could not only be used to characterize the real-world samples such as the active ingredients in drug tables and teas,plasticizer in plastic and fragrant citrus pericarps but also be applied to single cell analysis.