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Odorous emissions from wastewater treatment plants (WWTPs) cause negative impacts on the surrounding areas and possible health risks on nearby residents. However, the efficient and reliable identification of WWTPs’ odorants is still challenging. In this study, odorous volatile organic compounds (VOCs) from domestic wastewater at different processing units were profiled and identified using gas chromatography-ion mobility spectrometry (GC-IMS) and gas chromatography quadrupole-time-of-flight mass spectrometry (GC-QTOF-MS). The GC-QTOF-MS results confirmed the odor contribution of sulfur organic compounds in wastewater before primary sedimentation and ruled out the significance of most of the hydrocarbons in wastewater odor. The problems in odorous compounds analysis using GC-QTOF-MS were discussed. GC-IMS was developed for visualized analysis on composition characteristics of odorants. Varied volatile compounds were detected by GC-IMS, mainly oxygen-containing VOCs including alcohols, fatty acids, aldehydes and ketones with low odor threshold values. The fingerprint plot of IMS spectra showed the variation in VOCs’ composition, indicating the changes of wastewater quality during treatment process. The GC-IMS technique may provide an efficient profiling method for the changes of inlet water and performance of treatment process at WWTPs.