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In the work, infrared-assisted extraction (IRE) followed by headspace solid-phase microextraction was developed for rapid determination of paeonol in the Traditional Chinese medicine (TCM) Cortex Moutan.Using the proposed method, paeonol in Cortex Moutan was fast isolated by using IRE, followed by extraction and concentration by HS-SPME, and detected by gas chromatography-mass spectrometry (GC-MS).The experiment parameters of IRE and HS-SPME were investigated, and the method precision and recovery were also studied.