Abstract: | Tetramethylpyrazine (TTMP) is a key bioactive alkaloid and flavour compound found in Chinese sesame flavour liquor. Changes in TTMP concentration during the production of sesame flavour liquor have received little attention. Here, TTMP was tracked from raw material, fermented grains and fresh liquor in storage using high‐performance liquid chromatographic–tandem mass spectrometry (HPLC‐MS/MS). The results showed that TTMP was formed during stack fermentation, solid‐state fermentation and distillation, while no TTMP was produced during the storage process of fresh liquor. Furthermore, a higher temperature fermentation and bacterial starter culture were beneficial to TTMP generation. Accordingly, technology strategies for increasing the concentration of TTMP in sesame flavour liquor include raising the temperature of stack fermentation and distillation, reducing the distillation speed and screening for high TTMP producing Bacillus species. © 2018 The Institute of Brewing & Distilling |