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In this study, the detailed volatile compositions of Chinese herbaceous aroma-type Baijiu (HAB) were characterized by comprehensive two-dimensional gas chromatography-time of flight mass spectrometry (GC×GC-TOFMS). A total of 606 compounds were tentatively identified by similarity, mass spectral data, and retention indices, among which 247 compounds were positively verified by authentic standards. Esters were present in higher numbers (179), followed by aldehydes and ketones (111), and alcohols (81). In addition, there were also many terpenes (82), sulfides (37), furans (29), nitrogenous compounds (29), lactones (17), and so on. Meanwhile, the extraction effects of volatile components from different sample pretreatment methods (headspace solid-phase microextraction (HS-SPME), solid phase extraction (SPE), and stir bar sorptive extraction (SBSE)) for HAB were also revealed. The results indicated that HS-SPME has a better extraction effect on easily volatile compounds, such as alcohols and sulfides, especially for terpenes. SPE was particularly beneficial for the analysis of nitrogen-containing compounds; SBSE showed medium extraction ability for most types of compounds and was more suitable for the target analysis of trace content substances.

Three Extraction Methods in Combination with GC×GC-TOFMS for the Detailed Investigation of Volatiles in Chinese Herbaceous Aroma-Type Baijiu