Studying dynamic aroma release by headspace-solid phase microextraction-gas chromatography-ion mobility spectrometry (HS-SPME-GC-IMS): method optimization, validation, and application

To understand aroma perception from complex food matrices, determination of dynamic aroma release during simulated oral processing is necessary. In this study optimization, validation and application of a novel method coupling headspace-solid phase microextraction (HS-SPME) with gas chromatography-ion mobility spectrometry (GC-IMS) is presented. Thirteen character impact compounds imparting different chemical properties are studied to understand capabilities and limitations of the method. It was shown for the first time that the temperature of the IMS sample inlet can be increased up to 200 degrees C without instrumental constraints. Linear calibration was possible for eleven of the thirteen compounds with one decade dynamic range. The limit of detection and quantitation were 2.1-63.0 ppb and 7.2-210.1 ppb, respectively. Diacetyl could be detected in negative polarity mode of IMS, however with lower precision compared to the compounds detected in positive mode. Limitations of the method were short HS-SPME extraction time, which in the case of caproic acid was not sufficient for reliable quantification. Additionally, delta-decalactone could not be detected due to maximum GC temperature of 200 degrees C. Application of the method to determine dynamic aroma release from a dairy matrix was successfully shown for nine compounds. Analysis of complex food matrix was performed with similar precision compared to analysis in aqueous solution, thus proving high robustness of the method towards matrix effects.

Automated summary

A novel method coupling HS-SPME with GC-IMS was developed for analyzing dynamic aroma release from complex food matrices, showing promising results in detecting and quantifying thirteen character impact compounds. The method demonstrated advantages such as adjustable IMS sample inlet temperature, broad linear calibration range, reasonable detection and quantitation limits, while also revealing limitations such as short HS-SPME extraction time.