Abstract: In this study, two methods were established for the determination of the content and homologue composition of alkylresorcinols (ARs) in wheat flour, namely gas chromatography-mass spectrometry (GC-MS) and liquid chromatography-tandem mass spectrometry (LC-MS/MS). The sample was ultrasonically extracted with ethyl acetate. The extract was derivatized by silanization before GC-MS analysis in the selected ion monitoring (SIM) mode. Quantification was performed the by external standard method. Before LC-MS/MS, the extract was enriched and purified by solid phase extraction (SPE) on a C18 chromatographic column, and the separated analytes were detected in the negative ion scanning mode using multiple reaction monitoring (MRM) and quantified similarly by the external standard method. The results showed that both methods exhibited a good linear relationship in the concentration range of 0.001–5 μg/mL. The detection limit of the GC-MS method was 2.0–6.1 μg/g, and the spiked recoveries were 94.17%–99.15%, with relative standard deviation (RSD) of 2.94%–4.87%. The detection limit of the LC-MS/MS method was 2.0–8.4 μg/g, and the spiked recoveries were 89.05%–99.06%, with RSD of 2.21%–4.17%. These two detection methods, thanks to their good liner relationship, low detection limit, and high sensitivity, could be suitable for the qualitative and quantitative analysis of AR homologues in commercially available wheat flour products, which will provide a technical reference for the quality control and detection of whole-grain wheat products.

Key words: alkylresorcinols; wheat flour quality; gas chromatography-mass spectrometry; liquid chromatography-tandem mass spectrometry; ultrasonic extraction; purification