Rapid, High-Throughput Quantitation of Odor-Active 2-Acetyl Azaheterocycles in Food Products by UHPLC–MS/MS

A rapid, high-throughput method for the quantitation of the 2-acetyl azaheterocycles, 2-acetyl-1-pyrroline, 2-acetyl-1,4,5,6-tetrahydropyridine, 2-acetylpyrazine, and 2-acetyl-2-thiazoline, in different food products, by liquid chromatography-tandem mass spectrometry (LC-MS/MS), was developed. The quick extraction by bead beater homogenization, fast derivatization by 3-nitrophenylhydrazine (40 °C, 2 h), and efficient LC separation make this method suitable for high-throughput analysis. As established in this study, the highly precise LC-MS/MS method applies to different food products or beverages without requiring further adjustment. The analysis was performed with sample amounts of 0.2-0.5 g, and limit of quantitation values of 0.6, 0.5, 0.6, and 1.0 μg/kg were obtained for 2-acetyl-1-pyrroline, 2-acetyl-1,4,5,6-tetrahydropyridine, 2-acetylpyrazine, and 2-acetyl-2-thiazoline, respectively. Thus, it was possible to quantitate the analytes in the range of their odor thresholds.