Simultaneous Determination of 28 Food-Derived Metabolic Modulators in Instant Foods by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry with Automatic Dispersive Solid Phase Extraction

In view of the contamination risk of food-derived metabolic modulators caused by factors such as their residues in food raw materials and their illegal addition in instant foods, as well as the limitations of existing detection technologies such as mismatched matrix, small risk coverage, and complex analysis processes, an analytical method for the rapid determination of 28 food-derived metabolic modulators in instant foods was developed using automatic dispersive solid phase extraction (auto-dSPE) coupled with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The samples were extracted with 0.1% formic acid in acetonitrile, purified by matrix solid-phase dispersion extraction (MSPD), and separated by on a Shimadzu Shim-pack GIST C₁₈-AQ column (2.1 mm × 100 mm, 1.9 μm). Detection was performed using electrospray ionization (ESI) in both positive and negative ion modes. Data acquisition was performed using multiple reaction monitoring (MRM) and quantitation of each analyte was carried out using an external standard method. Under the optimal conditions, the 28 metabolic modulators had good linear relationship in their respective concentration ranges, with determination coefficients (R²) greater than 0.994. The detection limit of the developed method was between 0.05 and 2.0 μg/kg, and the quantification limit was between 0.1 and 5.0 μg/kg. The average recoveries from cereal protein bar and bread ranged from 63.4% to 112.0%, with relative standard deviations (RSDs) ranging from 1.4% to 17.7% (n = 6). This method was characterized by high automation, fast analysis speed, high sensitivity, accuracy and stability, and could meet the demand for rapid screening of the 28 food-derived metabolic modulators in instant foods.