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.

A method for the determination of 14 human milk oligosaccharides (HMOs) in infant formula milk powder was established by hydrophilic interaction liquid chromatography-tandem mass spectrometry (HILIC-MS/MS). The sample was deproteinized by ethanol precipitation and degreased by freezing prior to separation by HILIC. The analytes were detected by multiple reaction monitoring (MRM) and quantified by an external standard method. Under optimized conditions, all HMOs showed good linear relationships within their respective concentration ranges, with determination coefficients (R²) greater than 0.994. The average recovery rates from blank goat’s and cow’s milk powders at three spiked levels ranged from 90.3% to 109.2%, with relative standard deviation (RSD) in the range of 0.7%–9.7% (n = 6), and the limit of detection (LOD) between 0.002 and 0.048 μg/mL. The developed method is characterized by fast analysis speed, high sensitivity and good accuracy, and meets the requirements for the rapid detection of the 14 HMOs in infant formula milk powder.

This study established a method for the determination of pyrroloquinoline quinone (PQQ) disodium salt, a newly approved food ingredient in China, in foods using centrifugal ultrafiltration as a novel pretreatment technique combined with high performance liquid chromatography (HPLC). Ethylenediaminetetraacetic acid disodium (EDTA-2Na) solution was used as a stabilizing agent in sample extraction. After purification by centrifugal purification, chromatographic separation was accomplished on a RD-C₁₈ column (4.6 mm × 150 mm, 5 μm) with gradient elution using a mobile phase consisting of tetrabutylammonium bromide-potassium dihydrogen phosphate mixed solution and acetonitrile. Detection was carried out using a photodiode array detector. The calibration curve showed good linearity within the concentration range of 0.0400–10.0 mg/L with a determination coefficient of 0.9998. The limit of quantitation (LOQ) was 1.0 mg/kg for liquid samples and 4.0 mg/kg for soy sauce, semi-solid, and solid samples. The recoveries from spiked samples ranged from 82.1% to 103.3% with a relative standard deviation (RSD) ranging from 0.7% to 2.5%. This method was characterized by high sensitivity, simple operation, rapidity and accurate and reliable quantification, and suitable for the quantitative detection of PQQ disodium salt in various food matrices. This research effectively addresses the shortcomings of existing methods for detecting PQQ disodium salt in foods and provide strong technical support for the routine supervision of PQQ disodium salt in various food matrices.