In order to solve the problems of the detection of various foodborne stimulants in different animal-derived foods such as significant differences in matrix effects and many types of interference, a method was established for the determination of 10 protein anabolic agents, 8 glucocorticoids, and 12 diuretics in animal-derived foods by pass-through solid phase extraction (SPE) and ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The sample was extracted with 5% formic acid in acetonitrile, and the extract was purified by pass-through solid phase extraction before being analyzed by UPLC-MS/MS. The internal standard method was used for quantification. The results showed that good linearity was observed for all analytes within their respective concentration ranges. The average recoveries ranged from 67.5% to 114.3% with relative standard deviations (RSDs) between 0.7% and 16.1% (n = 6). This method is characterized by high sensitivity, simple operation, high throughput and high detection efficiency, which improves the measurement accuracy of different complex matrices and can meet the need for the detection of the 30 foodborne stimulants in animal-derived foods used in sports events.

To effectively assess food safety risks associated with potential plant toxin residues present in honey, this study aimed to establish and validate a method for the detection of 39 plant toxins in honey using solid-phase extraction combined with ultra-high performance liquid chromatography-tandem mass spectrometry (SPE-UPLC-MS/MS). The developed method involved sample extraction with 0.1% formic acid, purification using a hydrophilic-lipophilic balanced (HLB) cartridge, detection in the multiple reaction monitoring (MRM) mode, and quantification using the matrix-matched external standard method. The calibration curves exhibited good linearity for all the analytes. Average recoveries ranged from 78.7% to 112.8% with relative standard deviation (RSD) between 1.6% and 15.2% (n = 6). This method was characterized by ease of operation, high throughput and high sensitivity, and could be used for the monitoring these toxins in honey. Varying levels of pyrrolizidine alkaloids (PAs) and rhodojaponin Ⅲ were detected in some of the 36 tested batches of honey, confirming the presence of phytotoxin residue risks in honey.

A rapid method was developed for the simultaneous determination of flupyradifurone and its metabolites 6-chloronicotinic acid and difluoroacetic acid in milk using ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). A simple and efficient dispersive solid phase extraction method was used to purify milk samples, and the purification strategy was evaluated. After improved quick, easy, cheap, effective, rugged and safe (QuEChERS) treatment, 0.1% formic acid in acetonitrile was used as the mobile phase for chromatographic separation on a Shim-pack-GIST C₁₈ column, and the detection was performed in the multiple reaction monitoring (MRM) mode. The external standard method with matrix standard curves was used for quantification. The results showed that under the optimal conditions, good linearity (determination coefficient greater than 0.996) was observed for flurofuranone, 6-chloronicotinic acid and difluoroacetic acid in the concentration ranges of 0.005–0.5, 0.005–0.5 and 0.025–2.5 mg/L, respectively. The average recoveries of flupyradifurone and its metabolites at three spiked concentrations varied from 70.2% to 97.6%, with relative standard deviations (RSDs) between 3.6% and 5.3%, and the limits of detection (LODs) ranged from 0.01 to 0.05 mg/kg, much lower than the national maximum residue limits. This method was characterized by high accuracy, high sensitivity, and good reproducibility. Therefore, it is suitable for large batches of milk samples, and can provide reliable technical support for the management of the pesticide flupyradifurone.