Concurrent Quantification of Deoxynivalenol, Its Derivatives, and Nivalenol in Pet Food Using QuEChERS Combined with LC-MS/MS

In the current research, we optimized a simultaneous method for quantifying deoxynivalenol (DON) and its derivative forms, deoxynivalenol-3-glucoside (D3G), 3-acetyl-deoxynivalenol (3-AcDON), 15-acetyl-deoxynivalenol (15-AcDON), and nivalenol (NIV), in pet food using QuEChERS combined with liquid chromatography quadrupole mass spectrometry. The developed method’s linearity, sensitivity, selectivity, accuracy, and precision were also validated. The limits of detection and quantification for this analysis method were 6.7–9.4 ng g⁻¹ and 20.1–28.1 ng g⁻¹, respectively. The average recovery (60.1–107.2%, RSD ≤ 9.3%) met the recovery (60–110%) and precision (RSDr ≤ 20%) criteria for DON specified in Commission Regulation (EC) No. 401/2006. A total of 246 pet food samples (68 cat and 178 dog food samples) collected in South Korea were analyzed. DON was detected in 11.8% of cat food and 8.4% of dog food samples, with concentrations ranging from 122.9 to 799.4 ng g⁻¹ and 79.7 to 698.0 ng g⁻¹, respectively. The co-occurrence rate of DON and its metabolites was 7.3% in dog food and 10.3% in cat food. NIV was not detected in cat food samples but was detected in two (1.1%) dog food samples at 23.4 and 32.0 ng g⁻¹ contamination levels. All detected levels were below the regulatory guidance limit. Investigations of the effect of DON contamination levels according to the grain content of pet food revealed that the DON detection rate tended to increase with grain content. This study can be effectively utilized in quality control laboratories for high-throughput routine analysis of mycotoxins.