Abstract:In this study, a novel detection method for rapid and accurate detection of the tetraniliprole residues in cereal crop samples was developed using improved m-PFC purification combined with HPLC-MS/MS. The samples were extracted with acetonitrile, dehydrated by 4 g of anhydrous sodium sulfate and 4 g of anhydrous magnesium sulfate, purified by m-PFC HF-A column, separated on Agilent Venusil MP C18 (100 mm×2.1 mm, 3 μm), eluted in a gradient with methanol and water as the mobile phase, iscanned with electrospray ionization and in negative ion mode, and detected by the multiple reaction monitoring (SRM) mode, and quantified by the matrix-matched external standard method. The results showed that the coefficient of determination (r2) values of tetraniliprole within the linear range (0.1~20 μg/L) and in different grain and cereal food matrices were all higher than 0.999. The limit of quantification (S/N≥10) was 0.80 μg/kg. Taking rice, wheat, barley, millet, soybeans, green beans, corn, and sorghum as the substrates, the recovery rates of tetraniliprole spiked at three levels of 0.80, 1.6 and 8.0 μg/kg ranged from 84.67% to 98.14%. The evaluation of assay stability revealed that the relative standard deviation of six measurements within the same batch (RSD, n=6) had a minimum of 0.77% and a maximum of 3.36%, whilst the relative standard deviation of six replicates between different batches (RSD, n=6) was within the range of 0.95% to 2.53%. This method is convenient, efficient and highly precise, and meets the requirements for detecting tetraniliprole residues in grain and cereal foods.