Ultra-performance liquid chromatography-tandem mass spectrometry for quantification of pyrethroid pesticide residues in freshwater fish and shrimp

A sophisticated Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry (UPLC-MS/MS) approach was devised for the concurrent quantification of pyrethroid pesticide residues in freshwater fish and shrimp. This analytical method involved ultrasonic extraction using acetonitrile, succeeded by sample purification employing Primary Secondary Amine (PSA) and Zirconium Dioxide Silica (Z-Sep+) following low-temperature centrifugation. Chromatographic separation was achieved with an ACQUITY UPLC BEH C18 column utilizing a mobile phase of a 2 mmol/L ammonium formate aqueous solution and methanol, with detection conducted through ESI + ionization in Multiple Reaction Monitoring (MRM) mode. The assay demonstrated exceptional linearity for seven pyrethroids across a concentration range of 0.5–10 μg/L, evidenced by correlation coefficients surpassing 0.999. Detection limits were established between 0.08 and 0.52 μg/kg, and the lower limits of quantification ranged from 0.28 to 1.72 μg/kg. Furthermore, recovery rates for blank samples were outstanding, ranging from 91.40% to 108.83% at concentrations of 1.0, 4.0, and 20.0 μg/kg, with Relative Standard Deviations (RSDs) between 0.94% and 8.13%. This methodology proved to be rapid, convenient, sensitive, and robust, offering stable recovery rates. Notably, it facilitated the detection of seven pyrethroid pesticide residues in freshwater fish and shrimp within an expedited timeframe of 15 min. This pioneering technique constitutes a significant advancement in the development of new methods for ensuring food safety.