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

Abstract

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.

Graphical Abstract

Keywords:

• Dispersive solid-phase extraction
• freshwater fish
• freshwater shrimp
• pyrethroids
• ultra-performance liquid chromatography-tandem mass spectrometry

Acknowledgements

We would like to thank the National Key R&D Projects of China (No. 2023YFF1105100), Key Cultivation Project of Zhejiang Provincial Administration for Market Regulation (No. CY2023005), State Administration for Market Regulation Project (No. 2020YJ014) and Zhejiang Fangyuan Test Group Project” (Grant Number: ZL202301). The funders had no role in study design, data collection and analysis, decision to publish, or preparation of the manuscript.

Authors contributions

Shuifeng Zhang: Conceptualization, Investigation, Methodology, Funding acquisition, Writing-Review & Editing; Lulu Wang: Investigation, Data curation, Methodology, Writing-original draft, Writing-Review & Editing; Yuanxu Shi: Investigation, Supervision, Resources; Xiangjie Pan: Methodology, Investigation; Yunxuan Li: Investigation; Tianshu Li: Investigation; Ying Chen: Resources; Jiaqi Zhang: Resources; Huadong Sheng: Methodology.

Disclosure statement

No potential conflict of interest was reported by the author(s).