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Trace analysis of pesticide residues in sediments using liquid chromatography–high-resolution Orbitrap mass spectrometry

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Abstract

The present study describes the optimization and validation of an analytical method based on quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction and purification with dispersive solid-phase extraction (dSPE) before analysis, followed by ultrahigh-performance liquid chromatography–high-resolution linear ion trap/Orbitrap (LTQ Orbitrap) mass spectrometry for the determination of 18 pesticides in sediment. To optimize process efficiency, parameters such as pH, extraction salts, sediment amount, and cleanup sorbents were evaluated. Identification was based on both accurate mass and retention time, and further confirmation was achieved by mass spectrometry fragmentation. The optimized analytical method demonstrated good validation characteristics, such as accuracy (recoveries from 70.8% to 106.2%), method quantification limits (below 10 ng g-1 for 89% of the pesticides selected), linearity (coefficient of determination greater than 0.9921 in all cases), precision (repeatability and reproducibility with standard deviations below 18% and 21%, respectively), and matrix effect (signal suppression was exhibited for almost all analytes). The overall method performance, expressed as process efficiency, ranged from 58.8% to 102.1%. The validated method was successfully applied to real samples collected along two rivers in northwestern Greece, revealing the presence of three selected pesticides but at levels below the method quantification limit.

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Acknowledgements

This research was cofinanced by the European Union (European Social Fund) and Greek national funds through the operational program “Education and Lifelong Learning” of the National Strategic Reference Framework—Research Funding Program: ARCHIMEDES III, investing in knowledge society through the European Social Fund. It was also financially supported by the European project “Real time monitoring of SEA contaminants by an autonomous lab-on-a-chip biosensor” (SEA-on-a-CHIP; project ID 614168). The authors would like to thank the Unit of Environmental, Organic and Biochemical High Resolution Analysis-Orbitrap-LC-MS of the University of Ioannina for providing access to the facilities.

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  1. Laboratory of Analytical Chemistry, Department of Chemistry, University of Ioannina, 45110, Ioannina, Greece

    Christina I. Nannou, Vasiliki I. Boti & Triantafyllos A. Albanis

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  1. Christina I. Nannou
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  2. Vasiliki I. Boti
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Correspondence to Vasiliki I. Boti.

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Nannou, C.I., Boti, V.I. & Albanis, T.A. Trace analysis of pesticide residues in sediments using liquid chromatography–high-resolution Orbitrap mass spectrometry. Anal Bioanal Chem 410, 1977–1989 (2018). https://doi.org/10.1007/s00216-018-0864-6

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