Stir Bar Sorptive Extraction (SBSE)-HPLC-Tandem MS-Based Method for Multi-Residue Determination of Pesticides in Drinking Water

Pesticide residues in water contamination represent a significant public and political issue due to their harmful effects on the environment, biodiversity, and human health, even at low concentrations. Pesticides are chemically heterogeneous, covering a wide range of Log<i>K</i> <sub><i>o/w</i></sub> values. Therefore, developing sensitive methods to detect a broad spectrum of hazardous chemicals in aqueous matrices is challenging. Gas and liquid chromatography/high-performance liquid chromatography-mass spectrometry (GC/HPLC-MS) are established tools but typically require pre-concentration steps. Stir bar sorptive extraction (SBSE) is a green, simple, automatable, and HPLC-compatible technique. This study presents a multi-residue method for determining 131 pesticides in mineral water using SBSE followed by HPLC-tandem MS. The selected pesticides, from various chemical classes, were evaluated in fortified ultra-pure and mineral water samples. The method demonstrated excellent sensitivity, with lower limits of quantification ranging from 20 to 50 ng/L for all analytes, enabling detection at trace levels. Selectivity was high (SEL% <20%), and reproducibility was confirmed with RSD% values below 20%. Intra- and interday precision tests revealed RSD% values from 0.23% to 19.81%. Trueness was validated with BIAS% below 20% at all concentrations. Uncertainty values were acceptable, with U% ranging from 1.44% to 49.24%. This SBSE-HPLC-tandem MS method is a robust, efficient, and reliable alternative to traditional approaches for routine monitoring of pesticide residues in drinking water, with quantification limits below regulatory requirements. It offers a suitable tool for public health applications, ensuring reliable pesticide detection in complex water matrices.

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Publication Details

Journal
Mass Spectrometry
Published
2025-03-26
DOI
https://doi.org/10.5702/massspectrometry.a0172
Citations
4
Primary Topic
Analytical chemistry methods development
Type
article
Field-Weighted Citation Impact
3.01
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article

Stir Bar Sorptive Extraction (SBSE)-HPLC-Tandem MS-Based Method for Multi-Residue Determination of Pesticides in Drinking Water

Alessandra Grimmes Bernardo, Riccardo Aigotti, Sara Serra, Francesco Floris et al.
4 citations
Mass Spectrometry
Analytical chemistry methods development
3.01
article

Stir Bar Sorptive Extraction (SBSE)-HPLC-Tandem MS-Based Method for Multi-Residue Determination of Pesticides in Drinking Water

Alessandra Grimmes Bernardo, Riccardo Aigotti, Sara Serra, Francesco Floris, Federica Dal Bello, Claudio Medana, Alex Affricano
article en
4 citations

Abstract

Pesticide residues in water contamination represent a significant public and political issue due to their harmful effects on the environment, biodiversity, and human health, even at low concentrations. Pesticides are chemically heterogeneous, covering a wide range of Log<i>K</i> <sub><i>o/w</i></sub> values. Therefore, developing sensitive methods to detect a broad spectrum of hazardous chemicals in aqueous matrices is challenging. Gas and liquid chromatography/high-performance liquid chromatography-mass spectrometry (GC/HPLC-MS) are established tools but typically require pre-concentration steps. Stir bar sorptive extraction (SBSE) is a green, simple, automatable, and HPLC-compatible technique. This study presents a multi-residue method for determining 131 pesticides in mineral water using SBSE followed by HPLC-tandem MS. The selected pesticides, from various chemical classes, were evaluated in fortified ultra-pure and mineral water samples. The method demonstrated excellent sensitivity, with lower limits of quantification ranging from 20 to 50 ng/L for all analytes, enabling detection at trace levels. Selectivity was high (SEL% <20%), and reproducibility was confirmed with RSD% values below 20%. Intra- and interday precision tests revealed RSD% values from 0.23% to 19.81%. Trueness was validated with BIAS% below 20% at all concentrations. Uncertainty values were acceptable, with U% ranging from 1.44% to 49.24%. This SBSE-HPLC-tandem MS method is a robust, efficient, and reliable alternative to traditional approaches for routine monitoring of pesticide residues in drinking water, with quantification limits below regulatory requirements. It offers a suitable tool for public health applications, ensuring reliable pesticide detection in complex water matrices.

Mass SpectrometryVol. 14(1)
University of Turin (IT)
Clean water and sanitation
Openalex Percentile: Top 10%
Analytical chemistry methods development
3.01
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