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Multi-Residual Determination of Multi-Class Pesticides in Groundwater by Direct Immersion Solid-Phase Microextraction with Gas Chromatography-Selected Ion Monitoring Mass Spectrometry (GC–MS/SIM) Detection

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Abstract

This paper describes a simple, quick, and solvent-free multi-residue method to determine 90 pesticides in groundwater samples from 30 different chemical groups. The extraction was carried out by solid-phase microextraction in direct immersion mode (DI-SPME) using a polydimethylsiloxane/divinylbenzene fiber (65 µm thickness) followed by GC–MS detection. The main parameters affecting the DI-SPME process were studied in detail: temperature, NaCl addition, stirring rate, and extraction time. The validation parameters as linearity, precision (repeatability and reproducibility), and accuracy were evaluated. The limits of quantification (LOQs) were in the range of 0.009–0.976 µg L−1. The analytes recoveries in groundwater samples varied from 60 to 120% and were appropriate for this type of water. The validated analytical method was successfully applied to the analysis of groundwater from wells located in agricultural sites in the municipality of Cadereyta Jimenez in Nuevo Leon, Mexico. The pesticides p, p’-DDT, bifenthrin, 2,4’-D ethylhexyl ester, and aldrin were below the LOQs in 73% of the analyzed samples. Oxyfluorfen and fenoxycarb were quantified at 0.08 and 0.2 µg L−1, respectively. Fenoxycarb was above the maximum allowable concentration of 0.1 µg L−1 for drinking water established by the European Union.

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Funding

This work was funded by a grant from the Consejo Nacional de Ciencia y Tecnología (CONACYT), México, PDCPN-2015, No. 505 and PAICYT program of Universidad Autónoma de Nuevo León, México. The authors thank the support from the Red Temática de Toxicología de Plaguicidas—CONACYT, 280045. D. Elizarragaz thanks CONACYT (scholarship number 443152) for the economic support to pursue his Ph.D. studies. A special thanks to Víctor Manuel Alcantar Rosales for the analysis of the samples and training in the use of the analytical instruments.

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Authors and Affiliations

  1. Universidad Autónoma de Nuevo León, Facultad de Ciencias Químicas, Av. Universidad s/n, Cd. Universitaria, San Nicolás de los Garzas, Nuevo León, C.P. 66455, México

    Dalaú Elizarragaz-de la Rosa, Jorge Luis Guzmán-Mar, Laura Hinojosa-Reyes & Edgar Jocsan Ruiz-Ruiz

  2. Centro de Investigación y Asistencia en Tecnología y Diseño del Estado de Jalisco A.C., Sede Noreste, Vía de la Innovación 404, Autopista Monterrey-Aeropuerto Km 10, Parque PIIT, Apodaca, Nuevo León, C.P. 66628, México

    Edgar Arturo Salas-Espinosa, María Elena Heras-Ramírez & Octavio Gaspar-Ramírez

Authors
  1. Dalaú Elizarragaz-de la Rosa
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  2. Jorge Luis Guzmán-Mar
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  3. Edgar Arturo Salas-Espinosa
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  5. Laura Hinojosa-Reyes
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  6. Octavio Gaspar-Ramírez
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Contributions

Dalaú Elizarragaz-de la Rosa: performed the experimental research, wrote a first draft of the manuscript, and designed the figures.

Jorge L. Guzmán-Mar: provided critical feedback and helped shape the research, and reviewer manuscript.

Edgar Arturo Salas-Espinos: characterized the samples by instrumental techniques and contributed to the interpretation of the results.

María Elena Heras-Ramírez: characterized the samples by instrumental techniques and contributed to the interpretation of the results.

Laura Hinojosa-Reyes: provided critical feedback and helped shape the research, statistical analysis, and reviewer manuscript.

Octavio Gaspar-Ramírez: helped to supervise the project and to analyze the results, verified the analytical method, and reviewed the writing manuscript.

Edgar Jocsan Ruiz-Ruiz: was involved in planning, supervised the project, wrote the manuscript.

Corresponding authors

Correspondence to Octavio Gaspar-Ramírez or Edgar Jocsan Ruiz-Ruiz.

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Elizarragaz-de la Rosa, D., Guzmán-Mar, J.L., Salas-Espinosa, E.A. et al. Multi-Residual Determination of Multi-Class Pesticides in Groundwater by Direct Immersion Solid-Phase Microextraction with Gas Chromatography-Selected Ion Monitoring Mass Spectrometry (GC–MS/SIM) Detection. Water Air Soil Pollut 233, 76 (2022). https://doi.org/10.1007/s11270-022-05555-3

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