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Analytical and Bioanalytical Chemistry

, Volume 410, Issue 11, pp 2765–2779 | Cite as

Evaluation of on-line concentration coupled to liquid chromatography tandem mass spectrometry for the quantification of neonicotinoids and fipronil in surface water and tap water

  • Juan Manuel Montiel-León
  • Sung Vo Duy
  • Gabriel Munoz
  • Marc Amyot
  • Sébastien Sauvé
Research Paper

Abstract

A study was initiated to investigate a fast and reliable method for the determination of selected systemic insecticides in water matrixes and to evaluate potential sources of bias in their analysis. Acetamiprid, clothianidin, desnitro-imidacloprid, dinotefuran, fipronil, imidacloprid, nitenpyram, thiacloprid, and thiamethoxam were amenable to analysis via on-line sample enrichment hyphenated to ultra-high-performance liquid chromatography tandem mass spectrometry. The selection of on-line solid-phase extraction parameters was dictated by a multicriterion desirability approach. A 2-mL on-line injection volume with a 1500 μL min−1 loading flow rate met the objectives sought in terms of chromatographic requirements, extraction efficiency, sensitivity, and precision. A total analysis time of 8 min per sample was obtained with method limits of detection in the range of 0.1–5 ng L−1 for the scope of targeted analytes. Automation at the sample concentration step yielded intraday and interday precisions in the range of 1–23 and 2–26%, respectively. Factors that could affect the whole method accuracy were further evaluated in matrix-specific experiments. The impact of the initial filtration step on analyte recovery was evaluated in ultra-pure water, tap water, and surface water. Out of the nine membranes tested, glass fiber filters and polyester filters appeared as the most appropriate materials. Sample storage stability was also investigated across the three matrix types; the targeted analytes displayed suitable stability during 28 days at either 4 °C or − 20 °C, with little deviations (± 10%) with respect to the initial T0 concentration. Method applicability was demonstrated in a range of tap water and surface water samples from the province of Québec, Canada. Results from the present survey indicated a predominance of thiamethoxam (< 0.5–10 and 3–61 ng L−1 in tap water and river water, respectively), clothianidin (< 0.5–6 and 2–88 ng L−1 in tap water and river water, respectively), and imidacloprid (< 0.1–1 and 0.8–38 ng L−1 in tap water and river water, respectively) among the targeted analytes.

Graphical abstract

Development of solid-phase extraction coupled on-line to UHPLC-MS/MS for the rapid screening of systemic insecticides in water.

Keywords

Systemic pesticides Neonicotinoids On-line solid-phase extraction Water analysis Filtration Storage stability 

Notes

Funding information

We thank the Natural Sciences and Engineering Research Council of Canada (NSERC), the Quebec Research Fund (FRQ), and the Canada Foundation for Innovation (CFI) for their financial support. The authors acknowledge technical support from Thermo Fisher Scientific. Conacyt (Consejo Nacional de Ciencia y Tecnología, Mexico City, Mexico) is acknowledged for the PhD scholarship awarded to Juan Manuel Montiel León.

Compliance with ethical standards

Conflict of interest

The authors declare that they have no conflict of interest.

Supplementary material

216_2018_957_MOESM1_ESM.pdf (264 kb)
ESM 1 (PDF 263 kb)

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Copyright information

© Springer-Verlag GmbH Germany, part of Springer Nature 2018

Authors and Affiliations

  • Juan Manuel Montiel-León
    • 1
  • Sung Vo Duy
    • 1
  • Gabriel Munoz
    • 1
  • Marc Amyot
    • 2
  • Sébastien Sauvé
    • 1
  1. 1.Département de ChimieUniversité de MontréalMontréalCanada
  2. 2.GRIL, Département de Sciences BiologiquesUniversité de MontréalMontréalCanada

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