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Analytical and Bioanalytical Chemistry

, Volume 411, Issue 3, pp 669–678 | Cite as

Quantification of DEET and neonicotinoid pesticide biomarkers in human urine by online solid-phase extraction high-performance liquid chromatography-tandem mass spectrometry

  • Samuel E. Baker
  • Amanda Bishop Serafim
  • Pilar Morales-Agudelo
  • Meghan Vidal
  • Antonia M. Calafat
  • Maria OspinaEmail author
Research Paper

Abstract

Neonicotinoid insecticides are widely used replacements for organophosphate and carbamate insecticides, but the extent of human exposure is largely unknown. On the other hand, based on urinary concentrations of DEET metabolites, human exposure to N,N-diethyl-m-toluamide (DEET) appears to be widespread. We developed a fast online solid-phase extraction high-performance liquid chromatography-isotope dilution tandem mass spectrometry (HPLC-MS/MS) method to measure in 200 μL of human urine the concentrations of six neonicotinoid biomarkers (acetamiprid, N-desmethyl-acetamiprid, clothianidin, imidacloprid, 5-hydroxy-imidacloprid, thiacloprid), and two DEET biomarkers (3-diethyl-carbamoyl benzoic acid, 3-ethyl-carbamoyl benzoic acid). Limits of detection ranged from 0.01 to 0.1 μg/L, depending on the biomarker. Accuracy ranged from 91 to 116% and precision ranged from 3.7 to 10 %RSD. The presented method can be used to increase our understanding of exposure to neonicotinoid insecticides and DEET, and to evaluate the potential health effects from such exposures.

Keywords

DEET N,N-Diethyl-m-toluamide Neonicotinoids Biomarkers HPLC-MS/MS Online SPE 

Notes

Acknowledgements

We thank Charlie Chambers for technical assistance and Dr. Peter Kuklenyik for the diagram in the supplemental information.

Compliance with ethical standards

Conflict of interest

The authors declare they have no competing interests.

Supplementary material

216_2018_1481_MOESM1_ESM.pdf (328 kb)
ESM 1 (PDF 328 kb)

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Copyright information

© This is a U.S. Government work and not under copyright protection in the US; foreign copyright protection may apply 2018

Authors and Affiliations

  • Samuel E. Baker
    • 1
  • Amanda Bishop Serafim
    • 1
  • Pilar Morales-Agudelo
    • 1
    • 2
  • Meghan Vidal
    • 1
    • 2
  • Antonia M. Calafat
    • 1
  • Maria Ospina
    • 1
    Email author
  1. 1.Division of Laboratory Sciences, National Center for Environmental HealthCenters for Disease Control and PreventionAtlantaUSA
  2. 2.Battelle Memorial InstituteAtlantaUSA

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