Pyrethroid pesticide metabolite, 3-PBA, in soils: method development and application to real agricultural soils

  • Idalina Bragança
  • Paulo C. Lemos
  • Cristina Delerue-Matos
  • Valentina F. Domingues
Research Article


3-Phenoxybenzoic acid (3-PBA) is a shared metabolite of several synthetic pyrethroid pesticides (SPs) resulting from environmental degradation of parent compounds and thus occurs frequently as a residue in samples. Hence, the importance of 3-PBA evaluation after pyrethroid application. There is a gap of analytical methods to determine 3-PBA in soil samples. Therefore, an analytical method that combines the solid-phase extraction (SPE) and gas chromatography–mass spectrometry (GC/MS) detection has been developed for the determination of 3-PBA in soil samples. The analytical method was validated in terms of linearity, sensitivity, intra- and inter-day batch precisions, recoveries, and quantification limits. An SPE method using a Strata X cartridge allows obtaining limits of detection and quantification equal to 4.0 and 13.3 ng g−1, respectively. Under optimized conditions, the method average recovery levels ranged from 70.3 to 93.5% with a relative standard deviation below 3.4%. Method intra- and inter-day precision was under 5.0 and 4.8%, respectively. The developed method was applied to 11 agricultural soil samples in the north of Portugal. The developed methodology allowed for the determination of the pyrethroid metabolite, 3-PBA, in agricultural soil samples at levels of few ng g−1.

Graphical abstract


3-phenoxybenzoic acid Solid-phase extraction Soils Gas chromatography/mass spectrometry 



The authors are greatly indebted to all financing sources.

Funding information

I. Bragança is financially supported by FCT through the doctoral research grant financed by fellowship (SFRH/BD/52504/2014). This work was supported by the Associate Laboratory for Green Chemistry-LAQV which is financed by national funds from FCT/MCTES (UID/QUI/50006/2013) and co-financed by the ERDF under the PT2020 Partnership Agreement (POCI-01-0145-FEDER-007265).


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Copyright information

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

Authors and Affiliations

  1. 1.REQUIMTE/LAQV-GRAQInstituto Superior de Engenharia do Porto, Polytechnic PortoPortoPortugal
  2. 2.REQUIMTE/LAQV, Chemistry DepFCT/Universidade NOVA de LisboaCaparicaPortugal
  3. 3.RequimteInstituto Superior de Engenharia do Porto, Instituto Politécnico do PortoPortoPortugal

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