Analytical and Bioanalytical Chemistry

, Volume 400, Issue 2, pp 587–594 | Cite as

Semi-automated liquid chromatography–mass spectrometry (LC–MS/MS) method for basic pesticides in wastewater effluents

  • Michael G. Cahill
  • Giovanni Caprioli
  • Mary Stack
  • Sauro Vittori
  • Kevin J. JamesEmail author
Original Paper


Effluent from wastewater treatment plants have been identified as an important source of micro-organic contaminants in the environment. An online high-performance liquid chromatography–heated electrospray ionization tandem mass spectrometric method was developed and validated for the determination of basic pesticides in effluent wastewaters. Most available methods for pesticide analysis of wastewater samples are time-consuming, require complex clean-up steps and are difficult to automate. The method developed used a simple solid-phase extraction clean-up for salt and lipid reduction. On-line sample pre-concentration was performed using a reversed phase (C18) column, and analytes were separated by back-flushing onto an analytical column (C8) with detection using QqQ MS. An option to increase MS resolution was exploited to minimize interference from endogenous compounds in the matrix. A better than unit mass resolution was used (Q1 full width half maximum (FWHM) = 0.2 Da and Q3 FWHM = 0.7 Da), which was as rugged as a unit resolution method, and improved signal/noise and better detection limits were achieved for the targeted basic pesticides. This method was applied to the determination of 11 pesticides, including methoxytriazine, chlorotriazines, chloroacetanilides, phenylurea and carbamate pesticides. The percentage recovery values for these pesticides using the online trapping column were within the range, 73–95%, with relative standard deviation (RSD) values <8.9%. The highest concentrations of these pesticides in wastewater effluents in County Cork, Ireland, were simazine (0.51 μg/L), prometon (0.14 μg/L), diuron (0.21 μg/L) and atrazine (0.19 μg/L).

Online Abstract Figure

Effect of mass resolution change on signal/noise in the ion chromatograms for simazine at a) resolution setting, FWHM = 0.6 Da, b) resolution setting, FWHM = 0.2 Da.


Priority pollutants Online solid-phase extraction Triple quadrupole mass analyzer 



This research was funded by the Environmental Protection Agency of Ireland, STRIVE program (2007–2013); Monitoring Criteria for Priority Chemicals Leading to Emission Factors, and the Higher Education Authority of Ireland, as part of the EU Structural Funds Programs (2007–2013) and the European Regional Development Fund; Program for Research in Third Level Institutions (PRTLI-4), Environment and Climate Change: Impacts and Responses.


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Copyright information

© Springer-Verlag 2011

Authors and Affiliations

  • Michael G. Cahill
    • 1
    • 2
  • Giovanni Caprioli
    • 3
  • Mary Stack
    • 2
  • Sauro Vittori
    • 3
  • Kevin J. James
    • 1
    • 2
    Email author
  1. 1.Environmental Research InstituteUniversity College CorkCorkIreland
  2. 2.PROTEOBIO (Mass Spectrometry Centre)Cork Institute of TechnologyCorkIreland
  3. 3.Dipartimento di Scienze Chimiche, Facoltà di FarmaciaUniversità di CamerinoCamerinoItaly

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