Advertisement

Analytical and Bioanalytical Chemistry

, Volume 406, Issue 4, pp 1259–1266 | Cite as

Multi-residue analysis of emerging pollutants in sediment using QuEChERS-based extraction followed by LC-MS/MS analysis

  • Alexandra Berlioz-Barbier
  • Antoine Vauchez
  • Laure Wiest
  • Robert Baudot
  • Emmanuelle Vulliet
  • Cécile Cren-Olivé
Note

Abstract

Emerging contaminants are suspected to cause adverse effects in humans and wildlife. Aquatic ecosystems are continuously contaminated by agricultural and industrial sources. To establish a causality relationship between the occurrence of contaminants in the environment and disease, experiments including all environmental matrices must be performed. Consequently, the current analytical tools must be improved. A new multi-residue method for analysing 15 emerging pollutants in sediments based on the Quick, Easy, Cheap, Effective, Rugged and Safe approach is reported. The development of such a multirisque, inter-family method for sediment including pharmaceuticals, pesticides, personal care products and plasticizers is reported for the first time. The procedure involves salting-out liquid–liquid extraction using acetonitrile and clean-up with dispersive solid phase extraction, followed by liquid chromatography coupled with tandem mass spectrometry. The validated analytical procedure exhibited recoveries between 40 and 98 % for every target compound. This methodology facilitated the determination of pollutant contents at nanogram-per-gram concentrations.

Keywords

LC-MS/MS QuEChERS Multi-residue Emerging pollutants Sediment 

References

  1. 1.
    Kasprzyk-Hordern B, Dinsdale R-M, Guwy A-J (2008) The occurrence of pharmaceuticals, personal care products, endocrine disruptors and illicit drugs in surface water in South Wales, UK. Water Res 42(1):3498–3518CrossRefGoogle Scholar
  2. 2.
    Conley J-M, Symes S-J, Kindelberger S-A, Richards S-M (2008) Rapid liquid chromatography-tandem mass spectrometry method for the determination of broad pharmaceuticals in surface water. J Chromatogr A 1185:206–2015CrossRefGoogle Scholar
  3. 3.
    Varca L-M (2012) Pesticide residues in surface waters of Pagsanjan–Lumban catchment of Laguna de Bay, Philippines. Agric Water Manag 106:35–41CrossRefGoogle Scholar
  4. 4.
    Labadie P, Hill E-M (2007) Analysis of estrogens in river sediments by liquid chromatography–electrospray ionization mass spectrometry. Comparison of tandem mass spectrometry and time-of-flight mass spectrometry. J Chromatogr A 1141:174–181CrossRefGoogle Scholar
  5. 5.
    Petrovic M, Hernando M-D, Diaz-Cruz M-S, Barcelo D (2005) Liquid chromatography–tandem mass spectrometry for the analysis of pharmaceutical residues in environmental samples: a review. J Chromatogr A 1067:1–14CrossRefGoogle Scholar
  6. 6.
    Eiguren Fernández A, Sosa Ferrera Z, Santana Rodríguez J-J (2001) Application of microwave-assisted extraction using micellar media to the determination of polychlorinated biphenyls in marine sediments. Anal Chim Acta 433(2):237–244CrossRefGoogle Scholar
  7. 7.
    EN 15662: 2009-01-01- Food of plant origin—determination of pesticide residues using GC-MS and/or LC-MS/MS following acetonitrile extraction/partitioning and clean up by dispersive SPE-QuEChERS method (2009). Austrian Standards institute, Österreichisches Normungsinstitut (ON) Heinestaβe 38, 1020 WienGoogle Scholar
  8. 8.
    AOAC Official Method 2007–01. Pesticide residues in food by acetonitrile extraction and partitioning with magnesium sulfate (2007). AOAC InternationalGoogle Scholar
  9. 9.
    Rambla-Alegre M, Esteve-Romero J, Carda-Broch S (2012) Is it really necessary to validate an analytical method or not? That is the question. J Chromatogr A 1232:101–109CrossRefGoogle Scholar
  10. 10.
    ICH (2005) International Conference on Harmonisation of technical requirements for registration of pharmaceuticals for human use. Paper presented at the ICH harmonised tripartite guideline, validation of analytical procedures: text and methodology Q2 (R1). ICH, GenevaGoogle Scholar
  11. 11.
    Vial J, Jardy A (1999) Experimental comparison of the different approaches to estimate LOD and LOQ of an HPLC method. Anal Chem 71(14):2672–2677CrossRefGoogle Scholar
  12. 12.
    Zhang Z, Rhind SM, Kerr C, Osprey M, Kyle CE (2011) Selective pressurized liquid extraction of estrogenic compounds in soil and analysis by gas chromatography–mass spectrometry. Anal Chim Acta 685(1):29–35CrossRefGoogle Scholar
  13. 13.
    Salvia MV, Vulliet E, Wiest L, Baudot R, Cren-Olivé C (2012) Development of multi-residue method using acetonitrile-based extraction followed by liquid chromatography-tandem mass spectrometry for the analysis of steroids and veterinary and human drugs at trace levels in soil. J Chromatogr A 1245:122–133CrossRefGoogle Scholar
  14. 14.
    Vazquez-Roiga P, Segarraa R, Blascoa C, Andreub V, Picóa Y (2010) Determination of pharmaceuticals in soils and sediments by pressurized liquid extraction and liquid chromatography tandem mass spectrometry. J Chromatogr A 1217(16):2471–2483CrossRefGoogle Scholar
  15. 15.
    Araujo P (2009) Key aspects of analytical method validation and linearity evaluation. J Chromatogr B 877(23):2224–2234CrossRefGoogle Scholar

Copyright information

© Springer-Verlag Berlin Heidelberg 2013

Authors and Affiliations

  • Alexandra Berlioz-Barbier
    • 1
  • Antoine Vauchez
    • 1
  • Laure Wiest
    • 1
  • Robert Baudot
    • 1
  • Emmanuelle Vulliet
    • 1
  • Cécile Cren-Olivé
    • 1
  1. 1.Université de Lyon-Institut des Sciences AnalytiquesUMR 5280 CNRS-Equipe TRACESVilleurbanneFrance

Personalised recommendations