Skip to main content
SpringerLink
Log in

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

  • Note
  • Published:
Analytical and Bioanalytical Chemistry Aims and scope Submit manuscript

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.

ᅟ

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Fig. 1
Fig. 2
Fig. 3

Similar content being viewed by others

References

  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):3498–3518

    Article  CAS  Google Scholar 

  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 1185:206–2015

    Article  CAS  Google Scholar 

  3. Varca L-M (2012) Pesticide residues in surface waters of Pagsanjan–Lumban catchment of Laguna de Bay, Philippines. Agric Water Manag 106:35–41

    Article  Google Scholar 

  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 1141:174–181

    Article  CAS  Google Scholar 

  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 1067:1–14

    Article  CAS  Google Scholar 

  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):237–244

    Article  Google Scholar 

  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 Wien

  8. AOAC Official Method 2007–01. Pesticide residues in food by acetonitrile extraction and partitioning with magnesium sulfate (2007). AOAC International

  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 1232:101–109

    Article  CAS  Google Scholar 

  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, Geneva

    Google Scholar 

  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):2672–2677

    Article  CAS  Google Scholar 

  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):29–35

    Article  CAS  Google Scholar 

  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 1245:122–133

    Article  CAS  Google Scholar 

  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):2471–2483

    Article  Google Scholar 

  15. Araujo P (2009) Key aspects of analytical method validation and linearity evaluation. J Chromatogr B 877(23):2224–2234

    Article  CAS  Google Scholar 

Download references

Author information

Authors and Affiliations

  1. Université de Lyon-Institut des Sciences Analytiques, UMR 5280 CNRS-Equipe TRACES, Université Lyon1, ENS-Lyon - 5 rue de la Doua, 69100, Villeurbanne, France

    Alexandra Berlioz-Barbier, Antoine Vauchez, Laure Wiest, Robert Baudot, Emmanuelle Vulliet & Cécile Cren-Olivé

Authors
  1. Alexandra Berlioz-Barbier
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Antoine Vauchez
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Laure Wiest
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Robert Baudot
    View author publications

    You can also search for this author in PubMed Google Scholar

  5. Emmanuelle Vulliet
    View author publications

    You can also search for this author in PubMed Google Scholar

  6. Cécile Cren-Olivé
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Cécile Cren-Olivé.

Additional information

Published in the special issue Analytical Science in France with guest editors Christian Rolando and Philippe Garrigues.

Rights and permissions

Reprints and permissions

About this article

Cite this article

Berlioz-Barbier, A., Vauchez, A., Wiest, L. et al. Multi-residue analysis of emerging pollutants in sediment using QuEChERS-based extraction followed by LC-MS/MS analysis. Anal Bioanal Chem 406, 1259–1266 (2014). https://doi.org/10.1007/s00216-013-7450-8

Download citation

  • Received:

  • Revised:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s00216-013-7450-8

Keywords

Search

Navigation