Skip to main content
SpringerLink
Log in

Determination of organic priority pollutants in the low nanogram-per-litre range in water by solid-phase extraction disk combined with large-volume injection/gas chromatography–mass spectrometry

  • Research Paper
  • Published:
Analytical and Bioanalytical Chemistry Aims and scope Submit manuscript

Abstract

Polybrominated diphenyl ethers, polychlorinated biphenyls, polycyclic aromatic hydrocarbons and organochlorine pesticides in the low nanogram-per-litre range in water were enriched by solid-phase extraction (SPE) disks and their concentration determined by large-volume injection/gas chromatography–mass spectrometry (LVI/GC-MS). One advantage of using SPE disks in comparison with SPE cartridges is that suspended particulate matter (SPM) does not have to be separated prior to the enrichment step, which saves time and effort. To increase the sensitivity of the method, the SPE disk procedure was combined with LVI/GC-MS, which has not been reported so far for water analysis. The method was calibrated in ranges from 0.25 to 2.5 ng/L and from 2.5 to 25 ng/L. The average recovery was 76 % at an analyte concentration of 2.5 ng/L. The limits of quantification, defined at a signal-to-noise ratio of 6:1, reach from 0.1 to 24.0 ng/L and are up to 400 times lower than previously reported in water analysis. By the developed SPE/LVI/GC-MS method, it is possible to investigate the whole water sample without prior separation of the SPM within 2 h including GC-MS analysis.

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

Similar content being viewed by others

References

  1. Pichon V, Charpak M, Hennion MC (1998) Multiresidue analysis of pesticides using new laminar extraction disks and liquid chromatography and application to the French priority list. J Chromatogr A 795(1):83–92

    Article  CAS  Google Scholar 

  2. Bao ML, Pantani F, Barbieri K, Burrini D, Griffini O (1996) Multi-residue pesticide analysis in soil by solid-phase disk extraction and gas chromatography ion-trap mass spectrometry. Int J Environ Anal Chem 64(4):233–245

    Article  Google Scholar 

  3. Sun L, Liu Y, Chu XG, Lin JM (2010) Trace analysis of fifteen androgens in environmental waters by LC-ESI-MS-MS combined with solid-phase disk extraction cleanup. Chromatographia 71(9–10):867–873

    Article  CAS  Google Scholar 

  4. Werres F, Balsaa P, Schmidt TC (2009) Total concentration analysis of polycylic aromatic hydrocarbons in aqueous samples with high suspended particulate matter content. J Chromatogr A 1216(12):2235–2240

    Article  CAS  Google Scholar 

  5. Domingues V, Cabral M, Alves A, Delerue-Matos C (2009) Use and reuse of SPE disks for the determination of pyrethroids in water by GC-ECD. Anal Lett 42:706–726

    Article  CAS  Google Scholar 

  6. Steen RJCA, Freriks IL, Cofino WP, Brinkman UAT (1997) Large-volume injection in gas chromatography-ion trap tandem mass spectrometry for the determination of pesticides in the marine environment at the low ng/l level. Anal Chim Acta 353:153–163

    Article  CAS  Google Scholar 

  7. Teske J, Engewald W (2002) Methods for, and applications of, large-volume injection in capillary gas chromatography. Trends Anal Chem 21(9–10):584–593

    Article  CAS  Google Scholar 

  8. Mol HGJ, Janssen H-G, Cramers CA, Brinkman UAT (1996) Large-volume injection in gas chromatographic trace analysis using temperature-programmable (PTV) injectors. Trends Anal Chem 15(4):206–214

    Article  CAS  Google Scholar 

  9. Zhao Y, Yang L, Wang Q (2007) Pulsed large volume injection gas chromatography coupled with electron-capture negative ionization quadrupole mass spectrometry for simultaneous determination of typical halogenated persistent organic pollutants. J Am Soc Mass Spectrom 18:1375–1386

    Article  CAS  Google Scholar 

  10. Mol HGJ, Janssen H-G, Cramers CA, Brinkman UAT (1995) Large volume sample introduction using temperature programmable injectors: implications of liner diameter. J High Resolut Chromatogr 18:18–26

    Google Scholar 

  11. Hoh E, Mastovska K (2008) Large volume injection techniques in capillary gas chromatography. J Chromatogr A 1186:2–15

    Article  CAS  Google Scholar 

  12. van Leeuwen SPJ, de Boer J (2008) Advances in the gas chromatographic determination of persistent organic pollutants in the aquatic environment. J Chromatogr A 1186:161–182

    Article  Google Scholar 

  13. Wei H, Dassanayake PS, Li A (2010) Parametric evaluation for programmable temperature vaporisation large volume injection in gas chromatographic determination of polybrominated diphenyl ethers. Int J Environ Anal Chem 90(7):535–547

    Article  CAS  Google Scholar 

  14. Tollbäck P, Bjroklund J, Östman C (2003) Large-volume programmed-temperature vaporiser injection for fast gas chromatography with electron capture and mass spectrometric detection of polybrominated diphenyl ethers. J Chromatogr A 991(2):241–253

    Article  Google Scholar 

  15. Li YT, Whitaker J, McCarty C (2009) New advances in large-volume injection gas chromatography–mass spectrometry. J Liq Chromatogr R T 32(11–12):1644–1671

    CAS  Google Scholar 

  16. Erger C, Balsaa P, Werres F, Schmidt TC (2012) Occurrence of residual water within disk-based solid-phase extraction and its effect on GC-MS measurement of organic extracts of environmental samples. Anal Bioanal Chem 403:2541–2552

    Article  CAS  Google Scholar 

  17. Erger C, Balsaa P, Werres F, Schmidt TC (2012) Multi-component trace analysis of organic xenobiotics in surface water containing suspended particular matter by solid phase extraction/gas chromatography–mass spectrometry. J Chromatogr A 1249:181–189

    Article  CAS  Google Scholar 

  18. DIN 32 645 “Nachweis-, Erfassungs- und Bestimmungsgrenze-Ermittlung unter Wiederholbedingungen-Begriffe, Verfahren, Auswertung” (Mai 1994)

  19. European Commission (2000) Directive 2000/60/EC of the European Parliament and of the Council of 23 October 2000 establishing a framework for community action in the field of water policy

  20. Verordnung zum Schutz der Oberflächengewässer (Oberflächengewässerverordnung-OGewV), Bundesgesetzblatt Teil 1, Nr. 37 (25 July 2011)

  21. European Commission (2009) Directive 2009/90/EC of 31 July 2009 laying down, pursuant to Directive 2000/60/EC of the European Parliament and of the Council, technical specifications for chemical analysis and monitoring of water status

  22. European Commission (2009) Common implementation strategy for the Water Framework Directive (2000/60/EC)—guidance document no. 19—guidance on surface water chemical monitoring under the Water Framework Directive

  23. Brondi SHG, Spoljaric FC, Lancas FM (2005) Ultratraces analysis of organochlorine pesticides in drinking water by solid phase extraction coupled with large volume injection/gas chromatography/mass spectrometry. J Sep Sci 28:2243–2246

    Article  CAS  Google Scholar 

  24. Prieto A, Schrader S, Moeder M (2010) Determination of organic priority pollutants and emerging compounds in wastewater and snow samples using multiresidue protocols on the basis of microextraction by packed sorbents coupled to large volume injection gas chromatography—mass spectrometry analysis. J Chromatogr A 1217(38):6002–6011

    Article  CAS  Google Scholar 

  25. Prieto A, Telleria O, Etxebarria N, Fernandez LA, Usobiaga A, Zuloaga O (2008) Simultaneous preconcentration of a wide variety of organic pollutants in water samples. Comparison of stir bar sorptive extraction and membrane-assisted solvent extraction. J Chromatogr A 1214(1–2):1–10

    CAS  Google Scholar 

  26. European Commission (2010) Common implementation strategy for the Water Framework Directive (2000/60/EC)—guidance document no. 25—guidance on chemical monitoring of sediment and biota under the Water Framework Directive

  27. Nakamura S, Yamagami T, Daishima S (2001) Determination of organochlorine pesticides in river water by gas chromatography-negative-ion chemical-ionization mass spectrometry using large volume injection. Analyst 126(10):1658–1662

    Article  CAS  Google Scholar 

  28. Lüthje K, Hyötyläinen T, Riekkola M-L (2004) On-line coupling of microporous membrane liquid–liquid extraction and gas chromatography in the analysis of organic pollutants in water. Anal Bioanal Chem 378:1991–1998

    Article  Google Scholar 

  29. Schellin M, Popp P (2003) Membrane-assisted solvent extraction of polychlorinated biphenyls in river water and other matrices combined with large volume injection-gas chromatography–mass spectrometric detection. J Chromatogr A 1020(2):153–160

    Article  CAS  Google Scholar 

  30. Serôdio P, Salomé CM, Nogueira JMF (2007) Use of experimental design in the optimization of stir bar sorptive extraction for the determination of polybrominated diphenyl ethers in environmental matrices. J Chromatogr A 1141:259–270

    Article  Google Scholar 

  31. Labadie P, Tlili K, Alliot F, Bourges C, Desportes A, Chevreuil M (2010) Development of analytical procedures for trace-level determination of polybrominated diphenyl ethers and tetrabromobisphenol A in river water and sediment. Anal Bioanal Chem 396:865–875

    Article  CAS  Google Scholar 

  32. Li Y, George JE, McCarty CL (2007) Online in situ analysis of selected semi-volatile organic compounds in water by automated microscale solid-phase extraction with large-volume injection/gas chromatography/mass spectrometry. J Chromatogr A 1176(1–2):223–230

    CAS  Google Scholar 

  33. Li YT, McCarty CL, George EJ (2011) Determination of selected semi-volatile organic compounds in water using automated online solid-phase extraction with large-volume injection/gas chromatography/mass spectrometry. Front Environ Sci En 5(3):417–425

    Article  CAS  Google Scholar 

  34. Schellin M, Popp P (2007) Application of a poly siloxane-based extraction method combined with large volume injection-gas chromatography–mass spectrometry of organic compounds in water samples. J Chromatogr A 1152(1–2):175–183

    CAS  Google Scholar 

  35. Bizkarguenaga E, Ros O, Iparraguirre A, Navarro P, Vallejo A, Usobiaga A, Zuloaga O (2012) Solid-phase extraction combined with large volume injection-programmable temperature vaporization-gas chromatography–mass spectrometry for the multiresidue determination of priority and emerging organic pollutants in wastewater. J Chromatogr A 1247:104–117

    Article  CAS  Google Scholar 

  36. European Commission (2008) Directive 2008/105/EC of the European Parliament and of the Council of 16 December 2008 on environmental quality standards in the field of water policy, amending and subsequently repealing Council Directives 82/176/EEC, 83/513/EEC, 84/156/EEC, 84/491/EEC, 86/280/EEC and amending Directive 2000/60/EC of the European Parliament and of the Council

  37. López FJ, Beltran J, Hernández MFF (1998) Comparison of simplified methods for pesticide residue analysis. Use of large-volume injection in capillary gas chromatography. J Chromatogr A 823:25–33

    Article  Google Scholar 

Download references

Acknowledgements

The work was supported by the Federal Ministry for Economy and Technology based on a resolution of the German Parliament, ZIM—Zentrales Innovationsprogramm Mittelstand and AiF—Arbeitsgemeinschaft industrieller Forschungsvereinigungen “Otto von Guericke” e.V.. Furthermore, we thank Varian Inc. for donation of materials.

Author information

Authors and Affiliations

  1. IWW Water Centre, Moritzstrasse 26, 45476, Mülheim an der Ruhr, Germany

    Christine Erger, Peter Balsaa, Friedrich Werres & Torsten C. Schmidt

  2. Instrumental Analytical Chemistry, University of Duisburg-Essen, Universitätsstrasse 5, 45141, Essen, Germany

    Christine Erger & Torsten C. Schmidt

  3. Centre for Water and Environmental Research (ZWU), University of Duisburg-Essen, Universitätsstrasse 2, 45141, Essen, Germany

    Torsten C. Schmidt

Authors
  1. Christine Erger
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Peter Balsaa
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Friedrich Werres
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Torsten C. Schmidt
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Torsten C. Schmidt.

Electronic supplementary material

Below is the link to the electronic supplementary material.

ESM 1

(PDF 726 kb)

Rights and permissions

Reprints and permissions

About this article

Cite this article

Erger, C., Balsaa, P., Werres, F. et al. Determination of organic priority pollutants in the low nanogram-per-litre range in water by solid-phase extraction disk combined with large-volume injection/gas chromatography–mass spectrometry. Anal Bioanal Chem 405, 5215–5223 (2013). https://doi.org/10.1007/s00216-013-6918-x

Download citation

  • Received:

  • Revised:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s00216-013-6918-x

Keywords

Search

Navigation