Skip to main content
SpringerLink
Log in

Validation of an Adapted QuEChERS Method for the Simultaneous Analysis of Polycyclic Aromatic Hydrocarbons, Polychlorinated Biphenyls and Organochlorine Pesticides in Sediment by Gas Chromatography–Mass Spectrometry

  • Published:
Bulletin of Environmental Contamination and Toxicology Aims and scope Submit manuscript

Abstract

A Quick, Easy, Cheap, Effective, Rugged and Safe (QuEChERS) method has been adapted and validated for the simultaneous analysis of 16 PAHs, 12 PCBs and 9 OCPs in sediment. The sample preparation was adapted by modifying the nature of the extraction solvent, the extraction technique and the amount of sediment. The analytical performances were evaluated in terms of accuracy, linearity and quantification limits. The method was validated by the analysis of a reference marine sediment material (SRM 1941b). The obtained concentrations are in good agreement with the certified values with recoveries ranging 60 %–103 % for most of PAHs. Acceptable recoveries are obtained for PCBs, ranging 76 %–131 %, and for OCPs ranging 81 %–137 %. The method was applied to the analysis of sediments from the hydro-system Bizerte Lagoon/Ichkeul Lake (Tunisia). The Bizerte lagoon is mainly contaminated by PAHs whereas the Ichkeul lake is mainly by OCPs.

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

  • Anastassiades M, Lehotay SJ, Stajnbaher D, Schenck FJ (2003) Fast and easy multiresidue method employing acetonitrile extraction/partitioning and “dispersive solid-phase extraction” for the determination of pesticide residues in produce. JAOAC Int 86:412–431

    CAS  Google Scholar 

  • Bartolomé L, Cortazar E, Raposo JC, Usobiaga A, Zuloaga O, Etxebarria N, Fernandez LA (2005) Simultaneous microwave-assisted extraction of polycyclic aromatic hydrocarbons, polychlorinated biphenyls, phthalate esters and nonylphenols in sediments. J Chromatogr A 1068:229–236

    Article  Google Scholar 

  • Ben Said O, Goñi-Urriza M, El Bour M, Aissa P, Duran R (2010) Characterization of aerobic polycyclic aromatic hydrocarbon-degrading bacteria from Bizerte lagoon sediments, Tunisia. Microbiol Ecol 59:445–456

    Article  Google Scholar 

  • Bragança I, Plácido A, Paíga P, Domingues VF, Delerue Matos C (2012) QuEChERS: a new sample preparation approach for the determination of ibuprofen and its metabolites in soils. Sci Total Environ 433:281–289

    Article  Google Scholar 

  • Brondi SHG, de Macedo AN, Vicente GHL, Nogueira ARA (2011) Evaluation of the QuEChERS method and gas chromatography–mass spectrometry for the analysis pesticide residues in water and sediment. Bull Environ Contam Toxicol 86:18–22

    Article  CAS  Google Scholar 

  • Carvalho PN, Rodrigues PNR, Alves F, Evangelista R, Basto MCP, Vasconcelos MTSD (2008) An expeditious method for the determination of organochlorine pesticides residues in estuarine sediments using microwave assisted pre-extraction and automated headspace solid-phase microextraction coupled to gas chromatography–mass spectrometry. Talanta 76:1124–1129

    Article  CAS  Google Scholar 

  • Cieslik E, Sadowska-Rociek A, Molina Ruiz JM, Surma-Zadora M (2011) Evaluation of QuEChERS method for the determination of organochlorine pesticide residues in select groups of fruits. Food Chem 125:773–778

    Article  CAS  Google Scholar 

  • Concha-Graña E, Fernández-González V, Grueiro-Noche G, Muniategui-Lorenzo S, López-Mahía P, Fernández-Fernández E, Prada-Rodríguez D (2010) Development of an environmental friendly method for the analysis of organochlorine pesticide in sediments. Chemosphere 79:698–705

    Article  Google Scholar 

  • Cueva-Mestanza R, Sosa-Ferrera Z, Torres-Padrón ME, Santana-Rodríguez JJ (2008) Preconcentration of pharmaceuticals residues in sediment samples using microwave assisted micellar extraction coupled with solid phase extraction and their determination by HPLC–UV. J Chromatogr B 863:150–157

    Article  CAS  Google Scholar 

  • de Boer J, Law RJ (2003) Developments in the use of chromatographic techniques in marine laboratories for the determination of halogenated contaminants and polycyclic aromatic hydrocarbons. J Chromatogr A 1000:223–251

    Article  Google Scholar 

  • Errekatxo A, Prieto A, Zuloaga O, Usobiaga A, Etxebarria N, Fernández LA (2008) Simultaneous extraction of several persistent organic pollutants in sediment using focused ultrasonic solid–liquuid extraction. Anal Bioanal Chem 392:1471–1478

    Article  CAS  Google Scholar 

  • Itoh N, Numata M, Aoyagi Y, Yarita T (2008) Comparison of low-level polycyclic aromatic hydrocarbons in sediment revealed by Soxhlet extraction, microwave-assisted extraction, and pressurized liquid extraction. Anal Chim Acta 612:44–52

    Article  CAS  Google Scholar 

  • Kayal S, Connell DW (1995) Polycyclic Aromatic Hydrocarbons in Biota from the Brisbane River Estuary, Australia. Estuar Coast Shelf Sci 40:475–493

    Article  CAS  Google Scholar 

  • Lee SW, Choi JH, Cho SK, Yu HA, Abd El-Aty AM, Shim JH (2011) Development of a new QuEChERS method based on dry ice for the determination of 168 pesticides in paprika using tandem mass spectrometry. J Chromatogr A 1218:4366–4377

    Article  CAS  Google Scholar 

  • Lehotay SJ, Ae Son K, Kwon H, Koesukwiwat U, Fu W, Mastovska K, Hoh E, Leepipatpiboon N (2010) Comparison of QuEChERS sample preparation methods for the analysis of pesticide residues in fruits and vegetables. J Chromatogr A 1217:2548–2560

    Article  CAS  Google Scholar 

  • Moreno DA, Ilic N, Poulev A, Raskin I (2006) Effects of Arachis hypogaea nutshell extract on lipid metabolic enzymes and obesity parameters. Life Sci 78:2797–2803

    Article  CAS  Google Scholar 

  • Mzoughi N, Dachraoui M, Villeneuve JP (2005) Evaluation of aromatic hydrocarbons by spectrofluorometry in marine sediments and biological matrix: what reference should be considered? C R Chim 8:97–102

    Article  CAS  Google Scholar 

  • Norli HR, Christiansen A, Deribe E (2011) Application of QuEChERS method for extraction of selected persistent organic pollutants in fish tissue and analysis by gas chromatography mass spectrometry. J Chromatogr A 1218:7234–7241

    Article  CAS  Google Scholar 

  • Peysson W, Vulliet E (2013) Determination of 136 pharmaceuticals and hormones in sewage sludge using quick, easy, cheap, effective, rugged and safe extraction followed by analysis with liquid chromatography-time-of-flight-mass spectrometry. J Chromatogr A 1290:46–61

    Article  CAS  Google Scholar 

  • Pinto CG, Herrero Martín S, Pérez Pavón JL, Moreno Cordero B (2011) A simplified quick, easy, cheap, effective, rugged and safe approach for the determination of trihalomethanes and benzene, toluene, ethylbenzene and xylenes in soil matrices by fast gas chromatography with mass spectrometry detection. Anal Chim Acta 689:129

    Article  Google Scholar 

  • Ramalhosa MJ, Paiga P, Morais S, Delerue-Matos C, Oliveira MB (2009) Analysis of polycyclic aromatic hydrocarbons in fish: evaluation of a quick, easy, cheap, effective, rugged, and safe extraction method. J Sep Sci 32:3529–3538

    Article  CAS  Google Scholar 

  • Rouvière F, Bulete A, Cren-Olive C, Arnaudguilhem C (2012) Multiresidue analysis of aromatic organochlorines in soil by gas chromatography-mass spectrometry and QuEChERS extraction based on water/dichloromethane partitioning. Comparison with accelerated solvent extraction. Talanta 93:336–344

    Article  Google Scholar 

  • Subedi B, Aguilar L, Robinson EM, Hageman KJ, Björklund E, Sheesley RJ, Usenko S (2015) Selective pressurized liquid extraction as a sample-preparation technique for persistent organic pollutants and contaminants of emerging concern. TRAC-Trend Anal Chem 68:119–132

    Article  CAS  Google Scholar 

  • Thompson S, Budzinski H, LeMenach K, Letellier M, Garrigues P (2002) Multi-residue analysis of polycyclic aromatic hydrocarbons, polychlorobiphenyls, and organochlorine pesticides in marine sediments. Anal Bioanal Chem 372:196–204

    Article  CAS  Google Scholar 

  • Vagi MC, Petsas AS, Kostopoulou MN, Karamanoli MK, Lekkas TD (2007) Determination of organochlorine pesticides in marine sediments samples using ultrasonic solvent extraction followed by GC/ECD. Desalination 210:146–156

    Article  CAS  Google Scholar 

  • Wang L, Zhao P, Zhang F, Li Y, Du F, Pan C (2012) Dissipation and residue behavior of emamectin benzoate on apple and cabbage field application. Ecotox Environ Safe 78:260–264

    Article  CAS  Google Scholar 

  • Wilkowska A, Biziuk M (2011) Determination of pesticide residues in food matrices using the QuEChERS methodology. Food Chem 125:803–812

    Article  CAS  Google Scholar 

  • Yang XB, Ying GG, Kookana RS (2010) Rapid multiresidue determination for currently used pesticides in agricultural drainage waters and soils using gas chromatography–mass spectrometry. J Environ Sci Health B 45:152–161

    Article  CAS  Google Scholar 

Download references

Author information

Authors and Affiliations

  1. Laboratoire de Biosurveillance de l’Environnement, Faculté des Sciences de Bizerte, Université de Carthage, 7021 Zarzouna, Bizerte, Tunisia

    Fida Ben Salem & Olfa Ben Said

  2. Equipe Environnement et Microbiologie – IPREM UMR 5254 CNRS, Université de Pau et des Pays de l’Adour, Pau, France

    Fida Ben Salem, Olfa Ben Said & Robert Duran

  3. Laboratoire de Chimie Analytique Bio-Inorganique et Environnement, IPREM UMR 5254 CNRS, Université de Pau et des Pays de l’Adour, Pau, France

    Fida Ben Salem & Mathilde Monperrus

  4. UFR Sciences et Techniques de la Côte Basque Allée du Parc Montaury, 64600, Anglet, France

    Mathilde Monperrus

Authors
  1. Fida Ben Salem
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Olfa Ben Said
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Robert Duran
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Mathilde Monperrus
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Mathilde Monperrus.

Electronic supplementary material

Below is the link to the electronic supplementary material.

Supplementary material 1 (DOCX 20 kb)

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Ben Salem, F., Ben Said, O., Duran, R. et al. Validation of an Adapted QuEChERS Method for the Simultaneous Analysis of Polycyclic Aromatic Hydrocarbons, Polychlorinated Biphenyls and Organochlorine Pesticides in Sediment by Gas Chromatography–Mass Spectrometry. Bull Environ Contam Toxicol 96, 678–684 (2016). https://doi.org/10.1007/s00128-016-1770-2

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s00128-016-1770-2

Keywords

Search

Navigation