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Simultaneous analysis of organochlorine pesticides and polychlorinated biphenyls in air samples by using accelerated solvent extraction (ASE) and solid-phase micro-extraction (SPME) coupled to gas chromatography dual electron capture detection

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Abstract

An analytical method associating accelerated solvent extraction (ASE) and solid-phase micro-extraction (SPME) in immersion mode combined with gas chromatography dual electrons capture detectors (SPME-GC-2ECD) has been developed and studied for the simultaneous determination of 19 organochlorine pesticides (OCPs) and 22 polychlorinated biphenyls (PCBs) in air samples (active and XAD-2 passive samplers). Samples were extracted with ASE with acetonitrile using the following conditions: temperature, 150 °C; pressure, 1500 psi; static, 15 min; cycles, 3; purge, 300 s; flush, 100 %. Extracts were reduced to 1 mL, and 500 μL of this extract, filled with deionised water, was subject to SPME extraction. Experimental results indicated that the proposed method attained the best extraction efficiency under the optimised conditions: extraction of PCB-OCP mixture using 100-μm PDMS fibre at 80 °C for 40 min with no addition of salt. The performance of the proposed ASE-SPME-GC-2ECD methodology with respect to linearity, limit of quantification and detection was evaluated by spiking of XAD-2 resin with target compounds. The regression coefficient (R 2) of most compounds was found to be high of 0.99. limits of detection (LODs) are between 0.02 and 4.90 ng m−3, and limits of quantification (LOQs) are between 0.05 and 9.12 ng m−3 and between 0.2 and 49 ng/sampler and 0.52 and 91 ng/sampler, respectively, for XAD-2 passive samplers. Finally, a developed procedure was applied to determine selected PCBs and OCPs in the atmosphere.

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References

  • Aguilar C, Penalver A, Pocurull E, Ferre J, Borrull F, Marce RM (1999) Optimization of solid-phase microextraction conditions using a response surface methodology to determine organochlorine pesticides in water by gas chromatography and electron-capture detection. J Chromatogr A 844:425–432

    Article  CAS  Google Scholar 

  • Aslan-Sungur G, Gaga EO, Yenisoy-Karakas S (2014) Estimation of measurement uncertainty of polychlorinated biphenyls, polycyclic aromatic hydrocarbons and organochlorine pesticides in the atmosphere using gas chromatography–mass spectrometry and gas chromatography-electron capture detector. J Chromatogr A 1325:40–48

    Article  CAS  Google Scholar 

  • Bidleman TF, Jantunen LM, Harner T, Wiberg K, Wideman JL, Brice K, Su K, Falconer RL, Aigner EJ, Leone AD, Ridal JJ, Kerman B, Finizio A, Alegria H, Parkhurst WJ, Szeto SY (1998) Chiral pesticides as tracers of air-surface exchange. Environ Pollut 102:43–49

    Article  CAS  Google Scholar 

  • Biterna M, Voutsa D (2005) Polychlorinated biphenyls in ambient air of NW Greece and in particulate emissions. Environ Int 31:671–677

    Article  CAS  Google Scholar 

  • Brás I, Santos L, Alves A (2000) Monitoring organochlorine pesticides from landfill leachates by gas chromatography—electron-capture detection after solid-phase microextraction. J Chromatogr A 891:305–311

    Article  Google Scholar 

  • Chakraborty P, Zhang G, Eckhardt S, Li J, Breivik K, Lam PKS, Tanabe S, Jones KC (2013) Atmospheric polychlorinated biphenyls in Indian cities: levels, emission sources and toxicity equivalents. Environ Pollut 182:283–290

    Article  CAS  Google Scholar 

  • Cooper DA, Peterson K, Simpson D (1996) Hydrocarbon, PAH and PCB emissions from ferries: a case study in the Skagerak–Kattegatt–Öresund region. Atmos Environ 30:2463–2473

    Article  CAS  Google Scholar 

  • Derouiche A, Ridha Driss M, Morizur J-P, Taphanel M-H (2007) Simultaneous analysis of polychlorinated biphenyls and organochlorine pesticides in water by headspace solid-phase microextraction with gas chromatography–tandem mass spectrometry. J Chromatogr A 1138:231–243

    Article  CAS  Google Scholar 

  • Gonçalves C, Alpendurada MF (2002) Comparison of three different poly(dimethylsiloxane)-divinylbenzene fibres for the analysis of pesticide multiresidues in water samples: structure and efficiency. J Chromatogr A 963:19–26

    Article  Google Scholar 

  • Granier LK, Chevreuil M (1997) Behaviour and spatial and temporal; variations of polychlorinated biphenyls and lindane in the urban atmosphere of the Paris area, France. Atmos Environ 31:3787–3802

    Article  CAS  Google Scholar 

  • Guéguen F, Stille P, Millet M (2011) Air quality assessment by tree bark biomonitoring in urban, industrial and rural environments of the Rhine valley: PCDD/Fs, PCBs and trace metal evidence. Chemosphere 85:195–212

    Article  Google Scholar 

  • Guéguen F, Stille P, Millet M (2013) Coupling accelerated solvent extraction (ASE), flash chromatography and GC-ECD for the analysis of polychorobiphenyls (PCBs) in solid samples. Application to tree barks and XAD-2 passive samplers. Talanta 111:140–146

    Article  Google Scholar 

  • Harding GC, LeBlanc RJ, Vass WP, Addison RF, Hargrave BT, Pearre S Jr, Dupuis A, Brodie PF (1997) Bioaccumulation of PCBs in the marine pelagic food web, based on a seasonal study in the southern gulf of St. Lawrence 1976–1977. Mar Chem 56:145–179

    Article  Google Scholar 

  • Hernandez F, Beltran J, Lopez FJ, Gaspar JV (2000) Use for solid-phase microextraction for quantitative determination of herbicides in soil and water samples. Anal Chem 72:2313–2322

    Article  CAS  Google Scholar 

  • Junior JLR, Re-Poppi N (2007) Determination of organochlorine pesticides in ground water samples using solid-phase microextraction by gas chromatography-electron capture detection. Talanta 72:1833–1841

  • Lara-Gonzalo A, Sánchez-Uria JE, Segovia-Garcia E, Sanz-Medel A (2012) Selected ion storage versus tandem MS/MS for organochlorine pesticides determination in drinking waters with SPME and GC-MS. Int J Environ Anal Chem 92:856–867

    Article  CAS  Google Scholar 

  • Lord H, Pawliszyn J (2000) Evolution of solid-phase microextraction technology. J Chromatogr A 885:153–193

    Article  CAS  Google Scholar 

  • Louch D, Motlagh S, Pawliszyn J (1992) Dynamics of organic compound extraction from water using liquid-coated fused fibers. Anal Chem 64:1187–1199

    Article  CAS  Google Scholar 

  • Magdic S, Pawliszyn JB (1996) Analysis of organochlorine pesticides using solid-phase microextraction. J Chromatogr A 723:111–122

    Article  CAS  Google Scholar 

  • Meire RO, Chi Lee S, Targino AC, Torres JPM, Harner T (2012) Air concentrations and transport of persistent organic pollutants (POPs) in mountains of southeast and southern Brazil. Atmos Pollut Res 3:417–425

    Article  CAS  Google Scholar 

  • Namieśnik J, Zygmunt B (2002) Selected concentration techniques for gas chromatographic analysis of environmental samples. Chromatographia 56:S9–S18

    Article  Google Scholar 

  • Norstrom RJ, Simon M, Derek CG, Schweinsburg RE (1988) Organochlorine contaminants in arctic marine food chains: identification, geographical distribution, and temporal trends in polar bears. Environ Sci Technol 22:1063–1074

    Article  CAS  Google Scholar 

  • Page BD, Lacroix G (1997) Application of solid-phase microextraction to the headspace gas chromatographic analysis of semi-volatile organochlorine contaminants in aqueous matrices. J Chromatogr A 757:173–182

    Article  Google Scholar 

  • Pérez-Trujillo JP, Frìas S, Conde JE, Rodrìguez-Delgado MA (2002) Comparison of different coatings in solid-phase microextraction for the determination of organochlorine pesticides in ground water. J Chromatogr A 963:95–105

    Article  Google Scholar 

  • Porta M, Malats N, Jariod M, Grimault JO, Rifa J, Carrato A, Guarner L, Salas A, Santiago-Silva M, Corominas JM, Andreu M, Real FX (1999) Serum levels of organochlorine compounds and K-ras mutation in exocrine pancreatic cancer. Lancet 354:2125–2129

    Article  CAS  Google Scholar 

  • Raeppel C, Fabritius M, Nief M, Appenzeller BMR, Millet M (2014) Coupling ASE, sylilation and SPME-GC/MS for the analysis of current-used pesticides in atmosphere. Talanta 121:24–29

    Article  CAS  Google Scholar 

  • Rodrigues MVN, Reyes FGR, Rehder VLG, Rath S (2005) An SPME–GC–MS method for determination of organochlorine pesticide residues in medicinal plant infusions. Chromatographia 61:291–297

  • Salquèbre G, Schummer C, Millet M, Briand O, Appenzeller BMR (2012) Multi-class pesticide analysis in human hair by gas chromatography tandem (triple quadrupole) mass spectrometry with solid phase microextraction and liquid injection. Anal Chim Acta 710:65–74

    Article  Google Scholar 

  • Sanusi A, Millet M, Mirabel P, Wortham H (2000) Airborne pesticides concentrations and α/γ-HCH ratio in Alsace (East France) air. Sci Total Environ 263:263–277

    Article  CAS  Google Scholar 

  • Scheyer A, Graeff C, Morville S, Mirabel P, Millet M (2005) Analysis of some organochlorine pesticides in an urban atmosphere (Strasbourg, east of France). Chemosphere 58:1517–1524

    Article  CAS  Google Scholar 

  • Schummer C, Tuduri L, Briand O, Appenzeller BMR, Millet M (2012) Application of XAD-2 resin-based passive samplers and SPME-GC-MS/MS analysis for the monitoring of spatial and temporal variations of atmospheric pesticides in Luxembourg. Environ Pollut 170:88–94

    Article  CAS  Google Scholar 

  • Shu YY, Wang SS, Tardif M, Huang Y (2003) Analysis of polychlorinated biphenyls in aqueous samples by microwave-assisted headspace solid-phase microextraction. J Chromatogr A 1008:1–12

    Article  CAS  Google Scholar 

  • Sofuoglu SC, Sofuoglu A, Holsen TM, Alexander CM, Pagano JJ (2014) Atmospheric concentrations and potential sources of PCBs, PBDEs, and pesticides to Acadia national park. Environ Pollut 177:116–124

    Article  Google Scholar 

  • Tombesi N, Pozo K, Harner T (2014) Persistent organic pollutants (POPs) in the atmosphere of agricultural and urban areas in the province of Buenos Aires in Argentina using PUF disk passive air samplers. Atmos Pollut Res 5:170–178

    Article  CAS  Google Scholar 

  • Wania F, Shen L, Lei YD, Teixeira C, Muir DCG (2003) Development and calibration of a resin-based passive sampling system for monitoring persistent organic pollutants in the atmosphere. Environ Sci Technol 37:1352–1359

  • Yeo H-G, Choi M, Chun M-Y, Sunwoo Y (2003) Gas/particle concentrations and partitioning of PCBs in the atmosphere of Korea. Atmos Environ 37:3561–3570

    Article  CAS  Google Scholar 

  • Yu Y, Miller DJ, Hawthorne SB (1998) Solid-phase microextraction of polychlorinated biphenyls. J Chromatogr A 800:257–266

    Article  Google Scholar 

Download references

Acknowledgments

Financial support to the project from the CNRS for the “Zone Atelier de l’Environnement urbain de Strasbourg”(za-eus.in2p3.fr) as well as from REALISE, the Alsace network of engineering and research laboratories for environmental sciences (realise.unistra.fr) is gratefully acknowledged.

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Authors and Affiliations

  1. Laboratoire des Matériaux, Catalyse, Environnement et Méthodes Analytiques (MCEMA), Ecole doctorale des sciences et technologie, Beirut, Lebanon

    Haifaa Mokbel, Enaam Jamal Al Dine & Ahmad Elmoll

  2. Institut de Chimie et Procédés pour l’Energie, l’Environnement et la Santé (ICPEES)—Groupe de Physico-Chimie de l’Atmosphère (UMR 7515 CNRS-Université de Strasbourg), 1 rue Blessig, F-67084, Strasbourg Cedex, France

    Haifaa Mokbel, Enaam Jamal Al Dine, Céline Liaud & Maurice Millet

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  1. Haifaa Mokbel
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  2. Enaam Jamal Al Dine
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  3. Ahmad Elmoll
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  4. Céline Liaud
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  5. Maurice Millet
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Correspondence to Maurice Millet.

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Responsible editor: Philippe Garrigues

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Mokbel, H., Al Dine, E.J., Elmoll, A. et al. Simultaneous analysis of organochlorine pesticides and polychlorinated biphenyls in air samples by using accelerated solvent extraction (ASE) and solid-phase micro-extraction (SPME) coupled to gas chromatography dual electron capture detection. Environ Sci Pollut Res 23, 8053–8063 (2016). https://doi.org/10.1007/s11356-016-6072-z

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  • DOI: https://doi.org/10.1007/s11356-016-6072-z

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