International Journal of Environmental Monitoring and Analysis

| Peer-Reviewed |

GC/MS Monitoring of Selected PAHs in Soil Samples Using Ultrasound-assisted QuEChERS in Tandem with Dispersive Liquid-Liquid Microextraction

Received: 17 September 2015    Accepted: 30 September 2015    Published: 30 October 2015
Views:       Downloads:

Share This Article

Abstract

Herein, a method consisting of ultrasound-assisted QuEChERS in tandem with dispersive liquid-liquid microextraction (DLLME) was developed for monitoring of selected polycyclic aromatic hydrocarbons (PAHs) in various soil samples using gas chromatography coupled to a single quadrupole mass spectrometry (GC/MS). Ultrasound-assisted QuEChERS was employed to extract the PAHs from 2.0 g of soil using 7 ml of initial extraction solvent (acetonitrile: water (5:2 v/v)) and the salt mixture. The resulting supernatant extract was cleaned through the addition of C18, PSA and the mix salt followed by centrifugation, decantation and filtration. Of the clean organic phase, 1.0 ml was withdrawn and added with12 µl of C2Cl4 (disperser solvent). The resulting mixture was then injected rapidly into an aqueous sample (5.0 ml) by a syringe for further preconcentration. As a result, the cloudy solution consisting of fine particles of the extraction solvent dispersed into the aqueous phase was formed. After centrifuging, the fine particles were sedimented at the bottom of the conical test tube (5.0 ± 0.5µl). Of which, 1.0 µl was injected to the GC/MS for monitoring of the PAHs. Several influential parameters including ultrasound extraction time, initial extraction and disperser solvent and their respective volumes were all evaluated to achieve the optimal conditions. Under the optimal conditions, limits of quantification (2.5-4.0 ng/g) and linear ranges (r2≥ 0.98) were obtained for the PAHs. The method was then successfully applied for the extraction and monitoring of the PAHs in the real soil samples. Accuracy of the method was evaluated by the relative recovery experiments on spiked samples with the results ranging from 81 to 92%. In the mean time, the relative standard deviations (RSDs) were found to be in the range of 4.8–15.9%.

DOI 10.11648/j.ijema.20150305.17
Published in International Journal of Environmental Monitoring and Analysis (Volume 3, Issue 5, October 2015)
Page(s) 288-292
Creative Commons

This is an Open Access article, distributed under the terms of the Creative Commons Attribution 4.0 International License (http://creativecommons.org/licenses/by/4.0/), which permits unrestricted use, distribution and reproduction in any medium or format, provided the original work is properly cited.

Copyright

Copyright © The Author(s), 2024. Published by Science Publishing Group

Keywords

PAHs, Ultrasound-Assisted QuEChERS, Dispersive Liquid-Liquid Microextraction, Soil Samples

References
[1] L. Duedahl-Olesen, Polycyclic aromatic hydrocarbons (PAHs) in foods, National Food Institute Technical University of Denmark, Denmark, Woodhead Publishing Limited: 2013.
[2] R. Dabestani and I. N. Ivanov “A Compilation of Physical, Spectroscopic and Photophysical Properties of Polycyclic Aromatic Hydrocarbons” Photochemistry and Photobiology, vol. 70, pp. 10-34, 1999.
[3] T. Vo-Dinh, J. Fetzer and A. D. Campiglia “Monitoring and characterization of polyaromatic compounds in the environment” Talanta, vol. 47, pp. 943-969, 1998.
[4] P. Villar, M. Callejón, E.Alonso, J. C. Jiménez and A. Guiraúm“Optimization and validation of a new method of analysis for polycyclic aromatic hydrocarbons in sewage sludge by liquid chromatography after microwave assisted extraction” Analytica Chimica Acta, vol. 524, pp. 295–304, 2004.
[5] L. Correia-Sá, V. C. Fernandes, M. Carvalho, C. Calhau, V. F. Domingues and C. Delerue-Matos “Optimization of QuEChERS method for the analysis of organochlorine pesticides in soils with diverse organic matter” Journal of Separation Science, vol. 35, pp. 1521-1530, 2012.
[6] C. G. Pinto, S. H. Martín, J. L. P. Pavón and B. M. Cordero (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” Analytica Chimica Acta, vol. 689, pp. 129-136, 2011.
[7] V. Jose, L. Correia-Sá, P. Paíga, I. Bragança, V. C. Fernandes, V. F. Domingues and C. Delerue-Matos “QuEChERS and soil analysis” An Overview. Sample preparation, pp. 54-77, 2013.
[8] S. Kahn, L. Aijun, S. Zhang, Q. Hu and Y. G. Zhu, “Accumulation of polycyclic aromatic hydrocarbons and heavy metals in lettuce grown in the soils contaminated with long-term wastewater irrigation” Journal of Hazardous Materials, vol.152, pp. 506-515, 2008.
[9] M. Nording, K. Frech, Y. Persson, M. Forsman and P. Haglund, “Accumulation of polycyclic aromatic hydrocarbons and heavy metals in lettuce grown in the soils contaminated with long-term wastewater irrigation”Analytica Chimica Acta, vol. 555, pp. 107-113, 2006.
[10] T. Wenzl, R. Simon, J. Kleiner and E. Anklam, ”Analytical methods for polycyclic aromatic hydrocarbons (PAHs) in food and the environment needed for new food legislation in the European Union, Trends in Analytical Chemistry, vol. 25, pp. 716-725, 2006.
[11] S. S. Caldas, C. M. Bolzan, M. B. Cerqueira, D. Tomasini, E. B. Furlong, C. Fagundes and E. G. Primel, “Evaluation of a Modified QuEChERS Extraction of Multiple Classes of Pesticides from a Rice Paddy Soil by LC-APCI-MS/MS” Journal of Agricultural Food Chemistry, vol. 59, pp. 11918-11926, 2011.
[12] A. Rashid, S. Nawaz, H. Barker, I. Ahmad and M. Ashraf, “Development of a simple extraction and clean-up procedure for determination of organochlorine pesticides in soil using gas chromatography-tandem mass spectrometry” Journal of Chromatography A, vol. 1217, pp. 2933-2939, 2010.
[13] Y. H. Wang, L. W. Du, X.M. Zhou, H.H. Tan, L.Y. Bai, D.Q. Zeng and H. Tian, “QuEChERS extraction for high performance liquid chromatographic determination of pyrazosulfuron-ethyl in soils” Journal of Chemical Society of Pakistan, vol. 34, pp.28-32, 2012.
[14] C. G. Pinto, M. E. F. Laespada, S. H. Martín, A. M. C. Ferreira, J. L. P. Pavón and B. M. Cordero “Simplified QuEChERS approach for the extraction of chlorinated compounds from soil samples” Talanta, vol. 81, pp. 385-391, 2010.
[15] M. Asensio-Ramos, J. Hernandez-Borges, L. M. Ravelo-Perez and M. A. Rodriguez-Delgado “Evaluation of a modified QuEChERS method for the extraction of pesticides from agricultural, ornamental and forestal soils” Analytical and Bioanalytical Chemistry, vol. 396, pp. 2307-2319, 2010.
[16] M. Rezaee, Y. Assadi, M. R. Milani-Hosseini, E. Aghaee, F. Ahmadi and S. Berijani “Determination of organic compounds in water using dispersive liquid–liquid microextraction” Journal of Chromatography A, vol. 1116, pp. 1–9, 2006.
[17] M. Rezaee, Y. Yamini, M. Moradi, A. Saleh, M. Faraji and M. H. Naeen “Supercritical fluid extraction combined with dispersive liquid–liquid microextraction as a sensitive and efficient sample preparation method for determination of organic compounds in solid samples” Journal of Supercritical Fluids, vol. 55, pp.161-168, 2010.
[18] M. Rezaee, Y. Yamini and M. Faraji, “Evolution of dispersive liquid–liquid microextraction method” Journal of Chromatography A, vol. 1217, pp. 2342-2357, 2010.
[19] J. Kowalski, R. A. Amanda and J. Cochran (2013) “QuEChERS: The Concept”www.sepscience.com; Europe, 5.
Author Information
  • Department of Chemistry, Payame Noor University, Tehran, Iran

Cite This Article
  • APA Style

    Hamid Reza Sobhi. (2015). GC/MS Monitoring of Selected PAHs in Soil Samples Using Ultrasound-assisted QuEChERS in Tandem with Dispersive Liquid-Liquid Microextraction. International Journal of Environmental Monitoring and Analysis, 3(5), 288-292. https://doi.org/10.11648/j.ijema.20150305.17

    Copy | Download

    ACS Style

    Hamid Reza Sobhi. GC/MS Monitoring of Selected PAHs in Soil Samples Using Ultrasound-assisted QuEChERS in Tandem with Dispersive Liquid-Liquid Microextraction. Int. J. Environ. Monit. Anal. 2015, 3(5), 288-292. doi: 10.11648/j.ijema.20150305.17

    Copy | Download

    AMA Style

    Hamid Reza Sobhi. GC/MS Monitoring of Selected PAHs in Soil Samples Using Ultrasound-assisted QuEChERS in Tandem with Dispersive Liquid-Liquid Microextraction. Int J Environ Monit Anal. 2015;3(5):288-292. doi: 10.11648/j.ijema.20150305.17

    Copy | Download

  • @article{10.11648/j.ijema.20150305.17,
      author = {Hamid Reza Sobhi},
      title = {GC/MS Monitoring of Selected PAHs in Soil Samples Using Ultrasound-assisted QuEChERS in Tandem with Dispersive Liquid-Liquid Microextraction},
      journal = {International Journal of Environmental Monitoring and Analysis},
      volume = {3},
      number = {5},
      pages = {288-292},
      doi = {10.11648/j.ijema.20150305.17},
      url = {https://doi.org/10.11648/j.ijema.20150305.17},
      eprint = {https://download.sciencepg.com/pdf/10.11648.j.ijema.20150305.17},
      abstract = {Herein, a method consisting of ultrasound-assisted QuEChERS in tandem with dispersive liquid-liquid microextraction (DLLME) was developed for monitoring of selected polycyclic aromatic hydrocarbons (PAHs) in various soil samples using gas chromatography coupled to a single quadrupole mass spectrometry (GC/MS). Ultrasound-assisted QuEChERS was employed to extract the PAHs from 2.0 g of soil using 7 ml of initial extraction solvent (acetonitrile: water (5:2 v/v)) and the salt mixture. The resulting supernatant extract was cleaned through the addition of C18, PSA and the mix salt followed by centrifugation, decantation and filtration. Of the clean organic phase, 1.0 ml was withdrawn and added with12 µl of C2Cl4 (disperser solvent). The resulting mixture was then injected rapidly into an aqueous sample (5.0 ml) by a syringe for further preconcentration. As a result, the cloudy solution consisting of fine particles of the extraction solvent dispersed into the aqueous phase was formed. After centrifuging, the fine particles were sedimented at the bottom of the conical test tube (5.0 ± 0.5µl). Of which, 1.0 µl was injected to the GC/MS for monitoring of the PAHs. Several influential parameters including ultrasound extraction time, initial extraction and disperser solvent and their respective volumes were all evaluated to achieve the optimal conditions. Under the optimal conditions, limits of quantification (2.5-4.0 ng/g) and linear ranges (r2≥ 0.98) were obtained for the PAHs. The method was then successfully applied for the extraction and monitoring of the PAHs in the real soil samples. Accuracy of the method was evaluated by the relative recovery experiments on spiked samples with the results ranging from 81 to 92%. In the mean time, the relative standard deviations (RSDs) were found to be in the range of 4.8–15.9%.},
     year = {2015}
    }
    

    Copy | Download

  • TY  - JOUR
    T1  - GC/MS Monitoring of Selected PAHs in Soil Samples Using Ultrasound-assisted QuEChERS in Tandem with Dispersive Liquid-Liquid Microextraction
    AU  - Hamid Reza Sobhi
    Y1  - 2015/10/30
    PY  - 2015
    N1  - https://doi.org/10.11648/j.ijema.20150305.17
    DO  - 10.11648/j.ijema.20150305.17
    T2  - International Journal of Environmental Monitoring and Analysis
    JF  - International Journal of Environmental Monitoring and Analysis
    JO  - International Journal of Environmental Monitoring and Analysis
    SP  - 288
    EP  - 292
    PB  - Science Publishing Group
    SN  - 2328-7667
    UR  - https://doi.org/10.11648/j.ijema.20150305.17
    AB  - Herein, a method consisting of ultrasound-assisted QuEChERS in tandem with dispersive liquid-liquid microextraction (DLLME) was developed for monitoring of selected polycyclic aromatic hydrocarbons (PAHs) in various soil samples using gas chromatography coupled to a single quadrupole mass spectrometry (GC/MS). Ultrasound-assisted QuEChERS was employed to extract the PAHs from 2.0 g of soil using 7 ml of initial extraction solvent (acetonitrile: water (5:2 v/v)) and the salt mixture. The resulting supernatant extract was cleaned through the addition of C18, PSA and the mix salt followed by centrifugation, decantation and filtration. Of the clean organic phase, 1.0 ml was withdrawn and added with12 µl of C2Cl4 (disperser solvent). The resulting mixture was then injected rapidly into an aqueous sample (5.0 ml) by a syringe for further preconcentration. As a result, the cloudy solution consisting of fine particles of the extraction solvent dispersed into the aqueous phase was formed. After centrifuging, the fine particles were sedimented at the bottom of the conical test tube (5.0 ± 0.5µl). Of which, 1.0 µl was injected to the GC/MS for monitoring of the PAHs. Several influential parameters including ultrasound extraction time, initial extraction and disperser solvent and their respective volumes were all evaluated to achieve the optimal conditions. Under the optimal conditions, limits of quantification (2.5-4.0 ng/g) and linear ranges (r2≥ 0.98) were obtained for the PAHs. The method was then successfully applied for the extraction and monitoring of the PAHs in the real soil samples. Accuracy of the method was evaluated by the relative recovery experiments on spiked samples with the results ranging from 81 to 92%. In the mean time, the relative standard deviations (RSDs) were found to be in the range of 4.8–15.9%.
    VL  - 3
    IS  - 5
    ER  - 

    Copy | Download

  • Sections