Rapid Determination of PCDDs, PCDFs and DL-PCBs in Foods, Feedingstuffs and Vegetable Oils Using New Modified Acid Silica

Ovanes Chakoyan

doi:doi:10.11648/j.cbe.20230801.11

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Rapid Determination of PCDDs, PCDFs and DL-PCBs in Foods, Feedingstuffs and Vegetable Oils Using New Modified Acid Silica

Ovanes Chakoyan

Published in Chemical and Biomolecular Engineering (Volume 8, Issue 1)

Received: 2 December 2022 Accepted: 4 January 2023 Published: 9 June 2023

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Abstract

Polychlorinated dibenzo-p-dioxins, dibenzofurans and dioxin-like polychlorinated biphenyls are persistent organic pollutants (POPs), which in the recent years received huge attention due to their extreme stability, high potential toxicity and bioaccumulation in food chains. Main source of human exposure to these compounds is discovered in foods of animal origin, especially foods rich of fat. The target of the present study was to set up an analytical method for the determination of PCDDs/PCDFs and DL-PCB in vegetable oils, sunflower meals, sunflower seeds, rapeseeds and milk powder. The first step consisted of a semi-automatic Soxhlet extraction for 3 hours, by using a mixture of Hexane: Acetone - 80: 20, followed by acid digestion with 55% acid silica, and filtration. After concentration, the extract is purified on multilayer column (silica gel, silica-KOH, silica-H₂SO₄, anhydrous Na₂SO₄) followed by an alumina column separation in two fractions (first fraction containing PCDDs/PCDFs, and second containing only PCBs). The purified extract was then analyzed by GC/MS/MS. The newly developed approach in our lab was capable to reduce the overall time of sample preparation down to seven hours/per sample. Since the method shows good mean recoveries for all labelled congeners spiked in the samples (for PCDDs/PCDFs – 80-110%, for DL-PCBs – 70-85%), we assumed the absence of overestimation or underestimation in the analyzed samples.

Published in	Chemical and Biomolecular Engineering (Volume 8, Issue 1)
DOI	10.11648/j.cbe.20230801.11
Page(s)	1-15
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), 2023. Published by Science Publishing Group

Keywords

Oil, Extraction, Polychlorinated-p-Dioxins, Polychlorinated Dibenzofurans, Polychlorinated Biphenyls, GC/MS/MS

References

[1]	Van den Berg, M.; Birnbaum, L. S.; Denison, M.; De Vito, M.; Farland, W.; Feeley, M.; Fiedler, H.; Hakansson, H.; Hanberg, A.; Haws, L.; et al. The 2005 World Health Organization reevaluation of human and mammalian toxic equivalency factors for dioxins and dioxin-like compounds. Toxicol. Sci. 2006, 93, 223–241.
[2]	European Commission (EC) 2006. Commission Regulation No. 199/2006 of 3 February 2006 amending Regulation (EC) No 466/2001 setting maximum levels for certain contaminants in foodstuffs as regards dioxins and dioxin-like PCBs. Off J, L 32, 04/02/2006, 34-38.
[3]	Ellison S. L. R., Rosslein M. & Williams A. (eds). 2000. EURACHEM/CITAC Guide CG4: Quantifying uncertainty in analytical measurement, Second Ed. EURACHEM, QUAM: 2000. 1, 120 pp.
[4]	Method 1613, “Tetra-through Octa-Chlorinated Dioxins and Furans by Isotope Dilution HRGC/HRMS’’, Revision A, October 1993.
[5]	Method 1668 Rev. A: Chlorinated biphenyl congeners in water, soil, sediment, and tissue by HRGC/HRMS. USEPA, Washington DC.
[6]	Furst P. 2001. Contribution of dioxin-like PCB to total toxic equivalents of dairy products. Organohalogen Compounds, 51, 279-282.
[7]	Takakura M., Lehardy T., Marchard P. Analysis of Dioxins in Foods and Feeds Using GC-MS/MS, First Edition, July, 2018.
[8]	Hamm S., Grumping R. & Shwietering J. 2005. Levels of polychlorinated dibenzo(p)dioxins, dibenzofurans and dioxin-like PCBs in milk, milk products and eggs from west European countries. Organohalogen Compounds, 60, 199-202.
[9]	Vestraete F. 2005. EU-strategy to reduce the presence of dioxins, furans and dioxin-like PCBs in feed and food-existing measures. Organohalogen Compounds, 67, 1421-1423.
[10]	De Greyt, W., J. De Kock, M. Kokken, and M. Kellens. Removal of Contaminants from edible oils: Current Status and Future Developments. Paper presented at the Lipidforum Seminar on Recent Developments in the Processing of Oils and Fats, Blue Lagoon, Iceland, September 28-20, 2000.
[11]	Van den Berg, M., L. S. Birnbaum, A. T. C. Bosveld, B. Brunstorm, P. Cook, M. Feeley, J. P. Giesy, A. Hanberg, R. Hasegawa, S. W. Kennedy, T. et al., Toxic Equivalent Factors (TEFs) for PCBS, PCDDs, PCDFs for Humans and Wildlife, Environ. Health Perspect. 106: 775-792 (1998).
[12]	Fiedler, H., Cooper K. R., Bergek, S., Hjelt, M., Rappe, C. Polychlorinated dibenzodiuoxins and polychlorinated dibenzofurans (PCDD/PCDF) in food samples collected in Southern Mississippi, USA. Chemospfere 34, 1411-1419.
[13]	Ramos, L., Eljarrat, E., Henandez, L. M., Rivera, J., Gonzales, M. J. Levels of PCBs, PCDDs and PCDFs in commercial butter samples in Spain. Chemosphere 38, 3141-3153 (1999).
[14]	Bosio, A., Llobet, J. M., Domingo, J. L., Casas, C., Teixido, A., and Muller, L., 2002. Levels of PCDD/PCDFs in food samples from Catalonia, Spain, Organohalogen Compounds 57, 105.
[15]	EC Directive 2044/44/EC of 13 April 2004 amending Directive 2002/69/EC laying down the sampling methods and the methods of analysis for the official control of dioxins and the determination of dioxin-like PCBs in foodstuffs. OJEC L113/17.

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APA Style

Ovanes Chakoyan. (2023). Rapid Determination of PCDDs, PCDFs and DL-PCBs in Foods, Feedingstuffs and Vegetable Oils Using New Modified Acid Silica. Chemical and Biomolecular Engineering, 8(1), 1-15. https://doi.org/10.11648/j.cbe.20230801.11

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ACS Style

Ovanes Chakoyan. Rapid Determination of PCDDs, PCDFs and DL-PCBs in Foods, Feedingstuffs and Vegetable Oils Using New Modified Acid Silica. Chem. Biomol. Eng. 2023, 8(1), 1-15. doi: 10.11648/j.cbe.20230801.11

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AMA Style

Ovanes Chakoyan. Rapid Determination of PCDDs, PCDFs and DL-PCBs in Foods, Feedingstuffs and Vegetable Oils Using New Modified Acid Silica. Chem Biomol Eng. 2023;8(1):1-15. doi: 10.11648/j.cbe.20230801.11

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@article{10.11648/j.cbe.20230801.11,
  author = {Ovanes Chakoyan},
  title = {Rapid Determination of PCDDs, PCDFs and DL-PCBs in Foods, Feedingstuffs and Vegetable Oils Using New Modified Acid Silica},
  journal = {Chemical and Biomolecular Engineering},
  volume = {8},
  number = {1},
  pages = {1-15},
  doi = {10.11648/j.cbe.20230801.11},
  url = {https://doi.org/10.11648/j.cbe.20230801.11},
  eprint = {https://article.sciencepublishinggroup.com/pdf/10.11648.j.cbe.20230801.11},
  abstract = {Polychlorinated dibenzo-p-dioxins, dibenzofurans and dioxin-like polychlorinated biphenyls are persistent organic pollutants (POPs), which in the recent years received huge attention due to their extreme stability, high potential toxicity and bioaccumulation in food chains. Main source of human exposure to these compounds is discovered in foods of animal origin, especially foods rich of fat. The target of the present study was to set up an analytical method for the determination of PCDDs/PCDFs and DL-PCB in vegetable oils, sunflower meals, sunflower seeds, rapeseeds and milk powder. The first step consisted of a semi-automatic Soxhlet extraction for 3 hours, by using a mixture of Hexane: Acetone - 80: 20, followed by acid digestion with 55% acid silica, and filtration. After concentration, the extract is purified on multilayer column (silica gel, silica-KOH, silica-H2SO4, anhydrous Na2SO4) followed by an alumina column separation in two fractions (first fraction containing PCDDs/PCDFs, and second containing only PCBs). The purified extract was then analyzed by GC/MS/MS. The newly developed approach in our lab was capable to reduce the overall time of sample preparation down to seven hours/per sample. Since the method shows good mean recoveries for all labelled congeners spiked in the samples (for PCDDs/PCDFs – 80-110%, for DL-PCBs – 70-85%), we assumed the absence of overestimation or underestimation in the analyzed samples.},
 year = {2023}
}

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TY  - JOUR
T1  - Rapid Determination of PCDDs, PCDFs and DL-PCBs in Foods, Feedingstuffs and Vegetable Oils Using New Modified Acid Silica
AU  - Ovanes Chakoyan
Y1  - 2023/06/09
PY  - 2023
N1  - https://doi.org/10.11648/j.cbe.20230801.11
DO  - 10.11648/j.cbe.20230801.11
T2  - Chemical and Biomolecular Engineering
JF  - Chemical and Biomolecular Engineering
JO  - Chemical and Biomolecular Engineering
SP  - 1
EP  - 15
PB  - Science Publishing Group
SN  - 2578-8884
UR  - https://doi.org/10.11648/j.cbe.20230801.11
AB  - Polychlorinated dibenzo-p-dioxins, dibenzofurans and dioxin-like polychlorinated biphenyls are persistent organic pollutants (POPs), which in the recent years received huge attention due to their extreme stability, high potential toxicity and bioaccumulation in food chains. Main source of human exposure to these compounds is discovered in foods of animal origin, especially foods rich of fat. The target of the present study was to set up an analytical method for the determination of PCDDs/PCDFs and DL-PCB in vegetable oils, sunflower meals, sunflower seeds, rapeseeds and milk powder. The first step consisted of a semi-automatic Soxhlet extraction for 3 hours, by using a mixture of Hexane: Acetone - 80: 20, followed by acid digestion with 55% acid silica, and filtration. After concentration, the extract is purified on multilayer column (silica gel, silica-KOH, silica-H2SO4, anhydrous Na2SO4) followed by an alumina column separation in two fractions (first fraction containing PCDDs/PCDFs, and second containing only PCBs). The purified extract was then analyzed by GC/MS/MS. The newly developed approach in our lab was capable to reduce the overall time of sample preparation down to seven hours/per sample. Since the method shows good mean recoveries for all labelled congeners spiked in the samples (for PCDDs/PCDFs – 80-110%, for DL-PCBs – 70-85%), we assumed the absence of overestimation or underestimation in the analyzed samples.
VL  - 8
IS  - 1
ER  -

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Author Information

Ovanes Chakoyan

Department of Chromatography, Fidelitas Lab, Varna, Bulgaria

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Plain Text BibTeX RIS

APA Style

Ovanes Chakoyan. (2023). Rapid Determination of PCDDs, PCDFs and DL-PCBs in Foods, Feedingstuffs and Vegetable Oils Using New Modified Acid Silica. Chemical and Biomolecular Engineering, 8(1), 1-15. https://doi.org/10.11648/j.cbe.20230801.11

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ACS Style

Ovanes Chakoyan. Rapid Determination of PCDDs, PCDFs and DL-PCBs in Foods, Feedingstuffs and Vegetable Oils Using New Modified Acid Silica. Chem. Biomol. Eng. 2023, 8(1), 1-15. doi: 10.11648/j.cbe.20230801.11

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AMA Style

Ovanes Chakoyan. Rapid Determination of PCDDs, PCDFs and DL-PCBs in Foods, Feedingstuffs and Vegetable Oils Using New Modified Acid Silica. Chem Biomol Eng. 2023;8(1):1-15. doi: 10.11648/j.cbe.20230801.11

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@article{10.11648/j.cbe.20230801.11,
  author = {Ovanes Chakoyan},
  title = {Rapid Determination of PCDDs, PCDFs and DL-PCBs in Foods, Feedingstuffs and Vegetable Oils Using New Modified Acid Silica},
  journal = {Chemical and Biomolecular Engineering},
  volume = {8},
  number = {1},
  pages = {1-15},
  doi = {10.11648/j.cbe.20230801.11},
  url = {https://doi.org/10.11648/j.cbe.20230801.11},
  eprint = {https://article.sciencepublishinggroup.com/pdf/10.11648.j.cbe.20230801.11},
  abstract = {Polychlorinated dibenzo-p-dioxins, dibenzofurans and dioxin-like polychlorinated biphenyls are persistent organic pollutants (POPs), which in the recent years received huge attention due to their extreme stability, high potential toxicity and bioaccumulation in food chains. Main source of human exposure to these compounds is discovered in foods of animal origin, especially foods rich of fat. The target of the present study was to set up an analytical method for the determination of PCDDs/PCDFs and DL-PCB in vegetable oils, sunflower meals, sunflower seeds, rapeseeds and milk powder. The first step consisted of a semi-automatic Soxhlet extraction for 3 hours, by using a mixture of Hexane: Acetone - 80: 20, followed by acid digestion with 55% acid silica, and filtration. After concentration, the extract is purified on multilayer column (silica gel, silica-KOH, silica-H2SO4, anhydrous Na2SO4) followed by an alumina column separation in two fractions (first fraction containing PCDDs/PCDFs, and second containing only PCBs). The purified extract was then analyzed by GC/MS/MS. The newly developed approach in our lab was capable to reduce the overall time of sample preparation down to seven hours/per sample. Since the method shows good mean recoveries for all labelled congeners spiked in the samples (for PCDDs/PCDFs – 80-110%, for DL-PCBs – 70-85%), we assumed the absence of overestimation or underestimation in the analyzed samples.},
 year = {2023}
}

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TY  - JOUR
T1  - Rapid Determination of PCDDs, PCDFs and DL-PCBs in Foods, Feedingstuffs and Vegetable Oils Using New Modified Acid Silica
AU  - Ovanes Chakoyan
Y1  - 2023/06/09
PY  - 2023
N1  - https://doi.org/10.11648/j.cbe.20230801.11
DO  - 10.11648/j.cbe.20230801.11
T2  - Chemical and Biomolecular Engineering
JF  - Chemical and Biomolecular Engineering
JO  - Chemical and Biomolecular Engineering
SP  - 1
EP  - 15
PB  - Science Publishing Group
SN  - 2578-8884
UR  - https://doi.org/10.11648/j.cbe.20230801.11
AB  - Polychlorinated dibenzo-p-dioxins, dibenzofurans and dioxin-like polychlorinated biphenyls are persistent organic pollutants (POPs), which in the recent years received huge attention due to their extreme stability, high potential toxicity and bioaccumulation in food chains. Main source of human exposure to these compounds is discovered in foods of animal origin, especially foods rich of fat. The target of the present study was to set up an analytical method for the determination of PCDDs/PCDFs and DL-PCB in vegetable oils, sunflower meals, sunflower seeds, rapeseeds and milk powder. The first step consisted of a semi-automatic Soxhlet extraction for 3 hours, by using a mixture of Hexane: Acetone - 80: 20, followed by acid digestion with 55% acid silica, and filtration. After concentration, the extract is purified on multilayer column (silica gel, silica-KOH, silica-H2SO4, anhydrous Na2SO4) followed by an alumina column separation in two fractions (first fraction containing PCDDs/PCDFs, and second containing only PCBs). The purified extract was then analyzed by GC/MS/MS. The newly developed approach in our lab was capable to reduce the overall time of sample preparation down to seven hours/per sample. Since the method shows good mean recoveries for all labelled congeners spiked in the samples (for PCDDs/PCDFs – 80-110%, for DL-PCBs – 70-85%), we assumed the absence of overestimation or underestimation in the analyzed samples.
VL  - 8
IS  - 1
ER  -

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