Development of a Method for the Analysis of Polycyclic Aromatic Hydrocarbons Using FMS-TTP-SPE Pretreatment System: Application to Water Samples of Gölcük Lake in Isparta Province

Abstract

It is known that the carcinogenic effects of Polycyclic Aromatic Hydrocarbon (PAH) compounds are high. Therefore, accurate determination of PAH concentrations in water is an important research topic. Since PAHs have low solubility values in water (nanogram/liter), sensitive analytical techniques and sample pretreatment systems are required in order to determine the low levels of PAH compounds in water samples. One of these techniques is the extraction of PAHs from environmental water samples using the Fluid Management Systems- Turbo Trace Parallel-Solid Phase Extraction (FMS-TTP-SPE) pretreatment system. In this study, a chromatographic analysis and extraction method was validated and adopted for the extraction of 11 PAH compounds in water samples using the FMS-TTP-SPE pretreatment system and a gas chromatography equipped with a flame ionization detector (GC-FID). From the results, the LOD values were calculated between 6.5 and 13.7, and the LOQ values between 21.6 and 45.6 µg L-1. Recovery (R) results were changed between 85.0% and 97.0%. Concerning the proposed method, it has been shown that high concentrations of PAHs can be obtained in a single extraction procedure compared to conventional approaches. Using the developed method, twelve surface lake water samples were collected in April 2022 from Gölcük lake which is a volcanic lake. Eleven PAH compounds were investigated in the lake water samples using the proposed method.

Keywords

• PAH
• FMS Turbo Trace Paralel SPE System
• GC-FID
• Method Validation

FMS-TTP-SPE Ön Hazırlık Sistemi Kullanılarak Polisiklik Aromatik Hidrokarbonların Analizi için Yöntem Geliştirilmesi: Yöntemin Isparta İli Gölcük Gölünden Alınan Su Numunelerine Uygulanması

Abstract

Polisiklik Aromatik Hidrokarbon (PAH) bileşiklerinin kanserojen etkilerinin yüksek olduğu bilinmektedir. PAH’ların sulardaki çözünürlük değerlerinin düşük (nanogram/litre) olması nedeni ile PAH tayini ön hazırlık işlemlerinin doğru yapılması ve farklı analitik cihazlar ile düşük konsantrasyonlardaki tespitlerinin belirlenmesi için hassas analitik teknikler gereklidir. Bu tekniklerden bir tanesi de Akışkan Yönetim Sistemleri- Turbo Trace Paralel- Katı Faz Ekstraksiyonu (Fluid Management Systems - Turbo Trace Parallel - Solid Phase Extraction, FMS-TTP-SPE) ön hazırlık sistemi kullanılarak çevresel su numunelerinden PAH'ların ekstraksiyonudur. Bu çalışmada, FMS-TTP-SPE ön hazırlık sistemi kullanarak su numunelerinde bulunan 11 adet PAH bileşiğinin ekstraksiyonu ve sonrasında konsantrasyonlarının gaz kromatografi cihazında (GC-FID) belirlenmesi için kromatografik analiz ve ekstraksiyon metodu valide edilmiştir. Gaz kromatografisi ile konsantrasyon belirleme çalışmalarının doğrulama parametreleri için elde edilen sonuçlardan LOD değerleri 6,48 ile 13,69 arasında, LOQ değerleri ise 21,60 ile 45,62 µg L-1 arasında hesaplanmıştır. Geri kazanım (GK) testleri ise %85,0 ile %97,0 arasında tespit edilmiştir. Önerilen yöntem ile, geleneksel yaklaşımlara kıyasla tek bir ekstraksiyon prosedüründe çok düşük PAH konsantrasyonlarının tespit edilebildiği gösterilmiştir. Geliştirilen metot kullanılarak; 2022 yılı Nisan ayı içerisinde, volkanik göl olan Gölcük gölünden on iki adet göl suyu örneği toplanmış ve PAH’ların konsantrasyon tespit çalışmaları yapılmıştır.

Keywords

• PAH
• FMS Turbo Trace Paralel SPE Sistem
• GC-FID
• Metot Validasyon

References

1. European Environment Agency, Environment and health, [Online]. Available: https://www.eea.europa.eu/publications/eea_report_2005_10
2. L. H. Keith, “The Source of U.S. EPA's Sixteen PAH Priority Pollutants,” Polycycl. Aromat. Compd., 35, 2015.
3. G. L. Brun, O. M. C. Vaidya, M. G. Leger, “Atmospheric deposition of polycyclic aromatic hydrocarbons Atlantic Canada: geographic and temporal distributions and trends 1980–2001,” Environ. Sci. Technol., 38, 1941–1948, 2004
4. E. Manoli, C. Samara, I. Konstantinou, T. Albanis, “Polycyclic aromatic hydrocarbons in the bulk precipitation and surface waters of Northern Greece,” Chemosphere, 41, 1845–1855, 2000.
5. D. Golomb, D. Ryan, J. Underhill, T. Wade, S. Zemba, “Atmospheric deposition of toxics onto Massachusetts Bay—II. Polycyclic aromatic hydrocarbons. Polycyclic aromatic hydrocarbons,” Atmos. Environ., 31, 1361–1368, 1997.
6. United States Environmental Protection Agency, Priority Pollutant List, [Online]. Available: https://www.epa.gov/sites/default/files/2015-09/documents/priority-pollutant-list-epa.pdf
7. T. M. Gutierrez-Valencia, M. P. Garcia de Llasera, “On-line MSPD-SPE-HPLC/FLD analysis of polycyclic aromatic hydrocarbons in bovine tissues,” Food Chem., 223, 82–88, 2017.
8. D. R. D. Molle, C. Abballe, F. M. L. Gomes, R. P. Z. Furlani, S. A. V. Tfouni, “Polycyclic aromatic hydrocarbons in canola, sunflower and corn oils and estimated daily intake,” Food Control, 81, 96–100, 2017.

9. M. Pogorzelec, K. Piekarska, “Application of semipermeable membrane devices for long-term monitoring of polycyclic aromatic hydrocarbons at various stages of drinking water treatment,” Sci. Total Environ., 631-632, 1431–1439, 2018.
10. C. Cavaliere, C. M. Montone, A. L. Capriotti, G. L. Barbera, S. Piovesana, M. Rotatori, F. Valentino, A. Lagana, “Extraction of polycyclic aromatic hydrocarbons from polyhydroxyalkanoates before gas chromatography/mass spectrometry analysis,” Talanta, 188, 671–675, 2018.
11. S. Ncube, L. Madikizela, E. Cukrowska, L. Chimuka, “Recent advances in the adsorbents for isolation of polycyclic aromatic hydrocarbons (PAHs) from environmental sample solutions,” TrAC Trends in Anal. Chem., 99, 101–116, 2018.
12. Y. Chen, B. Lai, Y. Wei, Q. Ma, H. Liang, H. Yang, R. Ye, M. Zeng, H. Wang, Y. Wu, X. Liu, L. Guo, H. Tang, “Polluting characteristics, sources, cancer risk, and cellular toxicity of PAHs bound in atmospheric particulates sampled from an economic transformation demonstration area of Dongguan in the Pearl River Delta, China,” Environ. Res., 215(2), 2022.
13. S-C. C. Lung, C-H. Liu, “Fast analysis of 29 polycyclic aromatic hydrocarbons (PAHs) and nitro-PAHs with ultra-high performance liquid chromatography-atmospheric pressure photoionization-tandem mass spectrometry,” Sci. Rep., 5, 2015.
14. M. N. Yazdi, Y. Yamini, H. Asiabi, “Multiwall carbon nanotube- zirconium oxide nanocomposite hollow fiber solid phase microextraction for determination of polyaromatic hydrocarbons in water, coffee and tea samples,” J. Chromatogr. A, 1554, 8–15, 2018.
15. G. M. Chapman, R. Bravo, R.D. Stanelle, C.H. Watson, L. Valentin-Blasini, “Sensitive and selective gas chromatography-tandem mass spectrometry method for the detection of nitrobenzene in tobacco smoke,” J. Chromatogr. A, 1565, 124–129, 2018.
16. O. Geiss, C. Senaldi, I. Bianchi, A. Lucena, S. Tirendi, J. Barrero-Moreno, “A fast and selective method for the determination of 8 carcinogenic polycyclic aromatic hydrocarbons in rubber and plastic materials,” J. Chromatogr. A, 1566, 13–22, 2018.
17. G. Trouvé, C. Ngo, W. Almouallem, C. Joyeux, S. Dorge, J. Michel & D. Le Nouen, “Development of a Liquid/Liquid Extraction Method and GC/MS Analysis Dedicated to the Quantitative Analysis of PAHs and O-PACs in Groundwater from Contaminated Sites and Soils,” Polycycl. Aromat. Comp., 42(7), 4000–4018, 2022.
18. H. Vistnes, N. A. Sossalla, A. Røsvik, S. V. Gonzalez, J. Zhang, T. Meyn and A. G. Asimakopoulos, “The Determination of Polycyclic Aromatic Hydrocarbons (PAHs) with HPLC-DAD-FLD and GC-MS Techniques in the Dissolved and Particulate Phase of Road-Tunnel Wash Water: A Case Study for Cross-Array Comparisons and Applications,” toxics, 10, 399, 2022.
19. Z. Li, M. Yang, X. Shen, H. Zhu and B. Li, “The Preparation of Covalent Bonding COF-TpBD Coating in Arrayed Nanopores of Stainless Steel Fiber for Solid-Phase Microextraction of Polycyclic Aromatic Hydrocarbons in Water,” Int. J. Environ. Res. Public Health, 20, 1393, 2023.
20. N. Manousi, G. A. Zachariadis, “Recent advances in the extraction of polycyclic aromatic hydrocarbons from environmental samples,” Molecules, 25, 9, 2020.
21. C. L. Arthur, J. Pawliszyn, “Solid phase microextraction with thermal desorption using fused silica optical fibers,” Anal. Chem., 62 (19), 2145-2148, 1990.
22. J. Płotka-Wasylka, K. Owczarek, J. Namie_snik, “Modern solutions in the field of microextraction using liquid as a medium of extraction,” TrAC Trends Anal. Chem., 85, 46–64, 2016.
23. M. Rezaee, Y. Assadi, M.-R. Milani Hosseini, E. Aghaee, F. Ahmadi, S. Berijani, “Determination of organic compounds in water using dispersive liquid-liquid microextraction,” J. Chromatogr. A, 1116, 1-2, 1-9, 2006.
24. A. Sarafraz-Yazdi ve A. Amiri, “Liquid-phase microextraction,” TrAC Trends Anal. Chem., 29, 1-14, 2010.
25. S. Tang, G. H. Chia, Y. Chang, H. K. Lee, “Automated dispersive solid-phase extraction using dissolvable Fe3O4 -layered double hydroxide core-shell microspheres as sorbent,” Anal. Chem. 86 (22), 11070–11076, 2014.
26. D. A. Wells, T. L. Lloyd, “Chapter 24 automation of sample preparation for pharmaceutical and clinical analysis,” Comprehensive Analytical Chemistry, 37, 837–868, 2002.
27. Application note, Polycyclic Aromatic Hydrocarbons in Drinking Water by Solid Phase Extraction (SPE) with EPA 550.1, [Online]. Available: https://www.epa.gov/sites/default/files/2015-09/documents/priority-pollutant-list-epa.pdf https://fms-inc.com/wp-content/uploads/2020/05/EPA-550.1-Polycylic-Aromatic-Hydrocarbons-in-Drinking-Water-by-TurboTrace.pdf
28. S. Kılıç, S. Yenisoy-Karakaş, M. Kılıç, “Metal Contamination in Fruit Juices in Turkey: Method Validation and Uncertainty Budget,” Food Anal. Methods, 8, 2487–2495, 2015.