Abstract
This study presents a highly sensitive and accurate analytical strategy for the determination of fenuron in wastewater samples using gas chromatography–mass spectrometry (GC-MS). Simultaneous derivatization and spray-based fine droplet formation–liquid phase microextraction (SFDF-LPME) method was developed and performed to achieve low detection limits. The parameters of the derivatization and SFDF-LPME method were optimized by univariate approach to improve sensitivity and selectivity. Under the optimum SFDF-LPME-GC-MS conditions, the limit of detection (LOD) and limit of quantitation (LOQ) were found to be 0.15 and 0.49 mg/kg, respectively. In addition, the linear range was calculated as 0.51–24.50 mg/kg. Recovery studies were carried out on wastewater samples to determine the accuracy of the developed method and its applicability to real sample matrix. Matrix matching calibration strategy was applied to eliminate/reduce any possible interference effects caused by the complexity of the wastewater matrix and to increase the accuracy of the analytical results. Percent recovery results varied between 85.9 and 120.9% with small percent relative standard deviation values. These results were satisfactory in terms of the accuracy and applicability of the proposed method for wastewater samples.
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References
Ali, I., Alharbi, O. M. L., ALOthman, Z. A., Al-Mohaimeed, A. M., & Alwarthan, A. (2019). Modeling of fenuron pesticide adsorption on CNTs for mechanistic insight and removal in water. Environmental Research, 170, 389–397. https://doi.org/10.1016/j.envres.2018.12.066
Baltussen, E., Snijders, H., Janssen, H.-G., Sandra, P., & Cramers, C. A. (1998). Determination of phenylurea herbicides in water samples using on-line sorptive preconcentration and high-performance liquid chromatography with UV or electrospray mass spectrometric detection. Journal of Chromatography A, 802(2), 285–295. https://doi.org/10.1016/S0021-9673(97)01182-5
Bosch Ojeda, C., & Sánchez Rojas, F. (2014). Vortex-assisted liquid–liquid microextraction (VALLME): Applications. Chromatographia, 77(11–12), 745–754. https://doi.org/10.1007/s10337-014-2669-x
Brahmia, O., Boulkamh, A., Sehili, T., Aguer, J.-P., & Richard, C. (2002). Kinetics of photocatalytic decomposition of Fenuron over TiO2 in aqueous solution. International Journal of Photoenergy, 4(2), 85–89. https://doi.org/10.1155/S1110662X02000132
Carabias-Martı́nez, R., Rodrı́guez-Gonzalo, E., Herrero-Hernández, E., & Hernández-Méndez, J. (2004). Simultaneous determination of phenyl- and sulfonylurea herbicides in water by solid-phase extraction and liquid chromatography with UV diode array or mass spectrometric detection. Analytica Chimica Acta, 517(1–2), 71–79. https://doi.org/10.1016/j.aca.2004.05.007
Chu, X.-G., Hu, X.-Z., & Yao, H.-Y. (2005). Determination of 266 pesticide residues in apple juice by matrix solid-phase dispersion and gas chromatography–mass selective detection. Journal of Chromatography A, 1063(1–2), 201–210. https://doi.org/10.1016/j.chroma.2004.12.003
de Pinho, G. P., Neves, A. A., de Queiroz, M. E. L. R., & Silvério, F. O. (2010). Optimization of the liquid–liquid extraction method and low temperature purification (LLE–LTP) for pesticide residue analysis in honey samples by gas chromatography. Food Control, 21(10), 1307–1311. https://doi.org/10.1016/j.foodcont.2010.03.006
Diaw, P. A., Maroto, A., Mbaye, O. M. A., Gaye-Seye, M. D., Stephan, L., Coly, A., et al. (2013). Determination of phenylurea pesticides by direct laser photo-induced fluorescence. Talanta, 116, 569–574. https://doi.org/10.1016/j.talanta.2013.07.014
Diaw, P. A., Mbaye, O. M. A., Thiaré, D. D., Oturan, N., Gaye-Seye, M. D., Coly, A., et al. (2019). Combination of photoinduced fluorescence and GC–MS for elucidating the photodegradation mechanisms of diflubenzuron and fenuron pesticides. Luminescence, 34(5), 465–471. https://doi.org/10.1002/bio.3612
Ferrer, C., Martínez-Bueno, M. J., Lozano, A., & Fernández-Alba, A. R. (2011). Pesticide residue analysis of fruit juices by LC–MS/MS direct injection. One year pilot survey. Talanta, 83(5), 1552–1561. https://doi.org/10.1016/j.talanta.2010.11.061
Gatidou, G., Stasinakis, A. S., & Iatrou, E. I. (2015). Assessing single and joint toxicity of three phenylurea herbicides using Lemna minor and Vibrio fischeri bioassays. Chemosphere, 119, S69–S74. https://doi.org/10.1016/j.chemosphere.2014.04.030
Gennaro, M. C., Marengo, E., Gianotti, V., & Maurino, V. (2001). New strategies for the determination of phenylurea pesticides by gas chromatography with hot splitless inlet systems. Journal of Chromatography A, 910(1), 79–86. https://doi.org/10.1016/S0021-9673(00)01182-1
Hayat, W., Liu, Z., Wan, Y., & Zhang, Y. (2022). The analysis of efficiency of activated peroxymonosulfate for fenuron degradation in water. Environmental Technology & Innovation, 26, 102352. https://doi.org/10.1016/j.eti.2022.102352
Hong, K., Huang, Y., Zheng, L., Zheng, X., & Huang, X. (2022). One-pot fabrication of poly (ionic liquid)s functionalized magnetic adsorbent for efficient enrichment of phenylurea herbicides in environmental waters. Analytica Chimica Acta, 1198, 339549. https://doi.org/10.1016/j.aca.2022.339549
Islam, M. A., Amin, S. M. N., Rahman, M. A., Juraimi, A. S., Uddin, M. K., Brown, C. L., & Arshad, A. (2022). Chronic effects of organic pesticides on the aquatic environment and human health: A review. Environmental Nanotechnology, Monitoring & Management, 18, 100740. https://doi.org/10.1016/j.enmm.2022.100740
Jiang, H., Qin, Y., & Hu, B. (2008). Dispersive liquid phase microextraction (DLPME) combined with graphite furnace atomic absorption spectrometry (GFAAS) for determination of trace Co and Ni in environmental water and rice samples. Talanta, 74(5), 1160–1165. https://doi.org/10.1016/j.talanta.2007.08.022
Langeron, J., Sayen, S., Couderchet, M., & Guillon, E. (2014). Leaching potential of phenylurea herbicides in a calcareous soil: Comparison of column elution and batch studies. Environmental Science and Pollution Research International, 21(7), 4906–4913. https://doi.org/10.1007/s11356-012-1244-y
Mani, V., Devasenathipathy, R., Chen, S.-M., Wu, T.-Y., & Kohilarani, K. (2015). High-performance electrochemical amperometric sensors for the sensitive determination of phenyl urea herbicides diuron and fenuron. Ionics, 21(9), 2675–2683. https://doi.org/10.1007/s11581-015-1459-2
Mou, R.-X., Chen, M.-X., & Zhi, J.-L. (2008). Simultaneous determination of 15 phenylurea herbicides in rice and corn using HPLC with fluorescence detection combined with UV decomposition and post-column derivatization. Journal of Chromatography B, 875(2), 437–443. https://doi.org/10.1016/J.JCHROMB.2008.09.022
Oflu, S., Erarpat, S., Zaman, B. T., Günkara, Ö. T., Bakırdere, S., & Turak, F. (2023). Combination of quadrupole isotope dilution mass spectrometry with simultaneous derivatization and spray assisted droplet formation-liquid phase microextraction for the determination of methamphetamine in human urine and serum samples by gas chromatography. Journal of Pharmacological and Toxicological Methods, 119, 107207. https://doi.org/10.1016/j.vascn.2022.107207
Orazbayeva, D., Muratuly, A., Bektassov, M., Zhakupbekova, A., & Kenessov, B. (2022). Chromatographic determination of pesticides in soil: Current trends in analysis and sample preparation. Trends in Environmental Analytical Chemistry, 35, e00174. https://doi.org/10.1016/j.teac.2022.e00174
Oturan, M. A., Edelahi, M. C., Oturan, N., El kacemi, K., & Aaron, J.-J. (2010). Kinetics of oxidative degradation/mineralization pathways of the phenylurea herbicides diuron, monuron and fenuron in water during application of the electro-Fenton process. Applied Catalysis B: Environmental, 97(1), 82–89. https://doi.org/10.1016/j.apcatb.2010.03.026
Öztürk Er, E., Erarpat, S., Bodur, S., Günkara, Ö. T., Özbek, B., & Bakırdere, S. (2022). Accurate determination of amino acids by quadruple isotope dilution-reverse phase liquid chromatography-tandem mass spectrometry after derivatization with 2-naphthoyl chloride. Journal of Chromatography A, 462870. https://doi.org/10.1016/j.chroma.2022.462870
Panis, C., Candiotto, L. Z. P., Gaboardi, S. C., Gurzenda, S., Cruz, J., Castro, M., & Lemos, B. (2022). Widespread pesticide contamination of drinking water and impact on cancer risk in Brazil. Environment International, 165, 107321. https://doi.org/10.1016/j.envint.2022.107321
Peña, F. (2002). Analysis of phenylurea herbicides from plants by GC/MS. Talanta, 56(4), 727–734. https://doi.org/10.1016/S0039-9140(01)00616-6
Pimentel, D. (1995). Amounts of pesticides reaching target pests: Environmental impacts and ethics. Journal of Agricultural and Environmental Ethics, 8(1), 17–29. https://doi.org/10.1007/BF02286399
Rezaee, M., Yamini, Y., Khanchi, A., Faraji, M., & Saleh, A. (2010). A simple and rapid new dispersive liquid–liquid microextraction based on solidification of floating organic drop combined with inductively coupled plasma-optical emission spectrometry for preconcentration and determination of aluminium in water samples. Journal of Hazardous Materials, 178(1–3), 766–770. https://doi.org/10.1016/j.jhazmat.2010.02.006
Segura, J., Ventura, R., & Jurado, C. (1998). Derivatization procedures for gas chromatographic–mass spectrometric determination of xenobiotics in biological samples, with special attention to drugs of abuse and doping agents. Journal of Chromatography B: Biomedical Sciences and Applications, 713(1), 61–90. https://doi.org/10.1016/S0378-4347(98)00089-9
Soylak, M., & Uzcan, F. (2020). A novel ultrasonication-assisted deep eutectic solvent microextraction procedure for tartrazine at trace levels from environmental samples. Journal of the Iranian Chemical Society, 17(2), 461–467. https://doi.org/10.1007/s13738-019-01781-5
Tran, K., Eide, D., Nickols, S. M., Cromer, M. R., Sabaa-Srur, A., & Smith, R. E. (2012). Finding of pesticides in fashionable fruit juices by LC–MS/MS and GC–MS/MS. Food Chemistry, 134(4), 2398–2405. https://doi.org/10.1016/j.foodchem.2012.04.034
Trocewicz, J. (1996). Determination of herbicides in surface water by means of a supported liquid membrane technique and high-performance liquid chromatography. Journal of Chromatography A, 725(1), 121–127. https://doi.org/10.1016/0021-9673(95)01031-9
Turkish, G. M.. (2005). İnsani Tüketim Amaçlı Sular Hakkında Yönetmelik. Retrieved June 26, 2023, from https://www.mevzuat.gov.tr/mevzuat?MevzuatNo=7510&MevzuatTur=7&MevzuatTertip=5
Wang, Q.-Y., Yang, J., Dong, X., Chen, Y., Ye, L.-H., Hu, Y.-H., et al. (2020). Zirconium metal-organic framework assisted miniaturized solid phase extraction of phenylurea herbicides in natural products by ultra-high-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry. Journal of Pharmaceutical and Biomedical Analysis, 180, 113071. https://doi.org/10.1016/j.jpba.2019.113071
Woźniak, M. K., Wiergowski, M., Aszyk, J., Kubica, P., Namieśnik, J., & Biziuk, M. (2018). Application of gas chromatography–tandem mass spectrometry for the determination of amphetamine-type stimulants in blood and urine. Journal of Pharmaceutical and Biomedical Analysis, 148, 58–64. https://doi.org/10.1016/j.jpba.2017.09.020
Wu, Q., Wang, C., Liu, Z., Wu, C., Zeng, X., Wen, J., & Wang, Z. (2009). Dispersive solid-phase extraction followed by dispersive liquid–liquid microextraction for the determination of some sulfonylurea herbicides in soil by high-performance liquid chromatography. Journal of Chromatography A, 1216(29), 5504–5510. https://doi.org/10.1016/j.chroma.2009.05.062
Yang, E.-Y., & Shin, H.-S. (2013). Trace level determinations of carbamate pesticides in surface water by gas chromatography–mass spectrometry after derivatization with 9-xanthydrol. Journal of Chromatography A, 1305, 328–332. https://doi.org/10.1016/j.chroma.2013.07.055
Yang, X., Zhang, H., Liu, Y., Wang, J., Zhang, Y. C., Dong, A. J., et al. (2011). Multiresidue method for determination of 88 pesticides in berry fruits using solid-phase extraction and gas chromatography–mass spectrometry: Determination of 88 pesticides in berries using SPE and GC–MS. Food Chemistry, 127(2), 855–865. https://doi.org/10.1016/j.foodchem.2011.01.024
Zgoła-Grześkowiak, A., & Grześkowiak, T. (2011). Dispersive liquid-liquid microextraction. TrAC Trends in Analytical Chemistry, 30(9), 1382–1399. https://doi.org/10.1016/j.trac.2011.04.014
Authors contribution
Sude Oflu: data curation, formal analysis, investigation, methodology, validation, visualization, writing—original draft. Sezin Erarpat: data curation, formal analysis, methodology, validation, visualization, writing—original draft. Buse Tuğba Zaman: data curation, formal analysis, methodology, validation, visualization, writing—original draft. Kumsal Eroğlu: data curation, formal analysis, investigation, methodology, writing—original draft. Ömer Tahir Günkara: data curation, formal analysis, investigation, methodology, validation, writing—original draft. Sezgin Bakırdere: conceptualization, data curation, investigation, methodology, supervision, validation, writing—review and editing. Fatma Turak: conceptualization, data curation, investigation, methodology, supervision, validation, writing—original draft.
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Oflu, S., Erarpat, S., Zaman, B.T. et al. Quantification of trace fenuron in waste water samples by matrix matching calibration strategy and gas chromatography–mass spectrometry after simultaneous derivatization and preconcentration. Environ Monit Assess 195, 1063 (2023). https://doi.org/10.1007/s10661-023-11575-1
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DOI: https://doi.org/10.1007/s10661-023-11575-1