Abstract
This study presents the development of a sensitive and accurate dispersive liquid-liquid microextraction method using binary solvents for the simultaneous determination of endocrine disruptive compounds by GC-MS. Optimum binary solvent and dispersive solvent amounts were determined using an experimental design. The main effects of these parameters and their interaction effects were assessed using analysis of variance. The detection limits of the analytes under optimal experimental conditions ranged between 0.16–1.5 ng/mL. All analytes exhibited good linearity over broad calibration ranges, and high precision (%RSD < 8.0%) was obtained for six repeated readings of the lowest concentrations of the calibration plots. The method’s applicability and accuracy were tested on two municipal wastewater samples spiked at 10, 50, and 100 ng/mL. The recovery results obtained ranged between 82 and 108%, indicating that the method can be used to quantify the analytes in wastewater matrix with substantial accuracy. In addition, matrix matching calibration method was used to improve the percent recovery (≈ 100%) for a waste sludge sample spiked at 50 ng/mL.
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Aktar, M. W., Sengupta, D., & Chowdhury, A. (2009). Impact of pesticides use in agriculture: their benefits and hazards. Interdisciplinary Toxicology, 2, 1–12.
Bulgurcuoğlu, A. E., Yılmaz, B., Chormey, D. S., & Bakırdere, S. (2018). Simultaneous determination of estrone and selected pesticides in water medium by GC-MS after multivariate optimization of microextraction strategy. Environmental Monitoring and Assessment, 190(4), 252.
Chen, M.-L., Chen, J.-H., Ding, L., Xu, Z., Wen, L., Wang, L.-B., & Cheng, Y.-H. (2017). Study of the detection of bisphenol A based on a nano-sized metal-organic framework crystal and an aptamer. Analytical Methods, 9, 906–909.
Correia-Sá, L., Norberto, S., Delerue-Matos, C., Calhau, C., & Domingues, V. F. (2018). Micro-QuEChERS extraction coupled to GC–MS for a fast determination of bisphenol a in human urine. Journal of Chromatography B, 1072, 9–16.
Estevão, P. L. S., Peralta-Zamora, P., & Nagata, N. (2018). Binary solvent dispersive liquid-liquid microextraction for the determination of pesticides in natural water samples. Journal of the Brazilian Chemical Society, 29, 2104–2116.
Fortes, S. S., Barth, T., Furtado, N. A. J. C., Pupo, M. T., de Gaitani, C. M., & de Oliveira, A. R. M. (2013). Evaluation of dispersive liquid–liquid microextraction in the stereoselective determination of cetirizine following the fungal biotransformation of hydroxyzine and analysis by capillary electrophoresis. Talanta, 116, 743–752.
Geissen, V., Mol, H., Klumpp, E., Umlauf, G., Nadal, M., van der Ploeg, M., van de Zee, S. E. A. T. M., & Ritsema, C. J. (2015). Emerging pollutants in the environment: a challenge for water resource management. International Soil and Water Conservation Research, 3, 57–65.
Genuis, S. J., Beesoon, S., Birkholz, D., & Lobo, R. A. (2012). Human excretion of bisphenol a: blood, urine, and sweat (BUS) study. Journal of Environmental and Public Health, 2012, 10.
George, M. J., Tagwa, O. R., & Sichilongo, K. F. (2017). Extraction and pre-concentration of phthalic acid esters from aqueous solutions using agitation-assisted dispersed binary solvents microextraction. South African Journal of Chemistry, 70, 100–107.
Gondo, T. T., Obuseng, V. C., Mmualefe, L. C., & Okatch, H. (2016). Employing solid phase microextraction as extraction tool for pesticide residues in traditional medicinal plants. Journal of Analytical Methods in Chemistry, 2016, 2890219.
Jarman, W. M., & Ballschmiter, K. (2012). From coal to DDT: the history of the development of the pesticide DDT from synthetic dyes till Silent Spring. Endeavour, 36, 131–142.
Jayaraj, R., Megha, P., & Sreedev, P. (2016). Organochlorine pesticides, their toxic effects on living organisms and their fate in the environment. Interdisciplinary Toxicology, 9, 90–100.
Kelly, B. C., Ikonomou, M. G., Blair, J. D., Morin, A. E., & Gobas, F. A. (2007). Food web-specific biomagnification of persistent organic pollutants. Science, 317, 236–239.
Kwon, H., Lehotay, S. J., & Geis-Asteggiante, L. (2012). Variability of matrix effects in liquid and gas chromatography–mass spectrometry analysis of pesticide residues after QuEChERS sample preparation of different food crops. Journal of Chromatography. A, 1270, 235–245.
Lee, Y. M., Kim, K. S., Jacobs, D. R., & Lee, D. H. (2017). Persistent organic pollutants in adipose tissue should be considered in obesity research. Obesity Reviews, 18, 129–139.
Li, Y., Zhang, W., Wang, R.-G., Wang, P.-L., & Su, X.-O. (2015). Development of a efficient and sensitive dispersive liquid–liquid microextraction technique for extraction and preconcentration of 10 β(2)-agonists in animal urine. PLoS One, 10(9), e0137194.
Lynch, K. L. (2017). Chapter 6 - toxicology: liquid chromatography mass spectrometry. In H. Nair & W. Clarke (Eds.), Mass spectrometry for the clinical laboratory (pp. 109–130). San Diego: Academic.
Maham, M., Karami-Osboo, R., Kiarostami, V., & Waqif-Husain, S. (2013). Novel binary solvents-dispersive liquid-liquid microextraction (BS-DLLME) method for determination of patulin in apple juice using high-performance liquid chromatography. Food Analytical Methods, 6, 761–766.
Motomizu, S., & Sakai, T. (2008). Chapter 7 - on-line sample pretreatment: extraction and Preconcentration. In S. D. Kolev & I. D. McKelvie (Eds.), Comprehensive Analytical Chemistry (Vol. 54, pp. 159–201). Amsterdam: Elsevier.
Pleština, R. (2003). Pesticides and herbicides – types of pesticide. In L. Trugo & P. M. Finglas (Eds.), Encyclopedia of Food Sciences and Nutrition (pp. 4473–4483). Oxford: Academic.
Pojana, G., Gomiero, A., Jonkers, N., & Marcomini, A. (2007). Natural and synthetic endocrine disrupting compounds (EDCs) in water, sediment and biota of a coastal lagoon. Environment International, 33, 929–936.
Priac, A., Morin-Crini, N., Druart, C., Gavoille, S., Bradu, C., Lagarrigue, C., Torri, G., Winterton, P., & Crini, G. (2017). Alkylphenol and alkylphenol polyethoxylates in water and wastewater: a review of options for their elimination. Arabian Journal of Chemistry, 10, S3749–S3773.
Rezaee, M., Assadi, Y., Milani Hosseini, M.-R., Aghaee, E., Ahmadi, F., & Berijani, S. (2006). Determination of organic compounds in water using dispersive liquid–liquid microextraction. Journal of Chromatography A, 1116, 1–9.
Salgueiro-González, N., Muniategui-Lorenzo, S., López-Mahía, P., & Prada-Rodríguez, D. (2017). Trends in analytical methodologies for the determination of alkylphenols and bisphenol A in water samples. Analytica Chimica Acta, 962, 1–14.
Schug, T. T., Janesick, A., Blumberg, B., & Heindel, J. J. (2011). Endocrine disrupting chemicals and disease susceptibility. The Journal of Steroid Biochemistry and Molecular Biology, 127, 204–215.
Sung, Y.-H., Liu, C.-H., Leong, M.-I., & Huang, S.-D. (2014). Determination of alkylphenols in water by dispersive liquid–liquid microextraction based on solid formation without a disperser. Analytical Letters, 47(16), 2643–2654.
Willingham, E. (2004). Endocrine-disrupting compounds and mixtures: unexpected dose–response. Archives of Environmental Contamination and Toxicology, 46(2), 265–269.
Yang, X., Chen, X., Hu, S., & Bai, X.-h. (2018). In-syringe binary-solvent liquid-phase microextraction for the preconcentration of cinnamic acid derivatives in traditional Chinese medicine samples. Chromatographia 2018, 81, 257–264.
Zhu, J., Wang, Q., Li, M., Ren, L., Zheng, B., & Zou, X. (2018). Binary mixed solvent-based solvent demulsification-dispersive liquid-liquid microextraction coupled with gas chromatography-tandem mass spectrometry in determination of polycyclic aromatic hydrocarbons in water samples. Analytical Methods, 9, 1855–1863.
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Chormey, D.S., Fırat, M. & Bakırdere, S. Multivariate Optimization of Binary Solvent Microextraction for the Simultaneous Determination of Endocrine Disruptive Phenolic Compounds and Organochlorine Pesticides in Wastewater and Sludge Samples by GC-MS. Water Air Soil Pollut 229, 370 (2018). https://doi.org/10.1007/s11270-018-4024-6
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DOI: https://doi.org/10.1007/s11270-018-4024-6