HPLC-FLD determination of 4-nonylphenol and 4-tert-octylphenol in surface water samples
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Abstract
A simple, sensitive and reliable HPLC-FLD method for the routine determination of 4-nonylphenol, 4-NP and 4-tert-octylphenol, 4-t-OP content in water samples was developed. The method consists in a liquid–liquid extraction of the target analytes with dichloromethane at pH 3.0–3.5 followed by the HPLC-FLD analysis of the organic extract using a Zorbax Eclipse XDB C8 column, isocratic elution with a mixed solvent acetonitrile/water 65:35, at a flow rate of 1.0 mL/min and applying a column temperature of 40°C. The method was validated and then applied with good results for the determination of 4-NP and 4-t-OP in Ialomiţa River water samples collected each month during 2006. The concentration levels of 4-NP and 4-t-OP vary between 0.08–0.17 μg/L with higher values of 0.24–0.37 μg/L in the summer months for 4-NP, and frequently <0.05 μg/L but also between 0.06–0.09 μg/L with higher values of 0.12–0.16 μg/L in July and August for 4-t-OP and were strongly influenced by sesonial and anthropic factors. The method was also applied on samples collected over 2 years 2007 and 2008 from urban wastewaters discharged into sewage or directly into the rivers by economic agents located in 30 Romanian towns. Good results were obtained when the method was used for analysis of effluents discharged into surface waters by 16 municipal wastewater treatment plants, during the year 2008.
Keywords
4-Nonylphenol 4-tert-octylphenol LLE HPLC-FLD Surface waterPreview
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References
- Babay, P., Gettar, R., Magallanes, H., Becquart, E., Thiele, B., & Batistoni, D. (2007). Column temperature as an active variable in the isocratic, normal-phase high-performance liquid chromatography separation of lipophilic metabolites of nonylphenol ethoxylates. Journal of Chromatography. A, 1157, 227–236.CrossRefGoogle Scholar
- Basheer, C., & Lee, H. K. (2004). Analysis of endocrine disrupting alkylphenols, chlorophenols and bisphenol-A using hollow fiber-protected liquid-phase microextraction coupled with injection port-derivatization gas chromatography–mass spectrometry. Journal of Chromatography. A, 1057, 163–169.CrossRefGoogle Scholar
- Basheer, C., Parthiban, A., Jayaraman, A., Lee, H. K., & Valiyavee, S. (2005). Determination of alkylphenols and bisphenol-A. A comparative investigation of functional polymer-coated membrane microextraction and solid-phase microextraction techniques. Journal of Chromatography A, 1087, 274–282.CrossRefGoogle Scholar
- Baugros, J.-B., Giroud, B., Dessalces, G., Grenier-Loustalot, M.-F., & Cren-Olive, C. (2008). Multiresidue analytical methods for the ultra-trace quqntification of 33 priority substances present in the list of REACH in real water samples. Analytica Chimica Acta, 607, 191–203.CrossRefGoogle Scholar
- Brix, R., Postigo, C., González, S., Villagrasa, M., Navarro, A., Kuster, M., et al. (2010). Analysis and occurrence of alkylphenolic compoundsand estrogens in a European river basin and an evaluationof their importance as priority pollutants. Analytical and Bioanalytical Chemistry, 396, 1301–1309.CrossRefGoogle Scholar
- Cantero, M., Rubio, S., & Perez-Bendito, D. (2006). Determination of alkylphenols and alkylphenol carboxylates in wastewater and river samples by hemimicelle-based extraction and liquid chromatography–ion trap mass spectrometry. Journal of Chromatography. A, 1120, 260–267.CrossRefGoogle Scholar
- Cespedes, R., Lacorte, S., Ginegreda, A., & Barcelo, D. (2008). Occurence and fate of alkylphenols and alkylphenol ethoxylates in sewage treatment plants and impact on receiving waters along the Ter River (Catalonia, NE Spain). Environmental Pollution, 153, 384–392.CrossRefGoogle Scholar
- Cheng, Ch.-Y., Wu, Ch.-Y., Wang, Ch.-H., & Ding, W.-H. (2006). Determination and distribution characteristics of degradation products of nonylphenol polyethoxylates in the rivers of Taiwan. Chemosphere, 65, 2275–2281.CrossRefGoogle Scholar
- Cruceru, I., Vladescu, L., & Badea, I. (2007). Combined cation exchange – Liquid-liquid extraction method for GC-MS determination of 4-nonylphenol content in water. Revista de Chimie (Bucuresti), 58(12), 1305–1309.Google Scholar
- EC (2000). Directive 2000/60/EC of the European Parliament and of the council establishing a framework for community action in the field of water policy. Official Journal of the European Communities L327 (22 December 2000 European Communities, Brussels).Google Scholar
- EC (2003). European directive 2003/53/EC of the European Parliament and of the Council of 18 June 2003 amending for the 26th time council directive 76/769/EEC relating to restrictions on the marketing and use of certain dangerous substances and preparations (nonylphenol, nonylphenol ethoxylate and cement). Official Journal of the European Communities, Brussels.Google Scholar
- Fu, M., Li, Z., & Gao, H. (2007). Distribution characteristics of nonylphenol in Jiaozhou Bay of Qingdao and its adjacent rivers. Chemosphere, 69, 1009–1016.CrossRefGoogle Scholar
- Furuichi, T., Kannan, K., Giesy, J. P., & Masunaga, S. (2004). Contribution of known endocrine disrupting substances to the estrogenic activity in Tama River water samples from Japan using instrumental analysis and in vitro reporter gene assay. Water Research, 38, 4491–4501.CrossRefGoogle Scholar
- Gadzała-Kopciuch, R., Filipiak, A., & Buszewski, B. (2008). Isolation, purification and determination of 4-n-nonylphenol and 4-tert-octylphenol in aqueous and biological samples. Talanta, 74, 655–660.CrossRefGoogle Scholar
- Hao, R.-X., Zhou, Y.-W., Cheng, S.-Y., Li, J.-B., Zhao, M., Chen, X., et al. (2008). The accumulation on nonylphenol in a wastewater recycling process. Chemosphere, 70, 783–790.CrossRefGoogle Scholar
- HG (2005). Government decision on approval of the programme to phase out discharges, emissions and losses of priority hazardous substances. Monitorul Oficial nr. 428, 2005, Bucharest.Google Scholar
- Hoai, P. M., Tsunoi, S., Ike, M., Sei, K., Lu, X., Tanaka, M., et al. (2006). Dicarboxylic degradation products of nonylphenol polyethoxylates. Determination and structural elucidation in water samples by solid-phase extraction and gas chromatography–mass spectrometry after methylation. Journal of Chromatography. A, 1103, 125–132.CrossRefGoogle Scholar
- ISO (1992). Water quality – Sampling – Part 10: Guidance on sampling of waste waters. International Standards for Business, Government and Society, International Organization for Standardization.Google Scholar
- ISO (1997). Water quality – Sampling – Part 6: Guidance on sampling of river and surface water. International Organization for Standardization.Google Scholar
- Jian, X., Ping, W., Weifeng, G., Junxing, D., Lei, W., & Shugui, D. (2006). Seasonal and spatial distribution of nonylphenol in Lanzhou Reach of Yellow River in China. Chemosphere, 65, 1445–1451.CrossRefGoogle Scholar
- Jonkers, N., Laane, R. W. P. W., & Voogt, P. D. (2003). Fate of nonylphenol ethoxylates and their metabolites in two Dutch estuaries: Evidence of biodegradation in the fields. Environmental Science and Technology, 37, 321–327.CrossRefGoogle Scholar
- Kwack, S. J., Kwon, O. K., Hyung, S., Kim, S. S., Kim, S. H., Sohn, K. H., et al. (2002). Comparative evaluation of alkylphenolic compounds on estrogenic activity in vitro and in vivo. Journal of Toxicology and Environmental Health, 65, 419–431.CrossRefGoogle Scholar
- Li, D., Kim, M., Oh, J. R., & Park, J. (2004b). Distribution characteristics of nonylphenols in the artificial Lake Shihwa, and surrounding creeks in Korea. Chemosphere, 56, 783–790.CrossRefGoogle Scholar
- Li, D., Kim, M., Shim, V. J., Yim, U. H., Oh, J. R., & Kwon, Y. J. (2004a). Seasonal flux of nonylphenol in Han River, Korea. Chemosphere, 56, 1–6.CrossRefGoogle Scholar
- Li, D., Oh, J. R., & Park, J. (2003). Direct extraction of alkylphenols, chlorophenols and bisphenol A from acid-digested sediment suspension for simultaneous gas chromatographic– mass spectrometric analysis. Journal of Chromatography. A, 1012, 207–214.CrossRefGoogle Scholar
- Li, X., Luan, T., Liang, Y., Wong, M., & Lan, C. (2007). Distribution patterns of octylphenol and nonylphenol in the aquatic system at Mai Po Marshes Nature Reserve, a subtropical estuarine wetland in Hong Kong. Journal of Environmental Sciences, 19, 657–662.CrossRefGoogle Scholar
- Liu, J., Chi, Y., Jiang, G., Tai, C., Peng, J., & Hu, J. T. (2004). Ionic liquid-based liquid-phase microextraction, a new sample enrichment procedure for liquid chromatography. Journal of Chromatography. A, 1026(1–2), 143–147.CrossRefGoogle Scholar
- Loss, R., Hanke, G., Umlauf, G., & Eisenreich, S. J. (2007). LC–MS–MS analysis and occurence of octyl- and nonylphenol, their ethoxylates and their carboxylates in Belgian and Italian textile industry, waste water treatment plant effluents and surface waters. Chemosphere, 66, 690–699.CrossRefGoogle Scholar
- Loyo-Rosales, I. E., Schmitz-Afonso, J., Rice, C. P., & Torrents, A. (2003). Analysis of octyland nonylphenol and their ethoxylates in water and sediments by liquid chromatography tandem mass spectrometry. Analytical Chemiatry, 75, 4811–4817.CrossRefGoogle Scholar
- Luo, Q., Ban, M., Ando, H., Kitahashi, T., Bhandari, R. K., McCormick, S. D., et al. (2005). Distinct effects of 4-nonylphenol and estrogen- 17b on expression of estrogen receptor a gene in molting sockeye salmon. Comparative Biochemistry and Physiology, 140, 123–130.Google Scholar
- Matache, M. L., David, I. G., Matache, M., & Ropota, M. (2009). Seasonal variation in trace metals concentrations in the Ialomiţa River, Romania. Environmental Monitoring and Assessment, 153, 273–279.CrossRefGoogle Scholar
- Mayer, T., Bennie, D., Rosa, F., Rekas, G., Palabrica, V., & Schachtschneider, J. (2007). Occurrence of alkilphenolic substances in a Great Lakes coastal marsh, Cootes Paradise, ON, Canada. Environmental Pollution, 147, 683–690.CrossRefGoogle Scholar
- Mingzhu, F., Zhengyan, L., & Huiwang, G. (2007). Distribution characteristics of nonylphenol in Jiaozhou Bay of Qingdao and its adjacent rivers. Chemosphere, 69, 1009–1016.CrossRefGoogle Scholar
- Mitrita, M., Cruceru, I., Cruceru, L., & Petre, J. (2007). The results of collaborative interlaboratory study to estimate the performance characteristics of the gas chromatographic method for some alkyl phenols from water. Journal of Environmental Protection and Ecology, 8(2), 249–257.Google Scholar
- Pan, X. P., & Tsa, S. W. (2008). Solid phase microextraction procedure for the determination of alkylphenols in water by on-fiber derivatization with N-tert-butyl-dimethylsilyl-N-methyltrifluoroacetamide. Analytica Chimica Acta, 624, 247–252.CrossRefGoogle Scholar
- Patrolecco, L., Capri, S., De Angelis, S., Pagnotta, R., Polesello, S., & Valsecchi, S. (2006). Partition of nonylphenol and related compounds among different aquatic compartments in Timber River (Central Italy). Water, Air, and Soil Pollution, 172, 151–166.CrossRefGoogle Scholar
- Ribeiro, C., Tiritan, M. E., Rocha, E., & Rocha, M. J. (2009). Seasonal and spatial distribution of several endocrine-disrupting compounds in the Douro river estuary, Portugal. Archives of Environmental Contamination and Toxicology, 56, 1–11.CrossRefGoogle Scholar
- Schwaiger, J., Mallow, U., Ferling, H., Knoerr, S., Braunbeck, Th, Kalbfus, W., et al. (2002). How estrogenic is nonylphenol? A transgenerational study using rainbow trout (Oncorhynchus mykiss) as a test organism. Aquatic Toxicology, 59, 177–189.CrossRefGoogle Scholar
- Stihi, C., Popescu, V. I., Stihi, V., & Vlaicu, Gh. (2005). Inductively Coupled Plasma (ICP) and Total Dissolved Solids (TDS) measurements of surface waters from Ialomiţa River, Romanian. Journal of Physics, 50(9–10), 977–981.Google Scholar
- Takagai, Y., Kubota, Y., Akiyama, R., Aoyama, E., & Igarashi, S. (2004). Preconcentration technique for nonylphenol using cellulose cotton with homogenous liquid–liquid extraction for liquid chromatographic analysis. Analytical and Bioanalytical Chemistry, 380, 351–354.CrossRefGoogle Scholar
- US EPA (2006). US EPA priority pollutant list on EPA website. US Environmental Protection Agency (EPA), Washington, DC. Available from: http://www.epa.gov/waterscience/criteria/wqcriteria.html.
- Vanhoenacker, G., & Sandra, P. (2005). High temperature liquid chromatography and liquid chromatography–mass spectroscopy analysis of octylphenol ethoxylates on different stationary phases. Journal of Chromatography. A, 1082, 193.CrossRefGoogle Scholar
- Vitali, M., Ensabella, F., Stella, D., & Guidotti, M. (2004). Nonylphenols in freshwaters of the hydrologic system of an Italian district: Association with human activities and evaluation of human exposure. Chemosphere, 57, 1637–1647.CrossRefGoogle Scholar
- Ying, G. G. (2006). Fate, behaviour and effects of surfactants and their degradation products in the environment – a review. Environment International, 32, 417–431.CrossRefGoogle Scholar
- Ying, G. G., Williams, B., & Kookana, R. (2002). Environmental fate of alkylphenols and alkylphenol ethoxylates–a review. Environment International, 28, 1–12.CrossRefGoogle Scholar
- Zafra, A., Olmo, M., Suárez, B., Hontoria, E., Navalón, A., & Vílchez, J. L. (2003). Gas chromatographic–mass spectrometric method for the determination of bisphenol A and its chlorinated derivatives in urban wastewater. Water Research, 37(4), 735–742.CrossRefGoogle Scholar
- Zgoła-Grzes’kowiak, A., Grzes’kowiak, T., Rydlichowski, R., & Lukaszewski, Z. (2009). Determination of nonylphenol and short-chained nonylphenol ethoxylates in drain water from an agricultural area. Chemosphere, 75, 513–518.CrossRefGoogle Scholar