Abstract
Soil can contain large numbers of endocrine disrupting chemicals (EDCs). The varied physicochemical properties of EDCs constitute a great challenge to their determination in this type of environmental matrix. In this work, an analytical method was developed for the simultaneous determination of various classes of EDCs, including parabens, alkylphenols, phenylphenols, bisphenol A, and triclosan, in soils, sediments, and sewage sludge. The method uses microwave-assisted extraction (MAE) in combination with continuous solid-phase extraction for determination by gas chromatography–mass spectrometry. A systematic comparison of the MAE results with those of ultrasound-assisted and Soxhlet extraction showed MAE to provide the highest extraction efficiency (close to 100 %) in the shortest extraction time (3 min). The proposed method provides a linear response over the range 2.0 − 5000 ng kg−1 and features limits of detection from 0.5 to 4.5 ng kg−1 depending on the properties of the EDC. The method was successfully applied to the determination of target compounds in agricultural soils, pond and river sediments, and sewage sludge. The sewage sludge samples were found to contain all target compounds except benzylparaben at concentration levels from 36 to 164 ng kg−1. By contrast, the other types of samples contained fewer EDCs and at lower concentrations (5.6 − 84 ng kg−1).
Similar content being viewed by others
References
Hester RE, Harrison RM (1999) Endocrine disrupting chemicals. Royal Society of Chemistry, Cambridge
Gorga M, Insa S, Petrovic M, Barceló D (2014) Analysis of endocrine disrupters and related compounds in sediments and sewage sludge using on-line turbulent flow chromatography–liquid chromatography–tandem mass spectrometry. J Chromatogr A 1352:29–37
European Commission (2003) 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). Off J Eur Comm L178/24−L178/27
European Commission (2000) Working document on sludge, third draft, ENV-E. 3/LM. European Union, Brussels, pp 1–19
US EPA (2006) Aquatic life criteria for nonylphenol. http://www.epa.gov/waterscience/criteria/nonylphenol/final-doc.pdf. (Accessed 9.10.2015)
European Commission (2013) Directive 2013/39/EU of the European Parliament and of the Council of 12 August 2013 amending Directives 2000/60/EC and 2008/105/EC as regards priority substances in the field of water policy. Off J Eur Comm L226/1–L226/17
Meesters RJW, Schröder HF (2002) Simultaneous determination of 4-nonylphenol and bisphenol A in sewage sludge. Anal Chem 74:3566–3574
Gatidou G, Thomaidis NS, Stasinakis AS, Lekkas TD (2007) Simultaneous determination of the endocrine disrupting compounds nonylphenol, nonylphenol ethoxylates, triclosan and bisphenol A in wastewater and sewage sludge by gas chromatography–mass spectrometry. J Chromatogr A 1138:32–41
Nie Y, Qiang Z, Zhang H, Adams C (2009) Determination of endocrine-disrupting chemicals in the liquid and solid phases of activated sludge by solid phase extraction and gas chromatography–mass spectrometry. J Chromatogr A 1216:7071–7080
Yu Y, Huang Q, Cui J, Zhang K, Tang C, Peng X (2011) Determination of pharmaceuticals, steroid hormones, and endocrine-disrupting personal care products in sewage sludge by ultra-high-performance liquid chromatography–tandem mass spectrometry. Anal Bioanal Chem 399:891–902
Yang Y, Lu L, Zhang J, Yang Y, Wu Y, Shao B (2014) Simultaneous determination of seven bisphenols in environmental water and solid samples by liquid chromatography–electrospray tandem mass spectrometry. J Chromatogr A 1328:26–34
Cha J, Cupples AM (2009) Detection of the antimicrobials triclocarban and triclosan in agricultural soils following land application of municipal biosolids. Water Res 43:2522–2530
Albero B, Sánchez-Brunete C, Miguel E, Pérez RA, Tadeo JL (2012) Determination of selected organic contaminants in soil by pressurized liquid extraction and gas chromatography tandem mass spectrometry with in situ derivatization. J Chromatogr A 1248:9–17
Liu R, Zhou JL, Wilding A (2004) Microwave-assisted extraction followed by gas chromatography–mass spectrometry for the determination of endocrine disrupting chemicals in river sediments. J Chromatogr A 1038:19–26
Vega-Morales T, Sosa-Ferrera Z, Santana-Rodríguez JJ (2011) Determination of various estradiol mimicking-compounds in sewage sludge by the combination of microwave-assisted extraction and LC–MS/MS. Talanta 85:1825–1834
Martinez-Moral MP, Tena MT (2011) Focused ultrasound solid-liquid extraction and selective pressurised liquid extraction to determine bisphenol A and alkylphenols in sewage sludge by gas chromatography-mass spectrometry. J Sep Sci 34:2513–2522
Żwir-Ferenc A, Biziuk M (2006) Solid phase extraction technique–trends opportunities and applications. Polish J Environ Stud 15:677–690
Lee HB, Peart TE (2000) Determination of bisphenol A in sewage effluent and sludge by solid-phase and supercritical fluid extraction and gas chromatography/mass spectrometry. J AOAC Inter 83:290–298
Petrovic M, Barceló D, Diaz A, Ventura F (2003) Low nanogram per liter determination of halogenated nonylphenols, nonylphenol carboxylates, and their non-halogenated precursors in water and sludge by liquid chromatography electrospray tandem mass spectrometry. J Am Soc Mass Spectrom 14:516–527
Liao C, Liu F, Moon HB, Yamashita N, Yun S, Kannan K (2012) Bisphenol analogues in sediments from industrialized areas in the United States, Japan, and Korea: spatial and temporal distributions. Environ Sci Technol 46:11558–11565
Morales S, Canosa P, Rodríguez I, Rubí E, Cela R (2005) Microwave assisted extraction followed by gas chromatography with tandem mass spectrometry for the determination of triclosan and two related chlorophenols in sludge and sediments. J Chromatogr A 1082:128–135
Pérez RA, Albero B, Miguel E, Sánchez-Brunete C (2012) Determination of parabens and endocrine-disrupting alkylphenols in soil by gas chromatography-mass spectrometry following matrix solid-phase dispersion or in-column microwave-assisted extraction: a comparative study. Anal Bioanal Chem 402:2347–2357
Petrovic M, Barceló D (2000) Determination of anionic and nonionic surfactants, their degradation products, and endocrine-disrupting compounds in sewage sludge by liquid chromatography/mass spectrometry. Anal Chem 72:4560–4567
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. Environ Inter 33:929–936
Céspedes R, Lacorte S, Ginebreda A, Barceló D (2008) Occurrence and fate of alkylphenols and alkylphenol ethoxylates in sewage treatment plants and impact on receiving waters along the Ter River (Catalonia, NE Spain). Environ Pollut 153:384–392
Xu J, Wu L, Chen W, Chang AC (2008) Simultaneous determination of pharmaceuticals, endocrine disrupting compounds and hormone in soils by gas chromatography–mass spectrometry. J Chromatogr A 1202:189–195
Ramírez N, Marcé RM, Borrull F (2011) Determination of parabens in house dust by pressurised hot water extraction followed by stir bar sorptive extraction and thermal desorption–gas chromatography–mass spectrometry. J Chromatogr A 1218:6226–6231
Ferreira AMC, Möder M, Laespada MEF (2011) Stir bar sorptive extraction of parabens, triclosan and methyl triclosan from soil, sediment and sludge with in situ derivatization and determination by gas chromatography–mass spectrometry. J Chromatogr A 1218:3837–3844
Official Method 994.16 (2000) AOAC Official Methods of analysis, Chap 2. AOAC, Gaithersburg, pp 40–44
Dane JH, Topp GC (eds) (2002) Methods of soil analysis. Part 4. Physical methods, soil. Soil Science Society of America, Madison, pp 422–426
Hesse PR (1972) A testbook of soil chemical analysis. Chemical Publishing, New York
US Environmental Protection Agency (1996) Method 3540C: Soxhlet extraction. US Environmental Protection Agency, Washington, DC
Azzouz A, Ballesteros E (2014) Trace analysis of endocrine disrupting compounds in environmental water samples by use of solid-phase extraction and gas chromatography with mass spectrometry detection. J Chromatogr A 1360:248–257
Peng X, Yu Y, Tang C, Tang J, Huang Q, Wang Z (2008) Occurrence of steroid strogens, endocrine-disrupting phenols, and acid pharmaceutical residues in urban riverine water of the Pearl River Delta, South China. Sci Total Environ 397:158–166
Brown TJ, Kinney CA (2011) Rapid lab-scale microwave-assisted extraction and analysis of antropogenic organic chemicals in river sediments. Int J Geosci 2:267–273
Regueiro J, Becerril E, Garcia-Jares C, Llompart M (2009) Trace analysis of parabens, triclosan and related chlorophenols in water by headspace solid-phase microextraction with in situ derivatization and gas chromatography–tandem mass spectrometry. J Chromatogr A 1216:4693–4702
Acknowledgments
The authors would like to thank the Technical Research Service of the University of Jaén for access to its gas chromatograph–mass spectrometry system.
Author information
Authors and Affiliations
Corresponding author
Ethics declarations
Conflict of interest
The authors declare that there are no conflicts of interest.
Rights and permissions
About this article
Cite this article
Azzouz, A., Ballesteros, E. Determination of 13 endocrine disrupting chemicals in environmental solid samples using microwave-assisted solvent extraction and continuous solid-phase extraction followed by gas chromatography–mass spectrometry. Anal Bioanal Chem 408, 231–241 (2016). https://doi.org/10.1007/s00216-015-9096-1
Received:
Revised:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1007/s00216-015-9096-1