Skip to main content
SpringerLink
Log in

A Combination of Factorial Design, Off-line SPE and GC–MS Method for Quantifying Seven Endocrine Disrupting Compounds in Water

  • Research paper
  • Published:
International Journal of Environmental Research Aims and scope Submit manuscript

Abstract

A sensitive and reliable analytical method for the simultaneous determination of seven endocrine disrupting compounds (EDCs) in water was developed and validated. This quantification method is based on solid phase extraction (SPE) followed by a derivatization with BSTFA and finally the seven EDCs were analyzed by gas chromatography–mass spectrometry (GC–MS). A 23 factorial design was used to optimize the extraction procedure. Three factors, namely sample volume, elution solvent, and pH of sample were investigated using Doehlert matrix. The optimal conditions of SPE method were: HLB cartridge, 540 mL of water sample with a pH 8 and 10 mL of mixture of ethyl acetate/acetone with a ratio of (55/45, v/v) in the elution step. For validation of the technique, accuracy, precision, detection and quantification limits, linearity, sensibility and selectivity were determined. Extraction recovery of these seven EDCs were above 90% with relative standard deviations (RSD) ≤ 2%. The method limit of detection and limit of quantification were in the range of 0.33–3.33 and 1–10 ng/L, respectively.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Fig. 1
Fig. 2
Fig. 3
Fig. 4

Similar content being viewed by others

References

  • Aydin E, Talinli I (2013) Analysis, occurrence and fate of commonly used pharmaceuticals and hormones in the Buyukcekmece Watershed, Turkey. Chemosphere 90:2004–2012. doi:10.1016/j.chemosphere.2012.10.074

    Article  CAS  Google Scholar 

  • Ballesteros-Gómez A, Rubio S, Pérez-Bendito D (2009) Analytical methods for the determination of bisphenol A in food. J Chromatogr A 1216:449–469. doi:10.1016/j.chroma.2008.06.037

    Article  Google Scholar 

  • Belhaj D, Baccar R, Jaabiri I et al (2015) Fate of selected estrogenic hormones in an urban sewage treatment plant in Tunisia (North Africa). Sci Total Environ 505:154–160. doi:10.1016/j.scitotenv.2014.10.018

    Article  CAS  Google Scholar 

  • Evgenidou EN, Konstantinou IK, Lambropoulou DA (2015) Occurrence and removal of transformation products of PPCPs and illicit drugs in wastewaters: a review. Sci Total Environ 505:905–926. doi:10.1016/j.scitotenv.2014.10.021

    Article  CAS  Google Scholar 

  • Facco JF, Martins ML, Bernardi G et al (2015) Optimization and validation of a multiresidue method for pesticide determination in maize using gas chromatography coupled to tandem mass spectrometry. Anal Methods 7:359–365. doi:10.1039/C4AY01970A

    Article  Google Scholar 

  • Friedrich MT, Martins ML, Prestes OD, Zanella R (2016) Use of factorial design in the development of multiresidue method for determination of pesticide residues in wheat by liquid chromatography-tandem mass spectrometry. Food Anal Methods 9:2541–2551. doi:10.1007/s12161-016-0447-0

    Article  Google Scholar 

  • Gao L, Sun L, Wan S et al (2013) Degradation kinetics and mechanism of emerging contaminants in water by dielectric barrier discharge non-thermal plasma: the case of 17β-Estradiol. Chem Eng J 228:790–798. doi:10.1016/j.cej.2013.05.079

    Article  CAS  Google Scholar 

  • Gorga M, Petrovic M, Barceló D (2013) Multi-residue analytical method for the determination of endocrine disruptors and related compounds in river and waste water using dual column liquid chromatography switching system coupled to mass spectrometry. J Chromatogr A 1295:57–66. doi:10.1016/j.chroma.2013.04.028

    Article  CAS  Google Scholar 

  • Grover DP, Zhang ZL, Readman JW, Zhou JL (2009) A comparison of three analytical techniques for the measurement of steroidal estrogens in environmental water samples. Talanta 78:1204–1210. doi:10.1016/j.talanta.2008.12.049

    Article  CAS  Google Scholar 

  • Guedes-Alonso R, Sosa-Ferrera Z, Santana-Rodríguez JJ (2013) Simultaneous determination of hormonal residues in treated waters using ultrahigh performance liquid chromatography-tandem mass spectrometry. J Anal Methods Chem 2013:1–8. doi:10.1155/2013/210653

    Article  Google Scholar 

  • Hibbert DB (2012) Experimental design in chromatography: a tutorial review. J Chromatogr B 910:2–13. doi:10.1016/j.jchromb.2012.01.020

    Article  CAS  Google Scholar 

  • Huang B, Pan X-J, Wan X et al (2011) Simultaneous determination of steroid endocrine disrupting chemicals in water by solid phase extraction-derivatization- gas chromatographic-mass spectrometry. Chin J Anal Chem 39:449–454. doi:10.1016/S1872-2040(10)60431-8

    Article  CAS  Google Scholar 

  • Jiang J-Q, Zhou Z, Sharma VK (2013) Occurrence, transportation, monitoring and treatment of emerging micro-pollutants in waste water—a review from global views. Microchem J 110:292–300. doi:10.1016/j.microc.2013.04.014

    Article  CAS  Google Scholar 

  • Jin W, Huang B, Wang B et al (2013) Simultaneous determination of androgens and progestogen in surface water and sediment by gas chromatography-mass spectrometry. Chin J Anal Chem 41:205–209. doi:10.1016/S1872-2040(13)60628-3

    Article  Google Scholar 

  • Karnjanapiboonwong A, Suski JG, Shah AA, Cai Q, Morse AN, Anderson TA (2011) Occurrence of PPCPs at a wastewater treatment plant and in soil and groundwater at a land application site. Water Air Soil Pollut 216:257–273. doi:10.1007/s11270-010-0532-8

    Article  CAS  Google Scholar 

  • Kemmerich M, Rizzetti TM, Martins ML et al (2015) Optimization by central composite design of a modified QuEChERS method for extraction of pesticide multiresidue in sweet pepper and analysis by ultra-high-performance liquid chromatography–tandem mass spectrometry. Food Anal Methods 8:728–739. doi:10.1007/s12161-014-9951-2

    Article  Google Scholar 

  • Labadie P, Budzinski H (2005) Determination of steroidal hormone profiles along the Jalle d’Eysines River (near Bordeaux, France). Environ Sci Technol 39:5113–5120. doi:10.1021/es048443g

    Article  CAS  Google Scholar 

  • Latrous El Atrache L, Ben Sghaier R, Bejaoui Kefi B et al (2013) Factorial design optimization of experimental variables in preconcentration of carbamates pesticides in water samples using solid phase extraction and liquid chromatography–electrospray-mass spectrometry determination. Talanta 117:392–398. doi:10.1016/j.talanta.2013.09.032

    Article  CAS  Google Scholar 

  • Laurenson JP, Bloom RA, Page S, Sadrieh N (2014) Ethinyl estradiol and other human pharmaceutical estrogens in the aquatic environment: a review of recent risk Assessment Data. AAPS J 16:299–310. doi:10.1208/s12248-014-9561-3

    Article  CAS  Google Scholar 

  • Lee I-S, Lee S-H, Oh J-E (2010) Occurrence and fate of synthetic musk compounds in water environment. Water Res 44:214–222. doi:10.1016/j.watres.2009.08.049

    Article  CAS  Google Scholar 

  • Munaretto JS, Ferronato G, Ribeiro LC et al (2013) Development of a multiresidue method for the determination of endocrine disrupters in fish fillet using gas chromatography–triple quadrupole tandem mass spectrometry. Talanta 116:827–834. doi:10.1016/j.talanta.2013.07.047

    Article  CAS  Google Scholar 

  • Net S, Rabodonirina S, Sghaier RB et al (2015) Distribution of phthalates, pesticides and drug residues in the dissolved, particulate and sedimentary phases from transboundary rivers (France–Belgium). Sci Total Environ 521–522:152–159. doi:10.1016/j.scitotenv.2015.03.087

    Article  Google Scholar 

  • Nie Y, Qiang Z, Zhang H, Ben W (2012) Fate and seasonal variation of endocrine-disrupting chemicals in a sewage treatment plant with A/A/O process. Sep Purif Technol 84:9–15. doi:10.1016/j.seppur.2011.01.030

    Article  CAS  Google Scholar 

  • Nielsen S (2014) Food analysis. Springer Science & Business Media, New York

    Google Scholar 

  • Rabodonirina S, Net S, Ouddane B et al (2015) Distribution of persistent organic pollutants (PAHs, Me-PAHs, PCBs) in dissolved, particulate and sedimentary phases in freshwater systems. Environ Pollut 206:38–48. doi:10.1016/j.envpol.2015.06.023

    Article  CAS  Google Scholar 

  • Reinen J, Suter MJ-F, Vögeli AC et al (2010) Endocrine disrupting chemicals—linking internal exposure to vitellogenin levels and ovotestis in Abramis brama from Dutch surface waters. Environ Toxicol Pharmacol 30:209–223. doi:10.1016/j.etap.2010.07.004

    Article  CAS  Google Scholar 

  • Rice SL, Hale RC (2009) Parameters for ultra-performance liquid chromatographic/tandem mass spectrometric analysis of selected androgens versus estrogens in aqueous matrices. Anal Chem 81:6716–6724. doi:10.1021/ac900134m

    Article  CAS  Google Scholar 

  • Sghaier RB, Net S, Ghorbel-Abid I et al (2017) Simultaneous detection of 13 endocrine disrupting chemicals in water by a combination of SPE-BSTFA derivatization and GC–MS in transboundary rivers (France–Belgium). Water Air Soil Pollut. doi:10.1007/s11270-016-3195-2

    Google Scholar 

  • Sim W-J, Lee J-W, Oh J-E (2010) Occurrence and fate of pharmaceuticals in wastewater treatment plants and rivers in Korea. Environ Pollut 158:1938–1947. doi:10.1016/j.envpol.2009.10.036

    Article  CAS  Google Scholar 

  • Stafiej A, Pyrzynska K, Regan F (2007) Determination of anti-inflammatory drugs and estrogens in water by HPLC with UV detection. J Sep Sci 30:985–991. doi:10.1002/jssc.200600433

    Article  CAS  Google Scholar 

  • Sun Y, Huang H, Sun Y et al (2014) Occurrence of estrogenic endocrine disrupting chemicals concern in sewage plant effluent. Front Environ Sci Eng 8:18–26. doi:10.1007/s11783-013-0573-5

    Article  CAS  Google Scholar 

  • Thurman EM, Writer JH, Ferrer I (2013) Injection port derivatization for GC/MS–MS. In: Comprehensive analytical chemistry. Elsevier, pp 115–141

  • Vandenberg LN, Colborn T, Hayes TB et al (2012) Hormones and endocrine-disrupting chemicals: low-dose effects and nonmonotonic dose responses. Endocr Rev 33:378–455. doi:10.1210/er.2011-1050

    Article  CAS  Google Scholar 

  • Xu Y, Xu N, Llewellyn NR, Tao H (2014) Occurrence and removal of free and conjugated estrogens in wastewater and sludge in five sewage treatment plants. Env Sci Process Impacts 16:262–270. doi:10.1039/C3EM00199G

    Article  CAS  Google Scholar 

  • Yang S, Hai FI, Nghiem LD et al (2013) Understanding the factors controlling the removal of trace organic contaminants by white-rot fungi and their lignin modifying enzymes: a critical review. Bioresour Technol 141:97–108

    Article  CAS  Google Scholar 

  • Yang Y, Cao X, Zhang M, Wang J (2015) Occurrence and distribution of endocrine-disrupting compounds in the Honghu Lake and East Dongting Lake along the Central Yangtze River, China. Environ Sci Pollut Res 22:17644–17652. doi:10.1007/s11356-015-4980-y

    Article  CAS  Google Scholar 

  • Yu Y, Wu L (2015) Determination and occurrence of endocrine disrupting compounds, pharmaceuticals and personal care products in fish (Morone saxatilis). Front Environ Sci Eng 9:475–481. doi:10.1007/s11783-014-0640-6

    Article  CAS  Google Scholar 

  • Zhang R, Li N, Wang C et al (2011) Ionic liquid foam floatation coupled with solid phase extraction for separation and determination of hormones by high-performance liquid chromatography. Anal Chim Acta 704:98–109. doi:10.1016/j.aca.2011.08.016

    Article  CAS  Google Scholar 

  • Zoeller RT, Brown TR, Doan LL et al (2012) Endocrine-disrupting chemicals and public health protection: a Statement of Principles from The Endocrine Society. Endocrinology 153:4097–4110. doi:10.1210/en.2012-1422

    Article  CAS  Google Scholar 

Download references

Acknowledgements

The authors are grateful for the support provided by CPER CLIMBIO project. We acknowledge the financial support from the Tunisian Minister of Higher Education and Scientific Research, which provided a PhD scholarship for Rafika Ben Sghaier.

Author information

Authors and Affiliations

  1. LAboratoire de Spectrochimie Infrarouge et Raman (LASIR)-UMR CNRS 8516, Université de Lille, Equipe Physico-chimie de l’Environnement, Cité Scientifique, 59655, Villeneuve d’Ascq, France

    Rafika Ben Sghaier, Ines Tlili, Sopheak Net & Baghdad Ouddane

  2. Faculté des Sciences de Bizerte, Laboratoire d’Application de la Chimie aux Ressources et Substances Naturelles et à l’Environnement (LACReSNE), Université de Carthage, Zarzouna, 7021, Bizerte, Tunisie

    Rafika Ben Sghaier, Ines Tlili, Ibtissem Ghorbel-Abid, Dalila Ben Hassan-Chehimi & Malika Trabelsi-Ayadi

  3. Faculté des Sciences de Tunis, Laboratoire de Chimie Analytique et Electrochimie (LCAE), Université de Tunis El Manar, Campus universitaire, 2092, Tunis, Tunisie

    Latifa Latrous El Atrache

  4. Laboratoire méthodes et techniques d’analyses (LMTA), Institut national de recherche d’analyse physico-chimique (INRAP), Tunis, Tunisie

    Ibtissem Ghorbel-Abid

Authors
  1. Rafika Ben Sghaier
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Ines Tlili
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Latifa Latrous El Atrache
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Sopheak Net
    View author publications

    You can also search for this author in PubMed Google Scholar

  5. Ibtissem Ghorbel-Abid
    View author publications

    You can also search for this author in PubMed Google Scholar

  6. Baghdad Ouddane
    View author publications

    You can also search for this author in PubMed Google Scholar

  7. Dalila Ben Hassan-Chehimi
    View author publications

    You can also search for this author in PubMed Google Scholar

  8. Malika Trabelsi-Ayadi
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Sopheak Net.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Ben Sghaier, R., Tlili, I., Latrous El Atrache, L. et al. A Combination of Factorial Design, Off-line SPE and GC–MS Method for Quantifying Seven Endocrine Disrupting Compounds in Water. Int J Environ Res 11, 613–624 (2017). https://doi.org/10.1007/s41742-017-0054-y

Download citation

  • Received:

  • Revised:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s41742-017-0054-y

Keywords

Search

Navigation