Analytical and Bioanalytical Chemistry

, Volume 410, Issue 12, pp 2991–3001 | Cite as

Novel capsule phase microextraction in combination with liquid chromatography-tandem mass spectrometry for determining personal care products in environmental water

  • Sameer S. Lakade
  • Francesc Borrull
  • Kenneth G. Furton
  • Abuzar Kabir
  • Rosa Maria Marcé
  • Núria Fontanals
Research Paper


A novel sample preparation technique named capsule phase microextraction (CPME) is presented here. The technique utilizes a miniaturized microextraction capsule (MEC) as the extraction medium. The MEC consists of two conjoined porous tubular polypropylene membranes, one of which encapsulates the sorbent through sol-gel technology, while the other encapsulates a magnetic metal rod. As such, MEC integrates both the extraction and stirring mechanisms into a single device. The aim of this article is to demonstrate the application potential of CPME as sample preparation technique for the extraction of a group of personal care products (PCPs) from water matrices. Among the different sol-gel sorbent materials (UCON®, poly(caprolactone-dimethylsiloxane-caprolactone) (PCAP-DMS-CAP) and Carbowax 20M (CW-20M)) evaluated, CW-20M MEC demonstrated the best extraction performance for the selected PCPs. The extraction conditions for sol-gel CW-20M MEC were optimized, including sample pH, stirring speed, addition of salt, extraction time, sample volume, liquid desorption solvent, and time. Under the optimal conditions, sol-gel CW-20M MEC provided recoveries, ranging between 47 and 90% for all analytes, except for ethylparaben, which showed a recovery of 26%. The method based on CPME with sol-gel CW-20M followed by liquid chromatography-tandem mass spectrometry was developed and validated for the extraction of PCPs from river water and effluent wastewater samples. When analyzing different environmental samples, some analytes such as 2,4-dihydroxybenzophenone, 2,2-dihydroxy-4-4 methoxybenzophenone and 3-benzophenone were found at low ng L−1.


Capsule phase microextraction Microextraction capsule Liquid chromatography-tandem mass spectrometry Personal care products Environmental water samples 


Funding information

The authors would like to thank the Ministry of Economy, Industry and Competitiveness, Spain (Project CTQ2014–52617-P) for the financial support given.

Compliance with ethical standards

Conflict of interest

The authors declare that they have no conflict of interest.

Supplementary material

216_2018_984_MOESM1_ESM.pdf (143 kb)
ESM 1 (PDF 142 kb)


  1. 1.
    Kataoka H. Recent developments and applications of microextraction techniques in drug analysis. Anal Bioanal Chem. 2010;396:339–64.CrossRefGoogle Scholar
  2. 2.
    Pedrouzo M, Borrull F, Marcé RM, Pocurull E. Ultra-high-performance liquid chromatography-tandem mass spectrometry for determining the presence of eleven personal care products in surface and wastewaters. J Chromatogr A. 2009;1216:6994–7000.CrossRefGoogle Scholar
  3. 3.
    Sánchez-Prado L, Llompart M, Lores M, García-Jares, Bayona JM, Cela R. Monitoring the photochemical degradation of triclosan in wastewater by UV light and sunlight using solid-phase microextraction. Chemosphere. 2006;65:1338–47.CrossRefGoogle Scholar
  4. 4.
    Pedrouzo M, Borrull F, Marcé RM, Pocurull E. Stir-bar-sorptive extraction and ultra-high-performance liquid chromatography–tandem mass spectrometry for simultaneous analysis of UV filters and antimicrobial agents in water samples. Anal Bioanal Chem. 2010;397:2833–9.CrossRefGoogle Scholar
  5. 5.
    Lakade SS, Borrull F, Furton KG, Kabir A, Fontanals N, Marcé RM. Comparative study of different fabric phase sorptive extraction sorbents to determine emerging contaminants from environmental water using liquid chromatography–tandem mass spectrometry. Talanta. 2015;144:1342–51.CrossRefGoogle Scholar
  6. 6.
    Montesdeoca-Esponda S, Sosa-Ferrera Z, Kabir A, Furton KG, Santana-Rodríguez JJ. Fabric phase sorptive extraction followed by UHPLC-MS/MS for the analysis of benzotriazole UV stabilizers in sewage samples. Anal Bioanal Chem. 2015;407:8137–50.CrossRefGoogle Scholar
  7. 7.
    García-Guerra RB, Montesdeoca-Esponda S, Sosa-Ferrera Z, Kabir A, Furton KG, Santana-Rodríguez JJ. Rapid monitoring of residual UV-stabilizers in seawater samples from beaches using fabric phase sorptive extraction and UHPLC-MS/MS. Chemosphere. 2016;164:201–7.CrossRefGoogle Scholar
  8. 8.
    Silva ARM, Nogueira JMF. New approach on trace analysis of triclosan in personal care products, biological and environmental matrices. Talanta. 2008;74:1498–504.CrossRefGoogle Scholar
  9. 9.
    Cacho JI, Campillo N, Viñas P, Hernández-Córdoba M. Stir bar sorptive extraction with EG-silicone coating for bisphenols determination in personal care products by GC–MS. J Pharm Biomed Anal. 2013;78–79:255–60.CrossRefGoogle Scholar
  10. 10.
    Gilart N, Miralles N, Marcé RM, Borrull F, Fontanals N. Novel coatings for stir bar sorptive extraction to determine pharmaceuticals and personal care products in environmental waters by liquid chromatography and tandem mass spectrometry. Anal Chim Acta. 2013;774:51–60.CrossRefGoogle Scholar
  11. 11.
    Gilart N, Cormack PAG, Marcé RM, Borrull F, Fontanals N. Preparation of a polar monolithic coating for stir bar sorptive extraction of emerging contaminants from wastewaters. J Chromatogr A. 2013;1295:42–7.CrossRefGoogle Scholar
  12. 12.
    Bratkowska D, Marcé RM, Cormack PAG, Borrull F, Fontanals N. Development and application of a polar coating for stir bar sorptive extraction of emerging pollutants from environmental water samples. Anal Chim Acta. 2011;706:135–42.CrossRefGoogle Scholar
  13. 13.
    Huang X, Lin J, Yuan D, Hu R. Determination of steroid sex hormones in wastewater by stir bar sorptive extraction based on poly(vinylpyridine-ethylene dimethacrylate) monolithic material and liquid chromatographic analysis. J Chromatogr A. 2009;1216:3508–11.CrossRefGoogle Scholar
  14. 14.
    Huang X, Qiu N, Yuan D. Development and validation of stir bar sorptive extraction of polar phenols in water followed by HPLC separation in poly(vinylpyrrolididone-divinylbenzene) monolith. J Sep Sci. 2009;32:1407–14.CrossRefGoogle Scholar
  15. 15.
    Kabir A, Furton K G. Microextraction capsules and method of making. US Patent Application 2017; 20170023452: January 26, 2017.Google Scholar
  16. 16.
    Fent K, Zenker A, Rapp M. Widespread occurrence of estrogenic UV-filters in aquatic ecosystems in Switzerland. Environ Pollut. 2010;158:1817–24.CrossRefGoogle Scholar
  17. 17.
    Zenker A, Schmutz H, Fent K. Simultaneous trace determination of nine organic UV-absorbing compounds (UV filters) in environmental samples. J Chromatogr A. 2008;1202:64–74.CrossRefGoogle Scholar
  18. 18.
    Daiber EJ, DeMarini DM, Ravuri SA, Liberatore HK, Cuthbertson AA, Thompson-Klemish A, et al. Progressive increase in disinfection byproducts and mutagenicity from source to tap to swimming pool and spa water: impact of human inputs. Environ Sci Technol. 2016;50:6652–62.CrossRefGoogle Scholar
  19. 19.
    Giokas DL, Salvador A, Chisvert A. UV filters: from sunscreens to human body and the environment. TrAC Trends Anal Chem. 2007;26:360–74.CrossRefGoogle Scholar
  20. 20.
    Lakade SS, Borrull F, Furton KG, Kabir A, Marcé RM, Fontanals N. Dynamic fabric phase sorptive extraction for a group of pharmaceuticals and personal care products from environmental waters. J Chromatogr A. 2016;1456:19–26.CrossRefGoogle Scholar

Copyright information

© Springer-Verlag GmbH Germany, part of Springer Nature 2018

Authors and Affiliations

  • Sameer S. Lakade
    • 1
  • Francesc Borrull
    • 1
  • Kenneth G. Furton
    • 2
  • Abuzar Kabir
    • 2
  • Rosa Maria Marcé
    • 1
  • Núria Fontanals
    • 1
  1. 1.Department of Analytical Chemistry and Organic ChemistryUniversitat Rovira i Virgili, Sescelades CampusTarragonaSpain
  2. 2.International Forensic Research Institute, Department of Chemistry and BiochemistryFlorida International UniversityMiamiUSA

Personalised recommendations