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Trace analysis of UV filters and musks in living fish by in vivo SPME-GC-MS

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Abstract

A method was developed for the simultaneous determination of two groups of personal care products, namely UV filters (oxybenzone, 3-(4-methylbenzylidene)camphor, padimate-O, 2-ethylhexyl-4-methoxycinnamate, and octocrylene) and polycyclic aromatic musks (galaxolide and tonalide), in fish by in vivo solid-phase microextraction followed by gas chromatography–mass spectrometry. The in vivo method was validated by carrying out in vitro experiments; the method validation parameters were linearity (r2 > 0.98), interday precision (relative standard deviations < 35.50%), limits of detection and quantification ranging from 2 to 25 ng g−1 and 5 to 70 ng g−1, respectively. The calibrations in vivo and in vitro were determined using a pre-equilibrium sampling rate calibration method. In vivo sampling rate (Rs) was greater than that in vitro; therefore in vivo Rs was applied to the uptake and elimination tracing under controlled laboratory conditions to avoid quantitation error. All analytes were bioaccumulated in muscle tissue over the 5-day exposure in different grades depending on their molecular structure and physicochemical properties; the most absorbed compound was tonalide and the least absorbed compound was padimate-O. The elimination rate was initially high with a rapid decrease of the analyte concentrations for the first 24 h; thereafter, the rate of elimination tended to decrease which indicated that the target analytes were bioaccumulated. To our knowledge, this is the first time that UV filters have been analyzed with in vivo SPME-GC-MS. The proposed method is a simple, miniaturized, and non-lethal alternative for the determination of personal care products in living organisms.

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References

  1. Anca Caliman F, Gavrilescu M. Pharmaceuticals, personal care products and endocrine disrupting agents in the environment – a review. Clean. 2009;37:277–303. https://doi.org/10.1002/clen.200900038.

    Article  CAS  Google Scholar 

  2. Birkholz DA, Stilson SM, Elliott HS. Analysis of emerging contaminants in drinking water. In: Ahuja S, editor. Comprehensive water quality and purification, volume 2. Elsevier; 2014, pp. 212–229. https://doi.org/10.1016/B978-0-12-382182-9.00035-9.

  3. Witorsch RJ, Thomas JA. Personal care products and endocrine disruption: a critical review of the literature. Crit Rev Toxicol. 2010;40:1–30. https://doi.org/10.3109/10408444.2010.515563.

    Article  CAS  PubMed  Google Scholar 

  4. Organisation for Economic Co-operation and Development (OECD). Bioaccumulation in fish: aqueous and dietary exposure. In: Guidelines for testing of chemicals. OECD. 2011. https://www.oecd-ilibrary.org/environment/test-no-305-bioaccumulation-in-fish-aqueous-and-dietary-exposure_9789264185296-en;jsessionid=IsLXSzXJvm_hQV0QxkK0ldW3.ip-10-240-5-188. Accessed 12 May 2018.

  5. Gagnon MM, Hodson PV. Field studies using fish biomarkers – how many fish are enough? Mar Pollut Bull. 2012;64:2871–6. https://doi.org/10.1016/j.marpolbul.2012.08.016.

    Article  CAS  PubMed  Google Scholar 

  6. Núnez M, Borrull F, Pocurull E, Fontanals N. Sample treatment for the determination of emerging organic contaminants in aquatic organisms. Trends Anal Chem. 2017;97:136–45. https://doi.org/10.1016/j.trac.2017.09.007.

    Article  CAS  Google Scholar 

  7. Meinerling M, Daniels M. A validated method for the determination of traces of UV filters in fish using LC–MS/MS. Anal Bioanal Chem. 2006;386:1465–73. https://doi.org/10.1007/s00216-006-0706-9.

    Article  CAS  PubMed  Google Scholar 

  8. Gatermann R, Hellou J, Hühnerfuss H, Rimkus G, Zitko V. Polycyclic and nitro musks in the environment: a comparison between Canadian and European aquatic biota. Chemosphere. 1999;38:3431–41. https://doi.org/10.1016/S0045-6535(98)00564-5.

    Article  CAS  Google Scholar 

  9. Mottaleb MA, Usenko S, O’Donnell JG, Ramirez AJ, Brooks BW, Chambliss CK. Gas chromatography–mass spectrometry screening methods for select UV filters, synthetic musks, alkylphenols, an antimicrobial agent, and an insect repellent in fish. J Chromatogr A. 2009;1216:815–23. https://doi.org/10.1016/j.chroma.2008.11.072.

    Article  CAS  PubMed  Google Scholar 

  10. Draisci R, Marchiafav C, Ferretti E, Palleschi L, Catellani G, Anastasio A. Evaluation of musk contamination of freshwater fish in Italy by accelerated solvent extraction and gas chromatography with mass spectrometric detection. J Chromatogr A. 1998;814:187–97.

    Article  CAS  PubMed  Google Scholar 

  11. Gago-Ferrero P, Díaz-Cruz MS, Barceló D. Multi-residue method for trace level determination of UV filters in fish based on pressurized liquid extraction and liquid chromatography–quadrupole-linear ion trap-mass spectrometry. J Chromatogr A. 2013;1286:93–101. https://doi.org/10.1016/j.chroma.2013.02.056.

    Article  CAS  PubMed  Google Scholar 

  12. Negreira N, Rodríguez I, Rodil R, Rubí E, Cela R. Optimization of matrix solid-phase dispersion conditions for UV filters determination in biota samples. Intern J Environ Anal Chem. 2013;93:1174–88. https://doi.org/10.1080/03067319.2012.702277.

    Article  CAS  Google Scholar 

  13. Saraiva M, Cavalheiro J, Lanceleur L, Monperrus M. Synthetic musk in seafood products from South Europe using a quick, easy, cheap, effective, rugged and safe extraction method. Food Chem. 2016;200:330–5. https://doi.org/10.1016/j.foodchem.2016.01.017.

    Article  CAS  PubMed  Google Scholar 

  14. Xu J, Chen G, Huang S, Qiu J, Jiang R, Zhu F, et al. Application of in vivo solid-phase microextraction in environmental analysis. Trends Anal Chem. 2016;85:26–35. https://doi.org/10.1016/j.trac.2016.03.003.

    Article  CAS  Google Scholar 

  15. Wang S, Oakes KD, Bragg LM, Pawliszyn J, Dixon G, Servos MR. Validation and use of in vivo solid phase micro-extraction (SPME) for the detection of emerging contaminants in fish. Chemosphere. 2011;85:1472–80. https://doi.org/10.1016/j.chemosphere.2011.08.035.

    Article  CAS  PubMed  Google Scholar 

  16. Ouyang G, Oakes KD, Bragg L, Wang S, Liu H, Cui S, et al. Sampling-rate calibration for rapid and nonlethal monitoring of organic contaminants in fish muscle by solid-phase microextraction. Environ Sci Technol. 2011;45:7792–8. https://doi.org/10.1021/es201709j.

    Article  CAS  PubMed  Google Scholar 

  17. Huang S, Xu J, Wu J, Hong H, Chen G, Jiang R, et al. Rapid detection of five anesthetics in tilapias by in vivo solid phase microextraction coupling with gas chromatography-mass spectrometry. Talanta. 2017;168:263–8. https://doi.org/10.1016/j.talanta.2017.03.045.

    Article  CAS  PubMed  Google Scholar 

  18. Chen G, Jiang R, Qiu J, Cai S, Zhu F, Ouyang G. Environmental fates of synthetic musks in animal and plant: an in vivo study. Chemosphere. 2015;138:584–91. https://doi.org/10.1016/j.chemosphere.2015.07.003.

    Article  CAS  PubMed  Google Scholar 

  19. Allan IJ, Bæk K, Haugen TO, Hawley KL, Høgfeldt AS, Lillicrap AD. In vivo passive sampling of nonpolar contaminants in brown trout (Salmo trutta). Environ Sci Technol. 2013;47:11660–7. https://doi.org/10.1021/es401810r.

    Article  CAS  PubMed  Google Scholar 

  20. Vuckovic D, Shirey R, Chen Y, Sidisky L, Aurand C, Stenerson K, et al. In vitro evaluation of new biocompatible coatings for solid-phase microextraction: implications for drug analysis and in vivo sampling applications. Anal Chim Acta. 2009;638:175–85. https://doi.org/10.1016/j.aca.2009.02.049.

    Article  CAS  PubMed  Google Scholar 

  21. Zhang X, Oakes KD, Hoque ME, Luong D, Taheri-Nia S, Lee C, et al. Depth-profiling of environmental pharmaceuticals in biological tissue by solid-phase microextraction. Anal Chem. 2012;84:6956–62. https://doi.org/10.1021/ac3004659.

    Article  CAS  PubMed  Google Scholar 

  22. Zhang X, Oakes KD, Wang S, Cui S, Pawliszyn J, Metcalfe CD, et al. In vivo sampling of environmental organic contaminants in fish by solid-phase microextraction. Trends Anal Chem. 2012;32:31–9.

    Article  CAS  Google Scholar 

  23. Ouyang G, Vuckovic D, Pawliszyn J. Nondestructive sampling of living systems using in vivo solid-phase microextraction. Chem Rev. 2011;111:2784–814. https://doi.org/10.1021/cr100203t.

    Article  CAS  PubMed  Google Scholar 

  24. Bai Z, Pilote A, Sarker PK, Vandenberg G, Pawliszyn J. In vivo solid-phase microextraction with in vitro calibration: determination of off-flavor components in live fish. Anal Chem. 2013;85:2328–32. https://doi.org/10.1021/ac3033245.

    Article  CAS  PubMed  Google Scholar 

  25. Xu J, Luo J, Ruan J, Zhu F, Luan T, Liu H, et al. In vivo tracing uptake and elimination of organic pesticides in fish muscle. Environ Sci Technol. 2014;48:8012–20. https://doi.org/10.1021/es5009032.

    Article  CAS  PubMed  Google Scholar 

  26. Ocaña-Rios I, Peña-Alvarez A, Loeza-Fuentes E, Zuñiga-Perez I. Determination of personal care products in fish tissue based on matrix solid-phase dispersion combined with programmable split/splitless injector gas chromatography-mass spectrometry. Food Anal Methods. 2018;11:2272–9. https://doi.org/10.1007/s12161-018-1206-1.

    Article  Google Scholar 

  27. Akutsu K, Yoshimitsu M, Kitagawa Y, Takatori S, Fukui N, Osakada M, et al. Evaluation of the matrix-like effect in multiresidue pesticide analysis by gas chromatography with tandem mass spectrometry. J Sep Sci. 2017;40:1293–300. https://doi.org/10.1002/jssc.201600942.

    Article  CAS  PubMed  Google Scholar 

  28. American Society for Testing and Materials. Standard guide for conducting bioconcentration tests with fishes and saltwater bivalve mollusks (E 1022–94). ASTM. 1994 https://www.arpae.it/cms3/documenti/_cerca_doc/ecotossicologia/ASTM_E_1022_bioconcentrazione.pdf. Accessed 01 Feb 2019.

  29. Michael C, Bayona JM, Lambropoulou D, Agüera A, Fatta-Kassinos D. Two important limitations relating to the spiking of environmental samples with contaminants of emerging concern: how close to the real analyte concentrations are the reported recovered values? Environ Sci Pollut Res. 2017;24:15202–5. https://doi.org/10.1007/s11356-017-9154-7.

    Article  Google Scholar 

  30. Shepard KL. Functions for fish mucus. Rev Fish Biol Fish. 1994;4:401–29. https://doi.org/10.1007/BF00042888.

    Article  Google Scholar 

  31. Peck AM. Analytical methods for the determination of persistent ingredients of personal care products in environmental matrices. Anal Bioanal Chem. 2006;386:907–39. https://doi.org/10.1007/s00216-006-0728-3.

    Article  CAS  PubMed  Google Scholar 

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Acknowledgements

This work was supported by Dirección General de Asuntos del Personal Académico from the Universidad Nacional Autónoma de México (DGAPA-UNAM) [grant PAPIIT: IN 218116] and Faculty of Chemistry [grant PAIP: 5000-9026]. The authors want to thank Consejo Nacional de Ciencia y Tecnología (CONACYT) for the doctoral scholarship awarded to Iran Ocaña-Rios (scholar number 273473). The authors also want to thank Mr. Pascual Sánchez Ramírez for providing the trout, Rocío Juárez Cipres for technical support and Perkin Elmer de México S.A. for instrumental GC-MS support.

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Authors and Affiliations

  1. Facultad de Química, Departamento de Química Analítica, Universidad Nacional Autónoma de México, 04510, Ciudad de México, Mexico

    Iran Ocaña-Rios & Araceli Peña-Alvarez

  2. Perkin Elmer México S. A, 01020, Ciudad de México, Mexico

    Ignacio Zuñiga-Perez

  3. Facultad de Medicina Veterinaria y Zootecnia, Departamento de Abejas, Conejos y Organismos Acuáticos, Universidad Nacional Autónoma de México, 04510, Ciudad de México, Mexico

    Elena Loeza-Fuentes

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  1. Iran Ocaña-Rios
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  4. Elena Loeza-Fuentes
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Correspondence to Araceli Peña-Alvarez.

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All animal experimental procedures were approved by the Bioethic Committee for Animal Health (CICUAL, Faculty of Chemistry, UNAM).

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Ocaña-Rios, I., Peña-Alvarez, A., Zuñiga-Perez, I. et al. Trace analysis of UV filters and musks in living fish by in vivo SPME-GC-MS. Anal Bioanal Chem 411, 3209–3218 (2019). https://doi.org/10.1007/s00216-019-01791-5

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