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Determination of Caffeine and Its Metabolites in Wastewater Treatment Plants Using Solid-Phase Extraction and Liquid Chromatography–Tandem Mass Spectrometry

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Abstract

For caffeine and its seven major metabolites (i.e., theobromine, theophylline, paraxanthine, 1-methylxanthine, 3-methylxanthine, 7-methylxanthine, and xanthine), an optimized analytical method using liquid chromatography–tandem mass spectrometry (LC-MS/MS) for their detection in wastewater samples was developed in this study. Extraction of these compounds (recoveries ranged from 60.3 to 83.2%) was made possible by combining universal polymeric reversedphase cartridge and polymeric strong cation exchange cartridge. This method was applied to the determination of caffeine and its metabolites in the influent and effluent of an anaerobic–anoxic–oxic (A2O) process. In the A2O influent, caffeine and its metabolites (except xanthine) ranged from 1.39 to 5.45 μg/L, and their concentrations in the A2O effluent ranged from 10.2 to 171.3 ng/L. The mass load of caffeine was 14.9 g/day/1000 inhabitants, considering the population served by the target wastewater treatment plant (WWTP). The concentration of caffeine derivatives in wastewater influent is a tool for estimating the population size in the area served by WWTPs.

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References

  1. C. Vatovec, P. Phillips, E. Van Wagoner, T.M. Scott, E. Furlong, Sci. Total Environ., 2016, 572, 906.

    Article  CAS  PubMed  Google Scholar 

  2. Q. Sui, J. Huang, S. Deng, G. Yu, Q. Fan, Water Res., 2010, 44, 417.

    Article  CAS  PubMed  Google Scholar 

  3. L. Bijlsma, J.V. Sancho, E. Pitarch, M. Ibáñez, F. Hernandez, J. Chromatogr. A, 2009, 1216, 3078.

    Article  CAS  PubMed  Google Scholar 

  4. K. He, S. Echigo, S. Itoh, Sci. Total Environ., 2016, 565, 672.

    Article  CAS  PubMed  Google Scholar 

  5. T.A. Ternes, M. Bonerz, T. Schimdt, J. Chromatogr. A, 2001, 938, 175.

    Article  CAS  PubMed  Google Scholar 

  6. D.W. Kolpin, E.T. Furlong, M.T. Meyer, E.M. Thurman, S.D. Zaugg, L.B. Barber, H.T. Buxton, Environ. Sci. Technol., 2002, 36, 1202.

    Article  CAS  PubMed  Google Scholar 

  7. S. Franke, S. Hildebrandt, J. Schwarzbauer, M. Link, W. Francke, Fresenius, J. Anal. Chem., 1995, 353, 39.

    Article  CAS  Google Scholar 

  8. S. Ibrahim, M.Y. Shukor, M.A. Syed, A. Arina, N. Rahman, K. Abdul Khalil, S.A. Ahmad, Asian J. Plant Sci., 2014, 2, 18.

    Google Scholar 

  9. S.S. Dash and S.N. Gummadi, Biotechnol. Lett., 2006, 28, 1993.

    Article  PubMed  Google Scholar 

  10. M. Majewsky, T. Gallé, V. Yargeau, K. Fischer, Bioresour. Technol., 2011, 102, 7415.

    Article  CAS  PubMed  Google Scholar 

  11. S. Gokulakrishnan, K. Chandraraj, S.N. Gummadi, Enzyme Microb. Technol., 2005, 37, 225.

    Article  CAS  Google Scholar 

  12. A.Z. Tong, A.J. Ghoshdastidar, S. Fox, Environ. Sci. Pollut. Res., 2015, 22, 689.

    Article  Google Scholar 

  13. M. Huerta-Fontela, M.T. Galceran, J. Martin-Alonso, F. Ventura, Sci. Total Environ., 2008, 397, 31.

    Article  CAS  PubMed  Google Scholar 

  14. J.W. Kim, S.M. Yoon, S.J. Lee, M. Narumiya, N. Nakada, I.S. Han, H. Tanaka, in 2nd International Conference on Environment and Industrial Innovation, 2012, Singapore, 57.

  15. P. Segura, A. Garcîa-Ac, A. Lajeunesse, D. Ghosh, C. Gagnon, S. Sauvé, J. Environ. Monit., 2007, 9, 307.

    Article  CAS  PubMed  Google Scholar 

  16. A.M. Urtiaga, G. Pérez, R. Ibáñez, I. Ortiz, Desalination, 2013, 331, 26.

    Article  CAS  Google Scholar 

  17. M. Kim, P. Guerra, A. Shah, M. Parsa, M. Alaee, S.A. Smyth, Water Sci. Technol., 2014, 69, 2221.

    Article  CAS  PubMed  Google Scholar 

  18. O. Hillebrand, K. Nödler, T. Licha, M. Sauter, T. Geyer, Water Res., 2012, 46, 395.

    Article  CAS  PubMed  Google Scholar 

  19. N. Nakada, K. Komori, Y. Suzuki, C. Konishi, I. Houwa, H. Tanaka, Water Sci. Technol., 2007, 56, 133.

    Article  CAS  PubMed  Google Scholar 

  20. T. Okuda, N. Yamashita, H. Tanaka, H. Matsukawa, K. Tanabe, Environ. Int., 2009, 35, 815.

    Article  CAS  PubMed  Google Scholar 

  21. A.S. Ptolemy, E. Tzioumis, A. Thomke, S. Rifai, M. Kellogg, J. Chromatogr. B, 2010, 878, 409.

    Article  CAS  Google Scholar 

  22. T. Ogawa, H. Hattori, M. Iwai, K. Ito, K. Iwakura, A. Ishii, O. Suzuki, H. Seno, Forensic Toxicol., 2012, 30, 142.

    Article  CAS  Google Scholar 

  23. P.M.M. de Kesel, W.E. Lambert, C.P. Stove, Talanta, 2015, 144, 62.

    Article  PubMed  Google Scholar 

  24. J. Chae, D. Kim, B. Lee, E.J. Kim, K. Kwon, J. Chromatogr. B, 2012, 889-890, 44.

    Article  Google Scholar 

  25. R. Hao, J. Li, Y. Zhou, S. Cheng, Y. Zhang, Chemosphere, 2009, 75, 987.

    Article  CAS  PubMed  Google Scholar 

  26. E. Morita and E. Nakamura, Anal. Sci., 2011, 27, 489.

    Article  PubMed  Google Scholar 

  27. C.Y. Cheng, Y.C. Wang, W.H. Ding, Anal. Sci., 2011, 27, 197.

    Article  CAS  PubMed  Google Scholar 

  28. S. Castiglioni, K.V. Thomas, B. Kasprzyk-Hordern, L. Vandam, P. Griffiths, Sci. Total Environ., 2014, 487, 613.

    Article  CAS  PubMed  Google Scholar 

  29. K.V. Thomas and M.J. Reid, Environ. Sci. Technol., 2011, 45, 7611.

    Article  PubMed  Google Scholar 

  30. M.G. Cantwell, D.R. Katz, J.C. Sullivan, T. Borci, R.F. Chen, Mar. Pollut. Bull., 2016, 108, 321.

    Article  CAS  PubMed  Google Scholar 

  31. I. Senta, E. Gracia-Lor, A. Borsotti, E. Zuccato, S. Castiglioni, Water Res., 2015, 74, 23.

    Article  CAS  PubMed  Google Scholar 

  32. U. Kotowska, K. Biegañska, V. Isidorov, Polish J. Environ., 2012, 21, 129.

    CAS  Google Scholar 

  33. K. Arai, H. Terashima, S. Aizawa, A. Taga, A. Yamamoto, K. Tsutsumiuchi, S. Kodama, Anal. Sci., 2015, 31, 831.

    Article  CAS  PubMed  Google Scholar 

  34. H. Nishi and K. Nagamatsu, Anal. Sci., 2014, 30, 205.

    Article  PubMed  Google Scholar 

  35. Q. Sui, J. Huang, S.B. Deng, G. Yu, Chin. Sci. Bull., 2010, 54, 4633.

    Google Scholar 

  36. D.C. Harris, "Quantitative Chemical Analysis", 2010, W.H. Freeman, New York.

    Google Scholar 

  37. L. Tong, P. Li, Y. Wang, K. Zhu, Chemosphere, 2009, 74, 1090.

    Article  CAS  PubMed  Google Scholar 

  38. S.L. Rice and S. Mitra, Anal. Chim. Acta, 2007, 589, 125.

    Article  Google Scholar 

  39. W.M.A.W.M. Khalik, M.P. Abdullah, F.K. Baharudin, S.A. Zulkepli, J. Mater. Environ. Sci., 2016, 7, 720.

    Google Scholar 

  40. M.E. Dasenaki and N.S. Thomaidis, Anal. Bioanal. Chem., 2015, 407, 4229.

    Article  PubMed  Google Scholar 

  41. F. Gosetti, E. Mazzucco, D. Zampieri, M.C. Gennaro, J. Chromatogr. A, 2010, 1217, 3929.

    Article  CAS  PubMed  Google Scholar 

  42. K. Hájková, J. Pulkrabová, J. Schurek, J. Hajslová, J. Poustka, M. Nápravnfková, V. Kocourek, Anal. Bioanal. Chem., 2007, 387, 1351.

    Article  PubMed  Google Scholar 

  43. J. Radjenovi, A. Jeli, M. Petrovi, D. Barceló, Anal. Bioanal. Chem., 2009, 393, 1685.

    Article  Google Scholar 

  44. B. Li and T. Zhang, Chemosphere, 2011, 83, 1284.

    Article  PubMed  Google Scholar 

  45. L. Dimitra and L. Nollet, "Transformation Products of Emerging Contaminants in the Environment: Analysis, Processes, Occurrence, Effects and Risks", 2014, John Wiley and Sons, New York.

    Google Scholar 

  46. I.J. Buerge, T. Poiger, H. Buser, C. Wa, Environ. Sci. Technol., 2003, 37, 691.

    Article  CAS  PubMed  Google Scholar 

  47. B. Srdjenovic, V. Djordjevic-Milic, N. Grujic, R. Injac, Z. Lepojevic, J. Chromatogr. Sci., 2008, 46, 144.

    Article  CAS  PubMed  Google Scholar 

  48. Region-case.com, http://www.region-case.com/category/ranking/consume/consumption/, (in Japanese).

  49. S. Nicolardi, S. Herrera, M.J. Martinez Bueno, A.R. Fernandez-Alba, Anal. Methods, 2012, 4, 3364.

    Article  CAS  Google Scholar 

  50. K. Nödler, T. Licha, K. Bester, M. Sauter, J. Chromatogr. A, 2010, 1217, 6511.

    Article  PubMed  Google Scholar 

  51. A.Y.C. Lin, C.A. Lin, H.H. Tung, N.S. Chary, J. Hazard. Mater., 2010, 183, 242.

    Article  CAS  PubMed  Google Scholar 

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Authors and Affiliations

  1. Department of Environmental Engineering, Graduate School of Engineering, Kyoto University, Nishikyo, Kyoto, 615-8540, Japan

    Kai He, Yasuhiro Asada & Sadahiko Itoh

  2. Department of Environmental Health, National Institute of Public Health, Wako, Saitama, 351-0197, Japan

    Shinya Echigo

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  1. Kai He
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  2. Shinya Echigo
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  3. Yasuhiro Asada
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  4. Sadahiko Itoh
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He, K., Echigo, S., Asada, Y. et al. Determination of Caffeine and Its Metabolites in Wastewater Treatment Plants Using Solid-Phase Extraction and Liquid Chromatography–Tandem Mass Spectrometry. ANAL. SCI. 34, 349–353 (2018). https://doi.org/10.2116/analsci.34.349

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  • DOI: https://doi.org/10.2116/analsci.34.349

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