Determination of Triclocarban, Triclosan and Methyl-Triclosan in Environmental Water by Silicon Dioxide/Polystyrene Composite Microspheres Solid-Phase Extraction Combined with HPLC-ESI-MS


This paper developed a sensitive and efficient analytical method for triclocarban (TCC), triclosan (TCS) and Methyl-triclosan (MTCS) determination in environmental water, which involves enrichment by using silicon dioxide/polystyrene composite microspheres solid-phase extraction and detection with HPLC-ESI-MS. The influence of several operational parameters, including the eluant and its volume, the flow rate and acidity of water sample were investigated and optimized. Under the optimum conditions, the limits of detection were 1.0 ng/L, 2.5 and 4.5 ng/L for TCC, TCS, and MTCS, respectively. The linearity of the method was observed in the range of 5-2000 ng/L, with correlation coefficients (r2) >.99. The spiked recoveries of TCC, TCS and MTCS in water sampleswereachieved in the range of 89.5% -96.8% with RSD below 5.7%. The proposed method has been successfully applied to analyze real water samples and satisfactory results were achieved.

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Wang, Y. , Li, P. , Liu, Y. , Chen, B. , Li, J. and Wang, X. (2013) Determination of Triclocarban, Triclosan and Methyl-Triclosan in Environmental Water by Silicon Dioxide/Polystyrene Composite Microspheres Solid-Phase Extraction Combined with HPLC-ESI-MS. Journal of Geoscience and Environment Protection, 1, 13-17. doi: 10.4236/gep.2013.12003.

Conflicts of Interest

The authors declare no conflicts of interest.


[1] Ahn, K. C., Zhao, B., Chen, J., Cheredenichenko, G., Sanmarti, E., & Denision, M. S. (2008). In vitro bio-logical activities of the antimicrobials triclocarban, its analogues, and triclosan in bioassay screens: Receptorbased bioassay screens. Environmental Health Perspectives, 116, 1203-1210.
[2] Boehmer, W., Ruedel, H., Wenzel, A., & Schroeter-Kermani, C. (2004). Retrospective monitoring of triclosan and methyl-triclosan in fish: Results from the German environmental specimen bank. Organohalogen Compounds, 66, 1516-1521.
[3] Canosa, P., Pérez-Palacios, D., Garrido-López, A., Tena, T. M., Rodríguez, I., Rubi, E., & Cela, R. (2007). Pressurized liquid extraction with in-cell clean-up followed by gas chromatography-tandem mass spectrometry for the selective determination of parabens and triclosan in indoor dust. Journal of Chromatography A, 1161, 105-112.
[4] Chalew, T. E. A., & Halden, R. U. (2009). Environmental exposure of aquatic and terrestrial biota to triclosan and triclocarban. The Journal of the American Water Resources Association, 45, 4-13.
[5] Coogan, M. A., Edziyie, R. E., La Point, T. W., & Venable, B. J. (2007). Algal bioaccumulation of triclocarban, triclosan, and methyl-triclosan in a North Texas wastewater treatment plant receiving stream. Chemosphere, 67, 1911-1918.
[6] Coogan, M. A., & La Point, T. W. (2008). Snail bioaccumulation of triclocarban, triclosan, and methyltriclosan in a north texas, USA, stream affected by wastewater treatment plant runoff. Environmental Toxicology and Chemistry, 27, 1788-1793.
[7] Chu, S., & Metcalfe, C. D. (2007). Simultaneous determination of triclocarban and triclosan in municipal biosolids by liquid chromatography tandem mass spectrometry. Journal of Chromatography A, 1164, 212-218.
[8] Guo, J. H., Li, X. H., Cao, X. L., Li, Y., Wang, X. Z., & Xu, X. B. (2009). Determination of triclosan, triclocarban and methyl-triclosan in aqueous samples by dispersive liquid-liquid microextraction combined with rapid liquid chromatography. Journal of Chromatography A, 1216, 3038-3043.
[9] Halden, R. U., & Paull, D. H. (2004). Analysis of triclocarban in aquatic samples by liquid chromatography electrospray ionization mass spectrometry. Environmental Science and Technology, 38, 4849- 4855.
[10] Halden, R. U., & Paull, D. H. (2005). Co-occurrence of triclocarban and triclosan in US water resources. Environmental Science and Technology, 39, 1420-142.
[11] Hinther, A., Bromba, C. M., Wulff, J. E., & Helbing, C. C. (2011). Effects of triclocarban, triclosan, and methyl triclosan on thyroid hormone action and stress in frog and mammalian culture systems. Environmental Science and Technology, 45, 5395-5402.
[12] Kawaguchi, M., Ito, R., Honda, H., Endo, N., Okanouchi, N., Saito, K., Seto, Y., & Nakazawa, H. (2008). Stir bar sorptive extraction and thermal desorption-gas chromatography-mass spectrometry for trace analysis of triclosan in water sample. Journal of Chromatography A, 1206, 196-199.
[13] Liska, I., Krupcik, J., & Leclercp, P. A. (1989). The use of solid sorbents for direct accumulation of organic compounds from water matrices-a review of solid-phase extraction techniques. Journal of High Resolution Chromatography, 12, 577-590.
[14] Melwanki, M. B., & Fuh, M. R. (2008). Dispersive liquid-liquid micro- extraction combined with semi-automated in-syringe back extraction as a new approach for the sample preparation of ionizable organic compounds prior to liquid chromatography. Journal of Chromatography A, 1198, 1-6.
[15] Mezcua, M., Gomez, M. J., Ferrer, I., Aguera, A., Hernando, M. D., & Fernandez-Alba, A. R. (2004). Evidence of 2,7/2,8-dibenzodichloro- p-dioxin as a photodegradation product of triclosan in water and wastewater sam-ples. Analytica Chimica Acta, 524, 241-247.
[16] Montes, R., Rodríguez, I., Rubí, E., & Cela, R. (2005). Optimization of solid-phase microextraction conditions for the determination of triclosan and possible related compounds in water samples. Journal of Chromatography A, 1072, 107-115.
[17] Orvos, D. R., Versteeg, D. J., Inauen, J., Capdeveille, M., Rothenstein A., & Cunningham, V. (2002). Aquatic toxicity of triclosan. Environmental Toxicology and Chemistry, 21, 1338-1349.
[18] Ponte, C., Richard, J., Bonte, C., Lequien, P., & Lacombe, A. (1974). Methemoglobinemia in Newborn-Discussion of Etiological Role of Trichlorocarbanilide. Semaine Des Hopitaux, 50, 359-365.
[19] Sapkota, A., Heidler, J., & Halden, R. U. (2007). Detection of triclocarban and two co-contaminating chlorocarbanilides in US aquatic environments using isotope dilution liquid chromatography tandem mass spectrometry. Environmental Research, 103, 21-29.
[20] Shen, J. Y., Chang, M. S., Yang, S. H., & Wu, G. J. (2012). Simultaneous determination of triclosan, triclocarban, and transformation products of triclocarban in aqueous samples using solid-phase micro-extraction-HPLC-MS/MS. Journal of Separation Science, 35, 2544-2552.
[21] Shen, S. C., Bi, J. N., Sui, L. L., & Liu, Y. H, (2012). Preparation of SiO2/PS composite microsphere and its application as solid-phase extraction sorbent. Chinese Journal of Analysis Laboratory, 31, 51-54.
[22] Sun, J., Yi, C. L., Zhao, R. S., Wang, X., Jiang, W. Q., & Wang, X. K. (2012). Determination of trace triclosan in environmental water by microporous bamboo-activated charcoal solid-phase extraction combined with HPLC-ESI-MS. Journal of Separation Science, 35, 2781- 2786.
[23] Zhao, R., Cheng, C., Yuan, J., Jiang, T., Wang, X., & Lin, J. (2007). Sensitive measurement of ultratrace phenols in natural water by purge-and-trap with in situ acetylation coupled with gas chromatography-mass spectrometry. Analytical and Bioanalytical Chemistry, 387, 687-694.
[24] Zhao, R. S., Wang, X., Sun, J., Hu, C., & Wang, X. K. (2011). Determination of triclosan and triclocarban in environmental water samples with ionic liquid/ionic liquid dispersive liquid-liquid micro-extraction prior to HPLC-ESI-MS/MS. Microchimica Acta, 174, 145-151.

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