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Simultaneous determination of estrogenic odorant alkylphenols, chlorophenols, and their derivatives in water using online headspace solid phase microextraction coupled with gas chromatography-mass spectrometry

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Abstract

A simple online headspace solid-phase microextraction (HS-SPME) coupled with the gas chromatography-mass spectrometry (GC-MS) method was developed for simultaneous determination of trace amounts of nine estrogenic odorant alkylphenols and chlorophenols and their derivatives in water samples. The extraction conditions of HS-SPME were optimized including fiber selection, extraction temperature, extraction time, and salt concentration. Results showed that divinylbenzene/Carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber was the most appropriate one among the three selected commercial fibers, and the optimal extraction temperature, time, and salt concentration were 70 °C, 30 min, and 0.25 g/mL, respectively. The developed method was validated and showed good linearity (R 2 > 0.989), low limit of detection (LOD, 0.002–0.5 μg/L), and excellent recoveries (76–126 %) with low relative standard deviation (RSD, 0.7–12.9 %). The developed method was finally applied to two surface water samples and some of these target compounds were detected. All these detected compounds were below their odor thresholds, except for 2,4,6-TCAS and 2,4,6-TBAS wherein their concentrations were near their odor thresholds. However, in the two surface water samples, these detected compounds contributed to a certain amount of estrogenicity, which seemed to suggest that more attention should be paid to the issue of estrogenicity rather than to the odor problem.

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Acknowledgments

This work was financially supported by The Key Program of National Natural Science of China (No. 41330639); the Program for National Natural Science Foundation of China (No. 21107025; No. 21577040; U1501234); Special funds for public welfare research and capacity building in Guangdong Province(B2153210); Science and Technology Program of Guangzhou, China (No. 201510010162); and the Fundamental Research Funds for the Central Universities (2014ZM0073) as well as the funding for water odor research (D8144320).

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Correspondence to Ze-hua Liu.

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The manuscript has not been submitted to more than one journal for simultaneous consideration. The manuscript has not been published previously (partly or in full). The manuscript is a whole study, and is not split up into several parts to increase the quantity of submissions. No data have been fabricated or manipulated (including images) to support the conclusions. The manuscript is our own work, and no data, text, or theories by others are presented unless cited. All authors know the submission, and consents were obtained before the submission.

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Yuan, Sf., Liu, Zh., Lian, HX. et al. Simultaneous determination of estrogenic odorant alkylphenols, chlorophenols, and their derivatives in water using online headspace solid phase microextraction coupled with gas chromatography-mass spectrometry. Environ Sci Pollut Res 23, 19116–19125 (2016). https://doi.org/10.1007/s11356-016-7107-1

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