Determination of eleven polyhalogenated carbazoles in drinking water by solid-phase extraction-gas chromatography-mass spectrometry
WEI Yuan1, DIAO Yongqing2, HU Jielan2, LI Yuxin2, YU Xi2, WANG Xia1
1. School of Public Health, Fudan University, Shanghai 200032, China; 2. Qingpu District Center for Disease Control and Prevention, Shanghai 201799, China
Abstract：Objective To establish a method for the determination of 11 polyhalogenated carbazoles in drinking water by solid-phase extraction coupled with gas chromatography-mass spectrometry, so as to provide technical reference for monitoring such pollutants in aquatic environments. Methods The temperature programming conditions of chromatography and the eluent for solid-phase extraction were optimized to improve the separation efficiency of target compounds and reduce matrix interference. A total of 1 L finished water sample from a waterworks was collected, enriched and concentrated using a HC-C18 solid-phase extraction cartridge, eluted with dichloromethane, quantitatively analyzed under the selected ion monitoring mode of gas chromatography-mass spectrometry, and corrected using surrogate standards. Working curves of 11 polyhalogenated carbazoles were established, and the limits of detection, limits of quantification, average spiked recovery rates and relative standard deviation (RSD) were calculated. Results Under the optimized conditions, the analysis results of 11 polyhalogenated carbazoles and surrogate standards showed that all target compounds exhibited symmetrical peak shapes, low matrix interference and good resolution, meeting the requirements of quantitative and qualitative analysis. The 11 polyhalogenated carbazoles showed good linear relationships in the range of 0.1-5.0 ng/L, with all correlation coefficients ≥0.999 4. The limits of detection ranged from 0.02 to 0.08 ng/L, and the limits of quantification ranged from 0.04 to 0.25 ng/L. At spiked concentrations of 0.1, 0.2 and 1.0 ng/L, the average spiked recovery rates were 89.1%-107.6%, 97.8%-100.5% and 92.6%-100.4%, respectively, with RSD of 2.9%-9.2%, 1.0%-3.4% and 0.8%-3.1%, respectively. Conclusion The method based on solid-phase extraction-gas chromatography-mass spectrometry for the determination of 11 polyhalogenated carbazoles in drinking water demonstrates good accuracy and precision, and can be applied to the detection of polyhalogenated carbazoles in drinking water.
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