Determination of polyhalogenated carbazoles in waters at low nanogram-per-liter concentrations with solid-phase disk extraction

Polyhalogenated carbazoles, a class of emerging contaminants with persistence and dioxin-like toxicity, have received increasing attention in recent years. In this study, a simple, rapid, sensitive, and high throughput method based on solid-phase disk extraction and gas chromatography-mass spectrometry was described for the determination of polyhalogenated carbazoles in low nanogram-per-liter range in water samples. The proposed solid-phase disk extraction method was initially optimized, and the optimum experimental conditions found were 1 L water sample (pH 6-9) extracted and enriched by Empore 3-stn octadecyl disk at flow rate of 5 to 50 mL/min and eluted by 5 mL of acetone and 3 x 10 mL methylene dichloride. The linearity of the method ranged from 0.2 to 50 ng/L for carbazole and 11 polyhalogenated carbazoles, with correlation coefficients ranging from 0.9951 to 0.9996. The limits of detection were in the low nanogram per liter level, ranging from 0.018 to 0.12 ng/L. Finally, the optimized method was applied for determining trace levels of carbazole and 11 polyhalogenated carbazoles in tap water and seawater samples with good recovery of 86.6-112.8%. Carbazole and 3-7 polyhalogenated carbazoles were detected, and 3,6-dichlorocarbazole was the predominant congener both in tap water and seawater.

Automated summary

A high throughput method based on solid-phase disk extraction and gas chromatography-mass spectrometry was developed for the determination of polyhalogenated carbazoles in water samples, with good linearity and low limits of detection. The optimized method showed good recovery rates for carbazole and 11 polyhalogenated carbazoles in tap water and seawater samples. Carbazole and 3-7 polyhalogenated carbazoles were detected, with 3,6-dichlorocarbazole being the predominant congener in both tap water and seawater.