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固相盘萃取法测定低纳克/升浓度水中的多卤化咔唑。

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

机构信息

Key Laboratory of Sustainable Utilization of Technology Research for Fisheries Resources of Zhejiang Province, Zhejiang Marine Fisheries Research Institute, Zhoushan, P. R. China.

Key Laboratory of Microbial Technology for Industrial Pollution Control of Zhejiang Province, College of Environment, Zhejiang University of Technology, Hangzhou, P. R. China.

出版信息

J Sep Sci. 2021 Oct;44(20):3840-3848. doi: 10.1002/jssc.202100493. Epub 2021 Aug 19.

Abstract

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 × 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.

摘要

多卤代咔唑是一类具有持久性和类二恶英毒性的新兴污染物,近年来受到了越来越多的关注。本研究建立了一种基于固相圆盘萃取和气相色谱-质谱联用的测定水中痕量多卤代咔唑的简单、快速、灵敏和高通量方法。对固相圆盘萃取方法进行了初步优化,确定了最佳实验条件为:pH 值为 6-9 的 1 L 水样以 5-50 mL/min 的流速用 Empore 3-stn 十八烷基圆盘萃取和富集,然后用 5 mL 丙酮和 3×10 mL 二氯甲烷洗脱。该方法对于咔唑和 11 种多卤代咔唑的线性范围为 0.2-50ng/L,相关系数范围为 0.9951-0.9996。检出限在纳克每升水平,范围为 0.018-0.12ng/L。最后,该优化方法用于测定自来水中痕量的咔唑和 11 种多卤代咔唑以及海水中的这些物质,回收率为 86.6-112.8%。在自来水中和海水中均检测到了咔唑和 3-7 种多卤代咔唑,3,6-二氯咔唑是这两种水样中的主要同系物。

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