Liquid chromatography–negative ion atmospheric pressure photoionization tandem mass spectrometry for the determination of brominated flame retardants in environmental water and industrial efflu

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• 作者：Aless ; ro Bacaloni ; Luciano Callipo ; Eleonora Corradini ; Piero Giansanti ; Riccardo Gubbiotti ; Roberto Samperi ; Aldo Laganà
• 关键词：Brominated flame retardants ; LC– ; MS ; Atmospheric pressure photoionization ; Water analysis ; Solid-phase extraction ; Liquid– ; liquid extraction
• 刊名：Journal of Chromatography A
• 出版年：2009
• 出版时间：4 September 2009
• 年：2009
• 卷：1216
• 期：36
• 页码：6400-6409
• 全文大小：642 K

文摘

We describe the development of a liquid chromatography with negative-ion atmospheric pressure photoionization tandem mass spectrometric (LC/NI-APPI/MS/MS) method for the simultaneous determination of tetrabromobisphenol A (TBBP-A) and five polybrominated diphenyl ethers (BDE-47, BDE-99, BDE-100, BDE-153 and BDE-154) in water. A mobile phase methanol/acetone/water was used, where acetone acts also as dopant. NI-APPI produced precursor ions corresponding to [M−H]⁻ for TBBP-A, [M−Br+O]⁻, and [M−2Br+O]⁻ for the BDE congeners studied. Each compound was quantified operating in multiple reaction monitoring mode. Linearity was observed in the range 0.025–10 ng injected for all compounds. Coefficients of determination R² ranged from 0.9934 to 0.9982. BDEs were poorly retained by solid-phase extraction (SPE) from river water and sewage treatment plant effluent, thus liquid–liquid extraction (LLE) by n-hexane should be used for these samples. The recoveries of TBBP-A and PBDEs from tap water (SPE), river water and industrial wastewater (LLE) were in the range of 81–88 % , 78–92 % , and 43–99 % , respectively, with relative standard deviations below 17 % . The limits of detection, based on signal-to-noise ratio of 3, ranged from 0.004 to 0.1 ng injected, and method quantification limits were 0.2–3.3 ng L⁻¹ but BDE47 (20.3 ng L⁻¹). Only TBBP-A was found in a treated industrial sewage at 4 ng L⁻¹, while BDE-99 and BDE-100 were detected on suspended solids.