title: Liquid chromatography-negative ion atmospheric pressure photoionization tandem mass spectrometry for the determination of brominated flame retardants in environmental water and industrial effluents.
abstract: 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 R(2) 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.
authors: Department of Chemistry, "La Sapienza" University, Piazzale Aldo Moro 5, 00185 Rome, Italy.
authors: Alessandro
authors: A
authors: Bacaloni
authors: Luciano
authors: L
authors: Callipo
authors: Eleonora
authors: E
authors: Corradini
authors: Piero
authors: P
authors: Giansanti
authors: Riccardo
authors: R
authors: Gubbiotti
authors: Roberto
authors: R
authors: Samperi
authors: Aldo
authors: A
authors: Laganà
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D003102:Colloids; D005411:Flame Retardants / Q000032:analysis*; D055768:Halogenated Diphenyl Ethers / Q000032:analysis*; D006586:Hexanes; D006812:Humic Substances; D007220:Industrial Waste / Q000032:analysis*; D007558:Italy; D045483:Rivers / Q000737:chemistry*; D052616:Solid Phase Extraction; D053719:Tandem Mass Spectrometry / Q000379:methods*; D014867:Water / Q000737:chemistry; D014874:Water Pollutants, Chemical / Q000032:analysis*
chemical_list: D003102:Colloids; D005411:Flame Retardants; D055768:Halogenated Diphenyl Ethers; D006586:Hexanes; D006812:Humic Substances; D007220:Industrial Waste; D014874:Water Pollutants, Chemical; D014867:Water