LC-ESI-MS-MS method for the analysis of tetrabromobisphenol A in sediment and sewage sludge

Abstract

Tetrabromobisphenol A (4,4'-isopropylidenebis(2,6-dibromophenol), TBBPA) is the most widely used brominated flame retardant in the world. Due to its low water solubility TBBPA released in aquatic ecosystems ultimately accumulates in sediments, but the lack of data on its environmental level and temporal trend in sediment cores precludes establishing if the input of TBBPA is an on-going environmental problem. We developed an analytical method involving HPLC-ESI-MS-MS (ion trap) with detection of the negative pseudo-molecular ion of TBBPA and its fragmentation pattern. Recovery of TBBPA from spiked marine sediment (both lyophilized and wet) and dehydrated sewage sludge was better than 95%. The current detection limit of TBBPA is 60 pg injected and the linearity of the response is at least three orders of magnitude, ranging from 7 ng ml(-1) to 7000 ng ml(-1). The method was also applied to the analysis of urban sewage sludge where TBBPA was detected at a concentration of 300 ng g(-1)(dry weight). With an analysis time of less than 20 min, this method is adequate for a rapid re-assessment of archived sediment samples avoiding cumbersome derivatization procedures.

Identification of Tetrabromobisphenol A Allyl Ether and Tetrabromobisphenol A 2,3-Dibromopropyl Ether in the Ambient Environment near a Manufacturing Site and in Mollusks at a Coastal Region

“…The full-scan mass spectrum (m/z 450−800) of TBBPA AE using HPLC−Q-TOF-MS can be seen in Figure 1A , which is similar to ionization of TBBPA under ESI mode. 24,25 The other lesser ion fragments cannot be explained by TBBPA AE or TBBPA DBPE but might be due to the ionization of minor impurities. The results show that the two target chemicals were wellidentified using NMR, HPLC−UV, and Q-TOF-MS.…”

Rapid determination of tetrabromobisphenol A and its main derivatives in aqueous samples by ultrasound-dispersive liquid–liquid microextraction combined with high-performance liquid chromatography

“…The optimized US-DLLME method was compared with other methods for extracting and measuring of TBBPA in water (Table 2). Almost all papers have described methods that are only capable of detecting and quantifying TBBPA or one to two derivatives [11][12][13][14]25,26]. TBBPA and five derivatives were simultaneously determined in this work only.…”

Determination of Hexabromocyclododecane Diastereoisomers and Tetrabromobisphenol A in Water and Sediment by Liquid Chromatography/Mass Spectrometry

“…Lack of a reliable measurement method could be one of the reasons. Methods for determining TBBPA in water and sediment were readily developed, 12,13 and HBCD could be measured as the total of the three diastereoisomers (α, β, and γ) by gas chromatography/mass spectrometry (GC/MS). 14,15 However, it is necessary to be able to determine the HBCD diastereoisomers separately because the proportions of the three isomers reportedly varied with types of samples, sites and products.…”

“…PBDE congeners, of which the maximum theoretical number is 209, have been congener-specifically determined by GC/MS with exact mass measurement or with chemical ionization. [3][4][5][6][7][8] Less is known about the environmental distribution of TBBPA and HBCD; [9][10][11][12][13] in particular, it is not known why the reported abundance ratios of HBCD diastereoisomers were different for different samples, sites and environmental media. Lack of a reliable measurement method could be one of the reasons.…”