Determination of hexabromocyclododecane isomers in sewage sludge by LC-MS/MS
A method has been developed to determine α, β and γ diastereoisomers of hexabromocyclododecane (HBCD), a brominated flame retardant, in sewage sludge, based on the ultrasonic-assisted extraction (UAE) of samples with dichloromethane-ACN (11) and the subsequent clean-up of extracts by dispersive solid phase extraction with primary-secondary amine. Levels of HBCD diastereoisomers were determined by LC coupled with ESI MS/MS. Evaluation of the matrix effect showed a high ion suppression for all the diastereoisomers studied, which was counteracted by using a mixture of labelled HBCD diastereoisomers as internal standards. This method yielded recoveries in the range of 79.6-112.5% with SDs equal or lower than 9.1 The limits of detection were 0.3 ng/g for α-and β-HBCD and 0.2 ng/g for γ-HBCD. The developed method was successfully applied to 19 sludge samples collected from the province of Madrid (Spain). In most of the samples, β-HBCD was below the method detection limit, whereas α- and γ-HBCD were quantified in all of the sludge samples, and γ-HBCD was the predominant diastereoisomer in 63% of the analyzed samples and α-HBCD predominated in the rest.
| Main Authors: | , |
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| Format: | journal article biblioteca |
| Language: | English |
| Published: |
Wiley
2009
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| Subjects: | Dispersive solid phase extraction, Hexabromocyclododecane, LCMS, MS, Sludge, Ultrasonic-assisted extraction, |
| Online Access: | http://hdl.handle.net/20.500.12792/1640 http://hdl.handle.net/10261/293427 |
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