Determination of Brominated Flame Retardants in the Household Appliances by ASE-SPE-RRLC-MS/MS
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Abstract
A accelerated solvent extraction-solid phase extraction rapid resolution liquid chromatography-tandem mass spectrometry (ASE-SPE-RRLC-MS/MS) method for the determination of brominated flame retardants (HBCDs,TBBP-A)in the household appliance was developed. V(acetone)∶V(hexane)= 1∶1 as an extraction solvent and accelerated solvent extraction method were been adopted. The brominated flame retardants in sample solution were separated and enriched by solid phase extraction (SPE) on C18 column. The brominated flame retardants residue was separated by HPLC using methanol-water as the mobile phase,and was detective using electrospray ionization (ESI) on a tandem mass spectrometer in multiple reactions monitoring mode. The detection limits are 0.05—0.2 mg/kg, and the correlation coefficient is larger than 0.998. At the spiked level of 0.05—800 μg/kg, the recoveries are 87.72%—95.71%, and the relative standard deviations are in the range of 4.42% and 8.38%(n=10). This method is sensitive, recurrent and accurate. It can be used for the determination of brominated flame retardants in the household appliances,and can provide reference for the relevant national standards setting.
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