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CASE
Determination of Hexabromocyclododecanes in Marine Organisms by High Performance Liquid Chromatography － Tandem Mass Spectrometry Coupled with LC － Si
Key words: solid phase extraction ( SPE) ; UPLC － MS /MS; marine organisms; hexabromocyclododecanes(HBCDs)
Details
Abstract: A method was developed for the determination of hexabromocyclododecanes( HBCDs) in
marine organisms by high performance liquid chromatography － tandem mass spectrometry( HPLC －MS /MS) coupled with LC － Si SPE clean-up． The samples were extracted with n-hexane cleanedup by LC － Si SPE，and analyzed by LC － MS /MS． The major parameters affecting LC － Si SPE eluting conditions were also investigated． The chromatographic separation was performed on an ACQUITY UPLC BEH C18 column by gradient elution with water and methanol － acetonitrile solution( methanol∶ acetonitrile = 4 ∶ 6) as mobile phase． The detection of analyte was carried out by electrospraymass spectrometry in negative ionization under multiple reaction monitoring mode，and the internalstandard method was used for quantification． There existed good linear relationships for HBCDs in therange of 0. 50 － 100. 0 μg /L with correlation coefficients( r2 ) more than 0. 995． The quantitation limitsof the method were 0. 20 μg /kg． The recoveries for HBCDs were in the range of 85. 6% －97. 3%，with relative standard deviations of 3. 9% － 8. 8%． Therefore，the method could be applied in the identification and quantitation of HBCDs in marine organisms with low matrix interference and good reproducibility．
marine organisms by high performance liquid chromatography － tandem mass spectrometry( HPLC －MS /MS) coupled with LC － Si SPE clean-up． The samples were extracted with n-hexane cleanedup by LC － Si SPE，and analyzed by LC － MS /MS． The major parameters affecting LC － Si SPE eluting conditions were also investigated． The chromatographic separation was performed on an ACQUITY UPLC BEH C18 column by gradient elution with water and methanol － acetonitrile solution( methanol∶ acetonitrile = 4 ∶ 6) as mobile phase． The detection of analyte was carried out by electrospraymass spectrometry in negative ionization under multiple reaction monitoring mode，and the internalstandard method was used for quantification． There existed good linear relationships for HBCDs in therange of 0. 50 － 100. 0 μg /L with correlation coefficients( r2 ) more than 0. 995． The quantitation limitsof the method were 0. 20 μg /kg． The recoveries for HBCDs were in the range of 85. 6% －97. 3%，with relative standard deviations of 3. 9% － 8. 8%． Therefore，the method could be applied in the identification and quantitation of HBCDs in marine organisms with low matrix interference and good reproducibility．
