Suitability of tandem-in-time mass spectrometry for polybrominated diphenylether measurement in fish and shellfish samples: comparison with high resolution mass spectrometry.
The first part of the present study focused on the development of an alternative automated sample preparation method for the measurement of selected polybrominated diphenyl ethers (PBDEs) in fish and shellfish. A previously developed automated method has been further optimized and simplified to decrease blank levels and cost. Sorbent and solvent quantities have been significantly reduced without altering extract quality. The second part of the study consisted of comparing tandem-in-time quadrupole ion storage mass spectrometry (QISTMS/MS) to high resolution mass spectrometry (HRMS) for the isotope dilution (ID) measurement step after gas chromatography (GC) separation. Both mass spectrometric methods performed similarly in terms of accuracy but better precision was observed for HRMS. Although better sensitivity can be attained with the high resolution sector instrument, method limits of quantification (mLOQs) were very similar for both approaches as they were dependent on the procedural blanks levels. The mLOQ values ranged between 0.04 and 3.56 ng/g fat, depending on the congener. They allowed the unambiguous identification and quantification of all target analytes, except for BDE-183, in most considered fish extracts. An analytical procedure based on rapid automated sample preparation and QISTMS/MS appeared to be suitable for the measurement of PBDEs in fish and shellfish speciment under quality assurance/quality control (QA/QC) criteria.
CART, Mass Spectrometry Laboratory, University of Liège, Allée de la Chimie 3, Bat. B6c Sart-Tilman, B-4000 Liège, Belgium. Catherine.Pirard@ulg.ac.be
Catherine
C
Pirard
Edwin
E
De Pauw
Jean-François
JF
Focant
D000818:Animals; D049872:Bivalvia / Q000737:chemistry; D003060:Cod Liver Oil / Q000737:chemistry; D005399:Fishes; D005506:Food Contamination / Q000032:analysis*; D013058:Mass Spectrometry / Q000379:methods*; D010647:Phenyl Ethers / Q000032:analysis*; D011075:Polybrominated Biphenyls / Q000032:analysis*; D015203:Reproducibility of Results; D012474:Salmon; D012758:Shellfish / Q000032:analysis*; D014337:Trout
D010647:Phenyl Ethers; D011075:Polybrominated Biphenyls; D003060:Cod Liver Oil