Determination of polybrominated diphenyl ethers (PBDEs) using liquid chromatography coupled to negative ionisation atmospheric pressure photoionisation tandem mass spectrometry (LC-NI-APPI-MS/MS): validation and application to house dust
Fourteen tetra- to deca- PBDE congeners were separated on a C18 reversed phase LC column. PBDEs 47, 85, 99, 100, 153, 154, 183, 196, 197, 203, 206, 207, 208 and 209 were eluted using a gradient of methanol: water: toluene mobile phase system at a flow rate of 0.5 ml min.-1. 13C-BDE-47, 13C-BDE- 99, 13C-BDE-153, BDE-128 and 13C-BDE-209 were used as internal standards while 13C-BDE-100 was used as a syringe standard. Separated analytes were ionised using an APPI source equipped with a 10 eV krypton lamp and operated in negative ion mode. M-Br+Oˉ ions were monitored as precursor ions for all studied BDEs except for BDE-208, BDE-209 and 13C-BDE-209 which produced higher intensity at the C6Br5Oˉ ion cluster. Brˉ ions were monitored as fragment ions for all target compounds. Linear five point calibration curves (r2=0.996 to 0.998) were constructed for each of the studied PBDEs in range 20-5000 pg μl-1. Method detection limits ranged from 12.3 to 29.8 pg. The method was applied for determination of PBDEs in SRM 2585 and favourable results were obtained. Unlike GC methods; no thermal degradation is encountered in the analysis of higher brominated PBDEs. In addition, this method allows the use of 13C-labelled internal standards which can compensate for any instrumental fluctuations and/or any matrix-related ion suppression or enhancement that can occur in the ion source.
Mohamed Abou-Elwafa Abdallah Stuart Harrad Adrian Covaci
Division of Environmental Health and Risk Management,Public Health Building,School of Geography,Eart Division of Environmental Health and Risk Management,Public Health Building,School of Geography,Eart Toxicological Center,University of Antwerp,Universiteitsplein 1,2610 Wilrijk,Antwerp,Belgium
国际会议
北京
英文
1-6
2009-08-24（万方平台首次上网日期，不代表论文的发表时间）