A new method has been developed for the simultaneous analysis of five hydroxylated polybrominated di-Ph ethers (HO-PBDEs) in human serum using ultra performance liquid chromatography-electrospray ion source tandem mass spectrometry (UPLC-ESI-MS-MS) in negative ion mode. The serum samples were spiked with 13C12 Tetrabromobisphenol-A (TBBP-A) as surrogate internal standard before extracting, then the samples were further cleaned up and concentrated. Detection was performed by multiple reaction monitoring (MRM) mode in three channels, 555 f 431, 501 f 81 and 579 f 79. The recovery of spiked 13C12 TBBP-A and five HO-PBDE congeners in blank samples was from (76.2 (14)% to (97.8 ( 5.7), the limit of qualification (LOQ) were between 1.0 and 2.0 ng/g.lipid. 5-HO-2,2′,4,4′ tetrabromodiphenyl ether (5-HO-BDE-47), 6-HO-2,2′,4,4′ tetrabromodiphenyl ether (6-HOBDE-47), 5′-HO-2,2′,4,4′,5 pentabromodiphenyl ether (5′-HOBDE-99), 6′-HO-2,2′,4,4′,5 pentabromodiphenyl ether (6′-HOBDE-99) had been HO-PBDEs ranged from no(detected and the concentration of detection to 18.9 ng/g.lipid in six serum samples from volunteers living around PBDEs manufactory. 6-HO-BDE-47 was the most abundant HO-PBDEs congener accounting for 48.7% to 100.0% of total HO-PBDEs in each sample. The proposed method based on UPLC-MS-MS has been applied to directly det. HOPBDEs in human serum without derivatisation.
Authors: Wang, Ying; Ding, Wen-Wei; Jin, Jun ;Full Source: Fenxi Huaxue 2011, 39(1), 22-26 (Ch) ;