A new method has been developed for the simultaneous analysis of five hydroxylated polybrominated diphenyl 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 C12 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→431, 501→81 and 579→79. The recovery of spiked 13C12TBBP-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-HO-BDE-47), 5'-HO-2,2’, 4,4’, 5-pentabromodiphenyl ether (5'-HO-BDE99), 6'-HO-2, 2', 4,4', 5-pentabromodiphenyl ether (6'-HO-BDE-99) had been detected and the concentration of ∑ HO-PBDEs ranged from no 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 UPIC-MS-MS has been applied to directly determine HO-PBDEs in human serum without derivatization.%建立了超高效液相色谱-电喷雾离子源串联三重四极杆质谱(UPLC-ESI-MS-MS)在负离子模式下测定人血中5种羟基多溴联苯醚(HO-PBDEs)的方法.血清样品中加入替代内标13C<,12四溴双酚-A(13C<,12TBBP-A),经萃取、净化、浓缩等预处理过程,多重反应监测(MRM),扫描通道为:m/z 555→431,501→81,579→79;内标法定量.方法回收率为(76.25214)%～(97.8±5.7)%,检出限(LOQ)为1.0～2.0ng/g·脂肪.应用本方法对人血样品进行测定,检出 5-HO-BDE-47,6-HO BDE-47,5'-HO BDE-99,6'-HO BDE-99;∑HO-PBDEs浓度范围为未检出至19 ng/g(脂肪中),其中6-HO-BDE-47含量最高,占HO-PBDEs总量的48.7%～100%.
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