An atmospheric pressure gas chromatography-tandem mass spectrometry（APGC-MS/MS） method was established to simultaneously determine 8 types of polybrominated diphenyl ethers（PBDEs） and 9 types of novel brominated flame retardants（NBFRs）. Serum sample of 0.3 g was pretreated with HLB column solid-phase extraction and acidic silica gel column purification，and separated by DB-5HT capillary column（15 m×0.25 mm×0.10 μm）. PBDEs and NBFRs was quantitatively analyzed by APGC-MS/MS. The detection of PBDEs is using isotope dilution method，and the detection of NBFRs is using the internal standard method. This method was further validated using international serum standard reference material sample SRM 1958. Compared with the reference mass fraction range provided by SRM 1958，the measured concentrations of PBDEs were within the reference mass fraction range，with a relative standard deviation（RSD，

n

=6） of 6.1% to 18%. The low，medium，and high concentrations of NBFRs were added to the matrix for validation. The recoveries of matrix spiking ranged from 81.7% to 126%. The RSDs were between 6.2% and 18%. This method has high sensitivity and accuracy，stable performance，which meets the requirements for the determination of PBDEs and NBFRs in human serum and the method can be applied to human health risk assessment for PBDEs and NBFRs.