气相色谱-质谱法测定土壤中6种多溴联苯醚及2种羟基代谢物

GC-MS Determination of 6 Polybrominated Diphenyl Ethers and 2 Hydroxylated Metabolites in Soil

为了证实气相色谱-质谱法测定土壤中6种常见多溴联苯醚阻燃剂(PBDEs)及2种羟基代谢物(OHPBDEs)可行,以该方法对土壤中6种常见多溴联苯醚阻燃剂(PBDEs)及2种羟基代谢物(OH-PBDEs)进行测定分析。结果表明,6种PBDEs和2种OH-PBDEs分离效果较好,色谱峰峰形较好,无拖尾和重叠;基质效应|ME|为2.2%~10.5%,说明基质干扰较低;0.001~0.020 mg/L范围内8种物质线性良好,检出限(3 S/N)为1.046~2.830μg/kg(S/N=3),加标回收率为71.7%~109.7%,相对标准偏差(n=5)为0.7%~16%。证实本文建立的测定土壤中多溴联苯醚及羟基代谢物的分析方法满足批量土壤样品检测的要求。

In order to confirm the feasibility of determination of six common polybrominated diphenyl ethers(PBDEs) as flame retardants and two of their hydroxylated metabolites(OH-PBDEs) in the soil by gas chromatography-mass spectrometry(GC-MS), six common PBDEs and two OH-PBDEs in the soil were determined by GC-MS. The results showed that six PBDEs and two OH-PBDEs are well separated with good peak shape, no tailing and no overlapping within the chromatogram. The matrix effect(%ME)is 2.2%-10.5%, indicating that the matrix interference is low. The linearity of eight substances is good in the range of 0.001-0.020 mg·L-1, the detection limit(3 S/N) is 1.046-2.830 μg/kg(S/N=3), the spiking recovery is 71.7%-109.7%, and the relative standard deviation(RSD)(n=5) is 0.7%-16%. It is concluded that this analytical method established can meet the requirements for determination of PDBEs and OHPBDEs in batches of soil samples.