固相萃取净化-气相色谱-负化学源质谱法测定近岸海洋环境中的甲氧基多溴联苯醚

甲氧基多溴联苯醚（methoxypolybrominated diphenyl ethers， MeO-PBDEs）广泛存在于生物体和海洋环境。以象山海域的生物体和沉积物为样本，采用固相萃取净化-气相色谱-负化学源质谱法，检测了6种MeO-PBDEs，结果显示，当目标分析物浓度为0.1~20.0 μg?L^-1时，线性关系良好（R²>0.999），检出限为0.13~0.22 μg?kg^-1，定量限为0.42~0.72 μg?kg^-1，实际样品的平均回收率为71.2%~116.2%。MeO-PBDEs的分布状况调查结果显示，藻类样品中仅检出6-MeO-BDE-47，且浓度较低，其他生物体中检出3种MeO-PBDEs，检出率为31.3%，浓度为0.21~2.72 μg?kg^-1。沉积物中无MeO-PBDEs被检出。

Determination of methoxypolybrominated diphenyl ethers in the coastal marine environment using solid-phase extraction and gas chromatography coupled with negative chemical ionization mass spectrometry

Methoxypolybrominated diphenyl ethers (MeO-PBDEs) were widely present in marine organisms and the marine environment. An analytical method of six methoxypolybrominated diphenyl ethers for biological samples and sediment samples from Xiangshan Sea area using solid-phase extraction and gas chromatography coupled with negative chemical ionization mass spectrometry was developed and optimized. The developed method exhibited satisfying linearity in the range of 0.1-20.0 μg?L^-1 (R² >0.999). The detection limit (LOD) and limit of quantitation (LOQ) for MeO-PBDEs were 0.13-0.22 μg?kg^-1 and 0.42-0.72 μg?kg^-1 respectively. The spiked recovery was 71.2%-116.2%. The method was applied to the analysis of marine organisms and sediments collected from Xiangshan sea area. All kinds of MeO-PBDEs were not detected in sediment samples. Only 6-MeO-BDE-47 was detected in algae samples with low concentration. Three MeO-PBDEs were detected in other biological samples, and the ratio of detection was 31.3% with a concentration range of 0.21-2.72 μg?kg^-1 MeO-PBDEs were not detected in sediment samples.