鱼肉组织中多溴联苯醚的定量分析

Determination of Polybrominated Diphenyl Ethers in Fish Tissue

建立了鱼肉中多溴联苯醚（PBDEs）的检测方法及严格的质量控制和质量保证（QA／QC）措施。采用索氏抽提，凝胶渗透色谱柱、多层硅胶氧化铝柱分离净化，GC—NCI MS／SIM定量分析了鱼肉中PBDEs。在29个样品中，回收率指示物^13C—PCB141、PCB209的回收率分别为79％～105％，76％～108％。在18个样品中（6个加标空白及6个海鱼、6个淡水鱼基质加标样），除了极少几个样品BDE209的回收率大于120％，其他10种目标化合物的回收率为94％～120％。三溴-七溴联苯醚（即BDF28，47，66，100，99，85，154，153，138，183）的仪器检出限为0．19-1．00μg，十溴联苯醚（即BDE209）的仪器检出限为16．4pg。实验结果表明，除BDE209外，对其它多溴联苯醚该方法具有较低的方法检出限，较好的回收率和良好的重复性，完全适用于生物样品中多溴联苯醚的检测。

This study, with an emphasis on strict QA/QC performances, developed a method for polybrominated diphenyl ether（PBDEs） detection in fish tissue. It employed Soxhlet extraction, gel permeation chromatography column, muhilayer silica and alumina column for clean-up/fractionation to process fish tissue samples. The final extracts were analyzed for 11 PBDE congeners with GC - NCI MS in the selective ion monitoring mode. The recoveries of surrogate standards （ ^13C - PCB-141 and PCB 209） ranged from 79% to 105% and from 76% to 108% , respectively, for a total of 29 samples. In 18 spiked samples （ six blank spikes and six matrix spikes for fresh-water fish, and six for marine fish）, the recoveries of the ten target analytes were between 94% and 120% , except that the recoveries of BDE209 were larger than 120% in a few samples. The instrumental detection limit for PBDEs from trito hepta-BDEs（i, e. , BDE-28, 47, 66, 100, 99, 85, 154, 153, 138, and 183） were in the range of 0. 19 pg to 1.00 pg, and was 16.4 pg for deca-BDE（209）. Low method detection limits for the target analytes except for BDE209, satisfactory recoveries, and good reproducibility were obtained, indicating that this method was suitable for determination of PBDEs in biota samples.