GCMS/MS 同时测定鱼样中39 种多溴联苯醚

Determination of 39 polybrominated biphenyl ethers in fish using GCMS/MS

中文关键词:  GC-MS/MS  多溴联苯醚  分散性固相萃取  鱼  快速溶剂萃取

英文关键词:GC-MS/MS  polybrominated biphenyl ethers (PBDEs)  dispersive solid phase extraction (DSPE)  fish  accelerated solvent extraction (ASE)

中文摘要:

      目的 采用快速溶剂萃取(ASE)、系列固相萃取(SPE, 包括分散性固相萃取(DSPE)和串联SPE柱)和GCMS/MS, 建立一个便捷、高效测定鱼样中39种多溴联苯醚(PBDEs)的检测方法。方法 代表性鲈鱼样品(脂肪含量11%)经冷冻干燥后ASE提取, 然后采用DSPE去除脂肪和串联SPE柱净化, 最后采用GCMS/MS检测, 同位素内标法定量。结果 本方法的检测限(MDLs)为0.16~3.29 pg/g; 具有良好的线性范围(R2>0.998)、准确度(除BDE30为53%以外, 其他组分回收率为62%~1139%)和精密度(RSD<20%); 测定参考物质的结果均在标准值范围内, 与气相色谱磁场电场双聚焦高分辨质谱(GC/HRMS)测定结果一致。结论 本方法为鱼样中PBDEs检测提供了一个快速、简便和可靠的方法, 适用于对痕量PBDEs残留水平的食用鱼进行人体健康风险评价研究。

英文摘要:

      Objective A rapid method was developed to simultaneously determine the 39 PBDEs in fish based on the sample pretreatment of accelerated solvent extraction (ASE) and sequential solid phase extraction (including DSPE and tandem SPE cartridges) as well as chromatographic separation and detection of GC-MS/MS. Methods After frozen to dry, Weever sample (11% of fat content) was treated sequentially with ASE extraction, DSPE defatting and tandem SPE cleaning up, and consequently detected by GC-MS/MS in MRM detection mode with isotopically labelled internal standard. Results The method was validated with an MDLs range of 0.16~3.29 pg/g, and satisfactory linear dynamic range R2>0.998, and accuracy is 62%~139%, except for BDE30 with a 53% of recovery, precision is RSD<20%. A certified reference material (CRM) of fish was successfully detected with detection values in line with the certified values as well as those values provided by the gold standard method of GCHRMS. Conclusion This method is rapid, easy, and reliable, and suitable for the health risk assessment of consumed fishes with trace exposure level of part per trillion.