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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(D-SPE)和串联SPE柱]和GC-MS/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D-SPE去除脂肪和串联SPE柱净化,最后采用GC-MS/MS检测,同位素内标法定量。结果本方法的检测限(MDLs)为0.16～3.29pg/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%～139%)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,以便于日常监测和评估鱼中残留PBDEs对人体健康风险的研究。
OBJECTIVE To establish a convenient and efficient method for the determination of 39 kinds of fish samples using rapid solvent extraction (ASE), series of solid-phase extraction [SPE, including dispersive solid phase extraction (SPE) and tandem SPE] and GC- Polybrominated diphenyl ethers (PBDEs) detection methods. Methods Representative sea bass samples (11% fat content) were freeze-dried and extracted with ASE. Then fat was removed by D-SPE and cleaned up by serial SPE column. Finally, GC-MS / MS and isotope internal standard were used for quantification. Results The detection limits (MDLs) of this method ranged from 0.16 to 3.29 pg / g with good linearity (R2> 0.998) and accuracy (62% ~ 139% recovery of other components except for BDE30 of 53% And precision (RSD <20%). The results of determination of reference materials were all within the standard values, which were consistent with the results of gas chromatography-field double-resolution high resolution mass spectrometry (GC-HRMS) Conclusion This method provides a quick, easy and reliable method for the detection of PBDEs in fish in order to facilitate the routine monitoring and assessment of the human health risks of residual PBDEs in fish.