摘要:
采用索氏抽提、多层硅胶氧化铝柱分离净化和气相色谱质谱联用仪(GC-EI-MS和GC-ECNI-MS)分别对沉积物及土壤样品中的十溴二苯基乙烷(DBDPE),四溴双酚A双(2,3-二溴烯丙基)醚(TBBPA-DB-PE),1,2-双(2,4,6-三溴苯氧基)乙烷(BTBPE)3种新型溴代阻燃剂进行了定性和定量分析,并建立了环境样品中这3种新型溴代阻燃剂的检测方法.在3个流程空白中,所有目标物都低于检出限;加标空白中目标化合物DBDPE,TBBPA-DBPE,BTBPE的回收率分别为74.8%—82.5%,88.9%—100.7%,86.7%—102.3%.方法检出限分别为1ng·g-1,0.4ng·g-1和0.1ng·g-1.DBDPE,TBBPA-DBPE,BTBPE在沉积物和土壤样品中测定结果的相对标准偏差分别为16.29%,0.045%,0.051%.方法具有较低的方法检出限,较好的回收率和重复性,适用于一般环境样品中新型溴代阻燃剂的分析和检测.
Abstract:
Three novel brominated flame retardants(BFRs),decabromodiphenyl ethane(DBDPE),tetrabromobisphenol A bis(2,3-dibromopropyl ether)(TBBPA-DBPE)and 1,2-bis(2,4,6-tribromophenoxy)ethane(BTBPE)in soil and sediment samples,were identified and quantified.The method was based on Soxhlet extraction,multilayer silica and alumina column for clean-up,and subsequent analysis by GC-MS using both electron ionization(EI)and electron capture negative ionization(ECNI)modes.The target compounds were under the limit of detection in the procedural blanks and their recoveries were in the range of 74.8%—82.5%,88.9%—100.7% and 86.7%—102.3% for DBDPE,TBBPA-DBPE,and BTBPE in the spike blanks,respectively.The average relative standard deviations(RSD)for the repeatability of analysis of soil and sediment samples were 16.29%,0.045% and 0.051% for DBDPE,TBBPA-DBPE and BTBPE,respectively.Our results showed that the methods we adopted were certified for the analysis of the emerging novel BFRs in the environment.
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