环境样品中三种新型溴代阻燃剂的分析测定

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),四溴舣酚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;加标空白中日标化合物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.

DETERMINATION OF THREE NOVEL BROMINATED FLAME RETARDANTS IN ENVIRONMENTAL SAMPLES

Three novel brominated flame retardants (BFRs), decabromodiphenyl ethane (DBDPE), tetrabromobisphenol A his (2,3-dibromopropyl ether) (TBBPA-DBPE) and 1,2-his (2,4,6-tribromophenoxy) ethane (BTBPE) in soil and sediment samples, were identified and quantified. The method was based on Soxhlet extraction, muhilayer 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.