超高效液相色谱-串联质谱法同时检测溴代阻燃剂  

Simultaneous Analysis of Tetrabromobisphenol A,Tris-(2,3-dibromopropyl) Isocyanurate and Hexabromocyclododecanes Using Ultra Performance Liquid Chromatography-Mass Spectrometry

作　　者：应红梅[1] 朱丽波[1] 徐能斌[1] 冯加永[1] 钱飞中[1] 陈钟佺[1] 汪晟乐[1] 

机构地区：[1]宁波市环境监测中心,浙江宁波315012

出　　处：《中国环境监测》2013年第4期94-98,共5页Environmental Monitoring in China

基　　金：国家环保公益性行业科研专项(201209016);宁波市自然科学基金项目(2011A610087;201201A6107004)

摘　　要：采用Acquity BEH C18色谱柱,以甲醇-乙腈混合液和水为流动相,辅以电喷雾正离子模式多反应监测(MRM)进行定性定量分析,建立了一种同位素稀释超高效液相色谱-串联质谱(UPLC-MS/MS)同时检测四溴双酚A(TBBPA)、三-(2,3-二溴丙基)异氰脲酸酯(TBC)和3种六溴环十二烷(HBCD)异构体的方法。水样通过固相萃取进行净化,回收率达到85.3%～96.1%。土壤和底泥样品经加速溶剂萃取后,采用酸性硅胶和中性硅胶柱进行净化,回收率达到81.5%～102.7%。该方法对TBBPA、TBC、α-HBCD、β-HBCD、γ-HBCD在水和土壤中的检测限分别为1.0、1.2、2.0、0.8、1.2 ng/L和0.10、0.12、0.20、0.08、0.12 ng/g。A sensitive and selective method was developed for simultaneous analysis tetrabromohisphenol A （TBBPA） , tris-（2,3- dibromopropyl） isocyanurate （TBC） and hexahromocyclododeeanes （HBCD） in water, soil and sediment samples. The method included an Acquity BEH C18 column separation operated with a gradient elution solvent of methanol-acetonitrile and water coupled to a mass Spectrometry scanned in multiple reaction monitoring （MRM） mode and isotope dilution. Water samples were extracted and cleaned-up by solid phase extraction. The recoveries were in the range of 85.3%-96.1%. Soil and sediment samples were extracted using accelerated solvent extraction （ASE） , and further purified using acidic silica treatment and solid phase extraction with an activated silica gel column. The recoveries in soil and sediment samples were 81.5% -102.7%. Limits of detection of TBBPA, TBC, α-HBCD,β-HBCD, γ-HBCD were 1.0, 1.2, 2. 0, 0.8, 1.2 ng/L in water samples and 0.10, 0.12, 0.20, 0.08, 0.12 ng/g in soil and sediment samples, respectively.

关 键 词：溴代阻燃剂 四溴双酚A 三-（2 3-二溴丙基）异氰脲酸酯 六溴环十二烷 超高效液相色谱-质谱法 同位素稀释法 

分 类 号：X830.2[环境科学与工程—环境工程]