高效液相色谱-串联质谱法同时测定农田土壤中的六溴环十二烷和四溴双酚A  

Determination of Hexabromocyclododecanes and Tetrabromobisphenol A in Farmland Soils by High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：王晓春[1,2] 陶静[1] 李铁纯[1] 

机构地区：[1]鞍山师范学院化学与生命科学学院,辽宁鞍山114016 [2]国家地质实验测试中心,北京100037

出　　处：《分析测试学报》2016年第11期1440-1444,共5页Journal of Instrumental Analysis

基　　金：国家自然科学基金资助项目(41430641;41140032);中国地质局地质调查工作项目(1212351211006)

摘　　要：建立了加速溶剂萃取/高效液相色谱-三重四极杆串联质谱（ASE/HPLC-MS/MS）批量检测农田土壤中六溴环十二烷（HBCDs）和四溴双酚A（TBBPA）残留的分析方法。土壤样品经加速溶剂萃取,Sep-pak C18固相萃取柱净化后,在多反应监测（MRM）负离子电喷雾模式下进行HPLC-MS/MS分析。色谱柱为X Bridge C18反相柱（150 mm×2.1 mm×3.5μm）,流动相为梯度变化的甲醇和水溶液。在最佳实验条件下,六溴环十二烷和四溴双酚A在0.50-200.0μg/L范围内线性关系良好（r≥0.998）,方法检出限（S/N≥3）为1.80-10.0 ng/kg。在1.0-40.0μg/kg添加水平内,平均加标回收率为73.8%-106.9%,相对标准偏差（RSD）为5.8%~11.2%。采用该方法分析了我国某区域内表层土壤样品的HBCDs和TBBPA,得到理想的分析效果。A high performance liquid chromatography -tandem mass spectrometric method （HPLC - MS/MS） was developed for the sinmhaneous determination of hexabromocyclododeeanes（HBCDs） and tetrabromobisphenol A（TBBPA） in farmland soils. Samples were extracted by accelerated solvent extraction （ASE） and purified with Sep - pak C18 solid phase extraction （SPE） cartridges. The targeted compounds were separated on an X Bridge C18（150 mm ×2. 1 mm × 3.5 pom） using methanol -water as mobile phases, and then analyzed by HPLC - MS/MS in multiple reaction monitoring （MRM） mode with negtive eleetrospray ionization. The target compounds had good linear relationships（r≥0. 998） in the range of 0.50- 200.0 μg/L. The limits of detection （S/N ≥3 ） were in the range of 1.80 - 10.0 ng/kg, and the average recoveries at spiked levels of 1.0 - 40.0 pog/kg ranged from 73.8% to 106.9% with RSDs of 5.8% - 11.2% . The method was successfully applied in the detection of HBCDs and TBBPA residues in practical farmland soils.

关 键 词：加速溶剂萃取 高效液相色谱-串联质谱(HPLC-MS/MS) 农田土壤 六溴环十二烷(HBCDs) 四溴双酚A 

分 类 号：O657.63[理学—分析化学] TQ314.248[理学—化学]