Determination of Hexabromocyclododecanes and Tetrabromobisphenol A in Farmland Soils by High Performance Liquid Chromatography-Tandem Mass Spectrometry
Determination of Hexabromocyclododecanes and Tetrabromobisphenol A in Farmland Soils by High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. 2016,35(11):1440-1444.
Determination of Hexabromocyclododecanes and Tetrabromobisphenol A in Farmland Soils by High Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. 2016,35(11):1440-1444.DOI:
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 × 3.5 μm),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0.50~200.0 μg/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1.0~40.0 μg/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。
Abstract
A high performance liquid chromatography-tandem mass spectrometric method(HPLC-MS/MS) was developed for the simultaneous determination of hexabromocyclododecanes(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 μm) using methanol-water as mobile phases,and then analyzed by HPLC-MS/MS in multiple reaction monitoring(MRM) mode with negtive electrospray 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 μg/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.