高效液相色谱-串联质谱法测定土壤和沉积物中六溴环十二烷和四溴双酚A
Determination of Hexabromocyclododecane and Tetrabromobisphenol A in Soil and Sediment by High Performance Liquid Chromatography-Triple Quadrupole Mass Spectrometry
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摘要: 为服务我国履行斯德哥尔摩公约和新污染物监测需要,建立了同步分析土壤和沉积物中测定3种六溴环十二烷(HBCDs)异构体和四溴双酚A(TBBPA)的高效液相色谱-三重四极杆质谱法. 样品经冷冻干燥,以正己烷/丙酮(V/V,1/1)为提取溶剂进行加压流体提取,通过中性和酸性复合硅胶柱的净化处理后,利用HPLC-MS/MS检测,采用同位素稀释法进行定量分析. 结果表明:①目标物在液相色谱上得到有效的基线分离,保留时间变化量在0.13 min以内,标准曲线2~200 ng/mL内的平均相对响应因子的相对标准偏差小于15%. ②目标物α-HBCD、β-HBCD、γ-HBCD和TBBPA的方法检出限分别为0.06、0.04、0.04和0.06 μg/kg. ③石英砂、背景土壤和工业土壤、河流沉积物和海洋沉积物的低中高浓度平行添加实验,得到该方法精密度为0.56%~10.6%,正确度为92.9%~121%. ④以8种不同地区和类型的土壤进行添加实验,回收率范围为85.9%~104%. ⑤建立的方法具有灵敏度高、稳健性强,能够适用于复杂土壤和沉积物样品中HBCDs和TBBPA的分析测试.
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关键词:
- 土壤 /
- 沉积物 /
- 六溴环十二烷 /
- 四溴双酚A /
- 高效液相色谱-三重四极质谱
Abstract: A high performance liquid chromatography-triple quadrupole mass spectrometry method was developed to determinate three hexabromocyclododecane (HBCD) isomers and tetrabromobisphenol A (TBBPA) in soil and sediment, for the needs of Stockholm Convention and emerging pollutants monitoring in China. The samples were freeze-dried, extracted by pressurized fluid with n-hexane/acetone (V/V, 1/1), and then cleaned up by neutral and acidic silica gel column. After analyzed by high performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS), they were quantitated by isotope dilution method. The results showed that: ① effective baseline separation was achieved by liquid chromatography, and the retention time deviation was less than 0.13 min. The relative standard deviation of the mean relative response factor was less than 15% in the concentration range of 2-200 ng/mL. ②The limits of detection of α-HBCD, β-HBCD, γ-HBCD and TBBPA were 0.06, 0.04, 0.04 and 0.06 μg/kg, respectively. ③The precision of the method was 0.56%~10.6%, and the recoveries was 92.9%~121%. (4) The addition experiment was carried out with 8 different soil types and regions. The recoveries ranged from 85.9% to 104%. (5) The established method has demonstrated high sensitivity and strong robustness, and could be applied to the determination of HBCDs and TBBPA in complex soil and sediment samples.
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