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超高效液相色谱-串联质谱法测定污水中14种有机磷酸酯阻燃剂

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梁钪, 牛宇敏, 刘景富. 超高效液相色谱-串联质谱法测定污水中14种有机磷酸酯阻燃剂[J]. 环境化学, 2014, 33(10): 1681-1685. doi: 10.7524/j.issn.0254-6108.2014.10.011
引用本文: 梁钪, 牛宇敏, 刘景富. 超高效液相色谱-串联质谱法测定污水中14种有机磷酸酯阻燃剂[J]. 环境化学, 2014, 33(10): 1681-1685. doi: 10.7524/j.issn.0254-6108.2014.10.011
shu
LIANG Kang, NIU Yumin, LIU Jingfu. Determination of 14 organophosphate ester flame retardants in wastewater by UPLC-MS/MS[J]. Environmental Chemistry, 2014, 33(10): 1681-1685. doi: 10.7524/j.issn.0254-6108.2014.10.011
Citation: LIANG Kang, NIU Yumin, LIU Jingfu. Determination of 14 organophosphate ester flame retardants in wastewater by UPLC-MS/MS[J]. Environmental Chemistry, 2014, 33(10): 1681-1685. doi: 10.7524/j.issn.0254-6108.2014.10.011
shu

超高效液相色谱-串联质谱法测定污水中14种有机磷酸酯阻燃剂

  • 1.

    中国科学院生态环境研究中心, 环境化学与生态毒理学国家重点实验室, 北京, 100085

  • 基金项目:

    国家高技术研究发展计划(863)课题(2013AA065201)、国家自然科学基金项目(21025729)和中国科学院战略性先导科技专项(XDB14020101)资助.

Determination of 14 organophosphate ester flame retardants in wastewater by UPLC-MS/MS

  • 1.

    State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing, 100085, China

  • Fund Project:

摘要

  • 摘要: 建立了超高效液相色谱-串联质谱(UPLC-MS/MS)联用法同时测定污水中14种有机磷酸酯阻燃剂(OPEs)的分析方法.样品采集后,经GF/C膜过滤,HLB固相萃取小柱净化后进样分析.以BEH C18色谱柱为分离柱,乙腈和水混合液为流动相(0.2 mL min-1)梯度洗脱,15 min内可完成14种OPEs的分离.在电喷雾正离子模式下,采用多反应监测模式(MRM)进行质谱测定.在加标浓度为1.0 μg·L-1时,14种OPEs在污水处理厂进水和出水中的回收率分别为52.1%—119%、43.6%—114%,相对标准偏差(RSD)分别为1.2%—16.2%、0.4%—9.2%,方法的检出限(LOD)在0.3—6.0 ng·L-1间.方法精密度好,准确度高,可满足同时对污水样品中的14种OPEs进行定性及定量分析的要求.
    Abstract: An ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the simultaneous determination of 14 organophosphate esters (OPEs) in waste water. The collected water samples were filtered with GF/C membrane and purified by solid phase extraction (SPE) using HLB cartridges. The eluent was collected and concentrated to nearly drieness under a gentle stream of nitrogen gas, and then re-dissolved with 1 mL initial mobile phase (40%(V/V) acetonitrile in water) and analyzed by UPLC-MS/MS under positive electrospray ionization and multiple reaction monitoring (MRM). Separation of analytes was finished in 15 min by using a BEH C18 column, and gradient elution with a mixture of acetonitrile and water as mobile phases (0.2 mL·min-1). The recoveries of all the compounds from the influent water and effluent water of a wastewater treatment plant, at the spiked concentration levels of 1.0 μg·L-1, were respectively in the range of 52.1%—119% and 43.6%—114%, with the corresponding relative standard deviations (RSD) of 1.2%—16.2% and 0.4%—9.2%. The method detection limits ranged from 0.3 to 6.0 ng·L-1. The method could be applied in the analysis of 14 OPEs in waste water samples with good precisions and accuracies.
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  • 收稿日期:  2014-05-25
梁钪, 牛宇敏, 刘景富. 超高效液相色谱-串联质谱法测定污水中14种有机磷酸酯阻燃剂[J]. 环境化学, 2014, 33(10): 1681-1685. doi: 10.7524/j.issn.0254-6108.2014.10.011
引用本文: 梁钪, 牛宇敏, 刘景富. 超高效液相色谱-串联质谱法测定污水中14种有机磷酸酯阻燃剂[J]. 环境化学, 2014, 33(10): 1681-1685. doi: 10.7524/j.issn.0254-6108.2014.10.011
shu
LIANG Kang, NIU Yumin, LIU Jingfu. Determination of 14 organophosphate ester flame retardants in wastewater by UPLC-MS/MS[J]. Environmental Chemistry, 2014, 33(10): 1681-1685. doi: 10.7524/j.issn.0254-6108.2014.10.011
Citation: LIANG Kang, NIU Yumin, LIU Jingfu. Determination of 14 organophosphate ester flame retardants in wastewater by UPLC-MS/MS[J]. Environmental Chemistry, 2014, 33(10): 1681-1685. doi: 10.7524/j.issn.0254-6108.2014.10.011
shu

超高效液相色谱-串联质谱法测定污水中14种有机磷酸酯阻燃剂

  • 1. 中国科学院生态环境研究中心, 环境化学与生态毒理学国家重点实验室, 北京, 100085
  • 收稿日期:  2014-05-25
基金项目:

国家高技术研究发展计划(863)课题(2013AA065201)、国家自然科学基金项目(21025729)和中国科学院战略性先导科技专项(XDB14020101)资助.

摘要: 建立了超高效液相色谱-串联质谱(UPLC-MS/MS)联用法同时测定污水中14种有机磷酸酯阻燃剂(OPEs)的分析方法.样品采集后,经GF/C膜过滤,HLB固相萃取小柱净化后进样分析.以BEH C18色谱柱为分离柱,乙腈和水混合液为流动相(0.2 mL min-1)梯度洗脱,15 min内可完成14种OPEs的分离.在电喷雾正离子模式下,采用多反应监测模式(MRM)进行质谱测定.在加标浓度为1.0 μg·L-1时,14种OPEs在污水处理厂进水和出水中的回收率分别为52.1%—119%、43.6%—114%,相对标准偏差(RSD)分别为1.2%—16.2%、0.4%—9.2%,方法的检出限(LOD)在0.3—6.0 ng·L-1间.方法精密度好,准确度高,可满足同时对污水样品中的14种OPEs进行定性及定量分析的要求.

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