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多种色谱质谱联用技术测定沉积物中的十溴二苯醚

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王惠宇, 宋善军, 邵明武, 尹建道, 杨晨, 李彭辉. 多种色谱质谱联用技术测定沉积物中的十溴二苯醚[J]. 环境化学, 2019, (10): 2203-2211. doi: 10.7524/j.issn.0254-6108.2018111701
引用本文: 王惠宇, 宋善军, 邵明武, 尹建道, 杨晨, 李彭辉. 多种色谱质谱联用技术测定沉积物中的十溴二苯醚[J]. 环境化学, 2019, (10): 2203-2211. doi: 10.7524/j.issn.0254-6108.2018111701
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WANG Huiyu, SONG Shanjun, SHAO Mingwu, YIN Jiandao, YANG Chen, LI Penghui. Determination of decabromodiphenyl ether in sediment using chromatography-mass spectrometry methods[J]. Environmental Chemistry, 2019, (10): 2203-2211. doi: 10.7524/j.issn.0254-6108.2018111701
Citation: WANG Huiyu, SONG Shanjun, SHAO Mingwu, YIN Jiandao, YANG Chen, LI Penghui. Determination of decabromodiphenyl ether in sediment using chromatography-mass spectrometry methods[J]. Environmental Chemistry, 2019, (10): 2203-2211. doi: 10.7524/j.issn.0254-6108.2018111701
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多种色谱质谱联用技术测定沉积物中的十溴二苯醚

  • 1. 天津理工大学, 天津, 300384;

  • 2. 中国计量科学研究院, 北京, 100029

    • 通讯作者: 宋善军, E-mail: songsj@nim.ac.cn ; 
  • 基金项目:

    国家质量基础项目（2016YFF0201102）和国家自然科学基金青年基金（41601548）资助.

Determination of decabromodiphenyl ether in sediment using chromatography-mass spectrometry methods

  • 1. Tianjin University of Technology, Tianjin, 300384, China;

  • 2. National Institute of Metrology, China, Beijing, 100029, China

    • Corresponding author: SONG Shanjun, songsj@nim.ac.cn ; 
  • Fund Project: Supported by the National Key Research and Development Program of China (2016YFF0201102) and National Natural Science Foundation of China (41601548).

  • 摘要: 随着十溴二苯醚（BDE-209）正式进入《斯德哥尔摩公约》名单，准确测量其浓度水平对研究其环境行为具有重要意义.本文对多种色谱质谱联用技术——气相色谱-负化学电离质谱（GC-NCI-MS）、气相色谱-电子轰击电离质谱（GC-EI-MS）、气相色谱-电感耦合等离子体质谱（GC-ICP-MS）和高效液相色谱-电感耦合等离子体质谱（HPLC-ICP-MS）进行了优化和评估，并对其在实际环境沉积物样品中检测BDE-209的性能进行了考察.4种检测方法的定量限为3—200 ng·mL-1，在0.5-10 μg·mL-1的范围内有良好的线性关系（r2 > 0.995），测量结果的相对标准偏差（RSD）在0.5%—8.7%之间，可以满足BDE-209分析检测的需求.应用到沉积物实际样品的检测时，各方法测量结果的RSD为0.7%—15.7%，基质效应为98%—166%，其中GC-EI-MS和GC-NCI-MS表现出基质增强效应且分析结果的稳定性受到影响，可通过内标或基质加标方式进行校正，GC-ICP-MS、HPLC-ICP-MS几乎不受实际样品基质的影响，测量结果的准确性良好.
    Abstract: The accurate determination of decabrominated diphenyl ethers (BDE-209) is important for the study of its environmental behavior, especially after BDE-209 was officially listed in Stockholm Convention in 2017. This research optimized and evaluated most widely used gas/liquid chromatography-mass spectrometry methods for BDE-209 determination, including GC-NCI-MS, GC-EI-MS, GC-ICP-MS and HPLC-ICP-MS. The performances of each method were investigated for standard solution determination and field sediment samples determination. The limits of quantification ranged from 3-200 ng·mL-1 and linear fitting with coefficients >0.995 ranging from 0.5 to 10 μg·mL-1. The precision of each method was illustrated by relative standard deviation (RSD) of analysis results (n=5) ranging from 0.5%-8.7%. The performances of each method on field sediment sample analysis were investigated and the results showed the precision and matrix effects were 0.7%-15.7% and 98%-166%. GC-EI-MS and GC-NCI-MS signal intensities were enhanced, and the precision was affected by introduction of sediment matrix. Internal standards and matrix match calibration were suggested for these methods to analyze field samples. GC-ICP-MS and HPLC-ICP-MS showed robust performances with neglectable effects by sample matrix.
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  • 收稿日期:  2018-11-17

多种色谱质谱联用技术测定沉积物中的十溴二苯醚

    通讯作者: 宋善军, E-mail: songsj@nim.ac.cn ; 
  • 1. 天津理工大学, 天津, 300384;
  • 2. 中国计量科学研究院, 北京, 100029
  • 收稿日期:  2018-11-17
基金项目:

国家质量基础项目（2016YFF0201102）和国家自然科学基金青年基金（41601548）资助.

摘要: 随着十溴二苯醚（BDE-209）正式进入《斯德哥尔摩公约》名单，准确测量其浓度水平对研究其环境行为具有重要意义.本文对多种色谱质谱联用技术——气相色谱-负化学电离质谱（GC-NCI-MS）、气相色谱-电子轰击电离质谱（GC-EI-MS）、气相色谱-电感耦合等离子体质谱（GC-ICP-MS）和高效液相色谱-电感耦合等离子体质谱（HPLC-ICP-MS）进行了优化和评估，并对其在实际环境沉积物样品中检测BDE-209的性能进行了考察.4种检测方法的定量限为3—200 ng·mL-1，在0.5-10 μg·mL-1的范围内有良好的线性关系（r2 > 0.995），测量结果的相对标准偏差（RSD）在0.5%—8.7%之间，可以满足BDE-209分析检测的需求.应用到沉积物实际样品的检测时，各方法测量结果的RSD为0.7%—15.7%，基质效应为98%—166%，其中GC-EI-MS和GC-NCI-MS表现出基质增强效应且分析结果的稳定性受到影响，可通过内标或基质加标方式进行校正，GC-ICP-MS、HPLC-ICP-MS几乎不受实际样品基质的影响，测量结果的准确性良好.

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