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基质固相分散(MSPD)作为一种简单而有用的样品前处理技术,用于测定粉尘中的多溴二苯醚(PBDEs)。

Matrix solid-phase dispersion (MSPD) as simple and useful sample preparation technique for determination of polybrominated diphenyl ethers (PBDEs) in dust.

机构信息

Department of Analytical Chemistry, Faculty of Chemistry, Gdańsk University of Technology (GUT), Narutowicza 11/12 St, 80-233, Gdańsk, Poland.

Department of Analytical Chemistry, Faculty of Chemistry, Gdańsk University of Technology (GUT), Narutowicza 11/12 St, 80-233, Gdańsk, Poland.

出版信息

Anal Chim Acta. 2019 Nov 25;1084:33-42. doi: 10.1016/j.aca.2019.08.001. Epub 2019 Aug 6.

Abstract

In the present study a novel analytical procedure for the determination of polybrominated diphenyl ethers in dust samples was developed. The main aim of the research was the selection of the optimum conditions of the matrix solid-phase dispersion before the final determination of polybrominated diphenyl ethers in dust samples. In order to assess the best usefulness of this technique, a favourable ratio of sample amount to the mass of dispersing sorbent, as well as the type of this sorbent used has been tested. The type of sorbent responsible for additional purification (clean-up sorbent) of the extract during matrix solid-phase dispersion was also selected. Gas chromatography coupled with mass spectrometry will be used at the final determination step. Preliminary results indicate that the use of matrix solid-phase dispersion can be a promising alternative to other time-consuming and multi-stage analytical procedures. The proposed method provided satisfactory recoveries (76-119%) and limits of detection: 2.1-4.4 pg μL for tri-heptaBDE in linear range of 5-100 pg μL; 480 pg μL for decaBDE in linear range of 500-2000 pg μL from only 0.05 g of a dust sample. Finally, the method was applied to study the content of selected polybrominated diphenyl ethers in real dust samples. Some polybrominated diphenyl ether congeners reached up to (16.3 ± 3.0)·10 ng g.

摘要

本研究提出了一种测定粉尘样品中多溴二苯醚的新型分析方法。该研究的主要目的是选择基质固相分散的最佳条件,以便最终测定粉尘样品中的多溴二苯醚。为了评估该技术的最佳效果,我们测试了样品量与分散吸附剂质量的最佳比例,以及所使用的吸附剂类型。在基质固相分散过程中,还选择了负责提取中额外净化(净化吸附剂)的吸附剂类型。最终测定步骤将采用气相色谱-质谱联用技术。初步结果表明,基质固相分散法可作为替代其他耗时且多阶段分析程序的有前途的方法。该方法提供了令人满意的回收率(76-119%)和检测限:在 5-100pgμL 的线性范围内,三-六溴二苯醚的检测限为 2.1-4.4pgμL;在 500-2000pgμL 的线性范围内,十溴二苯醚的检测限为 480pgμL,仅需 0.05g 的粉尘样品。最后,该方法被应用于研究实际粉尘样品中选定的多溴二苯醚的含量。一些多溴二苯醚同系物的浓度高达(16.3±3.0)·10ngg。

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