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采用固相萃取预富集和超高效液相色谱-紫外检测法同时测定水样中的六种阻燃剂

The Simultaneous Determination of Six Flame Retardants in Water Samples Using SPE Pre-concentration and UHPLC-UV Method.

作者信息

Kowalski Bartosz, Mazur Maciej

机构信息

Department of Inorganic, Analytical and Electrochemistry, Chemical Faculty, The Silesian University of Technology, 7 Marcina Strzody Str, 44-100 Gliwice, Poland.

出版信息

Water Air Soil Pollut. 2014;225(3):1866. doi: 10.1007/s11270-014-1866-4. Epub 2014 Feb 12.

Abstract

Analytical method for the determination of six flame retardants (FRs) from two groups was proposed. These groups included the brominated flame retardants (BFRs) 3,3',5,5'-tetrabromobisphenol A (TBBPA), 1,2,5,6,9,10-hexabromocyclododecane (HBCD) and tetrabromophthalic anhydride (TBPA) and triester organophosphate flame retardants (OPFRs) tris(2,3-dibromopropyl) phosphate (TBPP), ethylhexyl diphenyl phosphate (EHDP) and triphenyl phosphate (TPhP). Reversed phase ultrahigh-performance liquid chromatography (UHPLC) with a UV detector, different chromatographic columns, different mobile phases and gradient elution programmes were used to obtain the best separations within the shortest possible time. Solid-phase extraction (SPE) was examined as a pre-concentration step from distilled water. The column with the highest recoveries (the Bond Elut ENV column gave recoveries over 70 % for all compounds) was then tested on 1-L blank surface water samples. The proposed analytical procedure was applied for the determination of FRs in surface water samples. The concentrations of FRs found in water samples ranged from 0.03 (TPhP) to 3.10 μg L (HBCD). Method detection limits (MDLs) ranged from 0.008 to 0.518 μg L, and method quantification limits (MQLs) ranged from 0.023 to 1.555 μg L for all compounds.

摘要

提出了一种测定两组六种阻燃剂(FRs)的分析方法。这两组包括溴化阻燃剂(BFRs)3,3',5,5'-四溴双酚A(TBBPA)、1,2,5,6,9,10-六溴环十二烷(HBCD)和四溴邻苯二甲酸酐(TBPA)以及三酯有机磷酸酯阻燃剂(OPFRs)磷酸三(2,3-二溴丙基)酯(TBPP)、乙基己基二苯基磷酸酯(EHDP)和磷酸三苯酯(TPhP)。使用配备紫外检测器的反相超高效液相色谱(UHPLC)、不同的色谱柱、不同的流动相和梯度洗脱程序,以在尽可能短的时间内实现最佳分离。研究了固相萃取(SPE)作为从蒸馏水中进行预浓缩步骤的方法。然后在1升空白地表水样品上测试回收率最高的柱(Bond Elut ENV柱对所有化合物的回收率均超过70%)。所提出的分析程序用于测定地表水样品中的FRs。水样中发现的FRs浓度范围为0.03(TPhP)至3.10μg/L(HBCD)。所有化合物的方法检测限(MDLs)范围为0.008至0.518μg/L,方法定量限(MQLs)范围为0.023至1.555μg/L。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/acf8/3955136/c59a9fbacfc7/11270_2014_1866_Fig1_HTML.jpg

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