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使用预处理碳纤维微电极对低分子量溴化酚和四溴双酚A进行高效液相色谱-电化学检测

HPLC-ED of low-molecular weight brominated phenols and tetrabromobisphenol A using pretreated carbon fiber microelectrode.

作者信息

Bartosova Zdenka, Jirovsky David, Riman Daniel, Halouzka Vladimir, Svidrnoch Martin, Hrbac Jan

机构信息

Department of Analytical Chemistry, Palacky University, Faculty of Science, 17. listopadu 12, CZ-771 46 Olomouc, Czech Republic.

Department of Analytical Chemistry, Palacky University, Faculty of Science, 17. listopadu 12, CZ-771 46 Olomouc, Czech Republic.

出版信息

Talanta. 2014 May;122:115-21. doi: 10.1016/j.talanta.2014.01.013. Epub 2014 Jan 31.

Abstract

Electrochemically pretreated carbon fiber microelectrode was used to develop a simple, fast and sensitive HPLC-ECD method for the determination of brominated phenols. In addition to simple mono-, di- and tri-bromophenols (4-bromophenol, 2,4-dibromophenol, 2,6-dibromophenol, 2,4,6-tri-bromophenol) the possibility of electrochemical detection of 3,3',5,5'-tetrabromobisphenol A in oxidation mode is reported for the first time. The isocratic separation was achieved within 14 min using ternary mobile phase consisting of 50mM-phosphate buffer (pH 3.5), acetonitrile and methanol (35/15/50, v/v), and detection potential of E=+1450 mV (vs. Ag/AgCl). The carbon fiber microelectrode permitted to use high anodic potentials (up to +1800 mV vs. Ag/AgCl), the optimum analytical response was achieved at +1450 mV vs. Ag/AgCl. The limits of detection (LOD) for the studied analytes were within the range of 1.8-56.6 ng mL(-1). The developed method was applied to determination of brominated phenols in spiked water samples. Furthermore, after simple extraction with methyl tert-butyl ether, it was possible to quantify tetrabromobisphenol A (TBBA) in a piece of CRT monitor plastic casing. The found amount of TBBA was 10.22 mg kg(-1) (±0.43).

摘要

采用电化学预处理的碳纤维微电极开发了一种简单、快速且灵敏的用于测定溴代酚的高效液相色谱 - 电化学检测法。除了简单的单溴、二溴和三溴酚(4 - 溴酚、2,4 - 二溴酚、2,6 - 二溴酚、2,4,6 - 三溴酚)外,首次报道了在氧化模式下对3,3',5,5'-四溴双酚A进行电化学检测的可能性。使用由50mM磷酸盐缓冲液(pH 3.5)、乙腈和甲醇(35/15/50,v/v)组成的三元流动相,在14分钟内实现了等度分离,检测电位为E = +1450 mV(相对于Ag/AgCl)。碳纤维微电极允许使用高阳极电位(相对于Ag/AgCl高达 +1800 mV),在相对于Ag/AgCl为 +1450 mV时获得了最佳分析响应。所研究分析物的检测限在1.8 - 56.6 ng mL(-1)范围内。所开发的方法应用于加标水样中溴代酚的测定。此外,在用甲基叔丁基醚进行简单萃取后,可以对一块阴极射线管显示器塑料外壳中的四溴双酚A(TBBA)进行定量。测得的TBBA含量为10.22 mg kg(-1)(±0.43)。

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