Bartosova Zdenka, Jirovsky David, Riman Daniel, Halouzka Vladimir, Svidrnoch Martin, Hrbac Jan
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.
Talanta. 2014 May;122:115-21. doi: 10.1016/j.talanta.2014.01.013. Epub 2014 Jan 31.
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).
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)。