Chi Xiyuan, Liu Jiyan, Yu Miao, Xie Zhouqing, Jiang Guibin
State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, P.O. Box 2871, Beijing 100085, China; Institute of Polar Environment, School of Earth and Space Sciences, University of Science and Technology of China, Hefei, Anhui 230026, China.
State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, P.O. Box 2871, Beijing 100085, China; College of Resources and Environment, University of Chinese Academy of Sciences, Beijing 100049, China.
Talanta. 2017 Mar 1;164:57-63. doi: 10.1016/j.talanta.2016.11.010. Epub 2016 Nov 8.
A reliable and effective method for simultaneous analysis of trace amount of bromophenols (BPs) in various aqueous samples was developed in this study. The aqueous samples must be acidified after sampling to prevent the fast degradation of bromophenols. Solid-phase extraction was chosen to extract and purify the water samples. High performance liquid chromatography coupled with tandem mass spectrometry with an electrospray ionization source (HPLC-ESI-MS/MS) was used for following identification and quantification. Under the optimized condition, fourteen out of fifteen target brominated phenols were successfully separated and detected with the exception of 2,6-bromophenol (2,6-BP) whose response was too low to be quantified by the MS detector. The method was validated by spiking river water and seawater samples with different concentrations of BPs, and the qualified spiking recoveries (64-100%) and precisions (0.4-11% RSD) were obtained. The method detection limits were 0.1-13.9ng/L and 0.1-21.9ng/L for 0.1L of river water and seawater samples, respectively, showing the influences from the sample matrix. The proposed method was successfully applied to the analysis of bromophenol contamination in real water samples, and six bromophenols were identified with a wide concentrations ranging from ng/L to μg/L.
本研究开发了一种可靠且有效的方法，用于同时分析各种水样中的痕量溴酚（BPs）。水样采集后必须酸化，以防止溴酚快速降解。选择固相萃取法对水样进行萃取和净化。采用高效液相色谱-电喷雾电离源串联质谱（HPLC-ESI-MS/MS）进行后续的定性和定量分析。在优化条件下，15种目标溴代酚中有14种成功分离并检测到，2,6-溴酚（2,6-BP）除外，其响应过低，无法通过质谱检测器进行定量。通过向河水和海水样品中添加不同浓度的溴酚进行方法验证，获得了合格的加标回收率（64-100%）和精密度（相对标准偏差0.4-11%）。对于0.1L河水和海水样品，方法检出限分别为0.1-13.9ng/L和0.1-21.9ng/L，显示了样品基质的影响。所提出的方法成功应用于实际水样中溴酚污染的分析，鉴定出6种溴酚，浓度范围从ng/L到μg/L。
