Liu Runzeng, Ruan Ting, Song Shanjun, Lin Yongfeng, Jiang Guibin
State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085, China.
State Key Laboratory of Environmental Chemistry and Ecotoxicology, Research Center for Eco-Environmental Sciences, Chinese Academy of Sciences, Beijing 100085, China.
J Chromatogr A. 2015 Feb 13;1381:13-21. doi: 10.1016/j.chroma.2014.11.042. Epub 2014 Nov 21.
Robust analytical methods were developed for the determination of eight emerging synthetic phenolic antioxidants (SPAs) and three metabolites in sewage sludge, effluent and river water matrices. Accelerated solvent extraction was employed for the extraction of the target analytes from sludge, dichloromethane/hexane=3:1 (extraction solvent) and 90°C (extraction temperature) were used after optimization. Silica gel packed column was chosen for the subsequent clean-up procedure for sludge extract. For the water sample analysis, liquid-liquid extraction combined with silica gel clean-up was used. The targets were determined by optimized high performance liquid chromatography-tandem mass spectrometry method in negative electrospray ionization mode. The method quantification limits of the 11 analytes ranged from 0.1 to 23 ng/L, 0.1 to 20 ng/L and 0.1 to 15 ng/g for sewage effluent, river water and sludge matrices, respectively. The total recoveries of the pretreatment varied from 63 to 106%, with relative standard deviations less than 17% for the three matrices at different spiking levels. Nine targets including 2,6-di-tert-butyl-4-methylphenol (BHT), 3,5-di-tert-butyl-4-hydroxybenzaldehyde (BHT-CHO), 2,6-di-tert-butyl-1,4-benzoquinone (BHT-Q), 2,6-di-tert-butyl-4-hydroxy-4-methyl-2,5-cyclohexadienone (BHT-quinol), 3-tert-butyl-4-hydroxyanisole (BHA), 4-tert-octylphenol (4-tOP), 2,2'-methylenebis(6-tert-butyl-4-methylphenol) (AO 2246), 4,4'-butylidenebis(2-(1,1-dimethylethyl)-5-methyl-phenol) (AO 44B25) and 1,3,5-trimethyl-2,4,6-tris(3,5-di-tert-butyl-4-hydroxybenzyl)benzene (AO 330) were identified in the collected samples, with concentrations ranging 1.1-2325 ng/g and 0.4-2510 ng/L for sludge and water matrices, respectively. Sewage effluent was considered as a possible contamination source of certain SPA homologues and relative metabolites to the recipient aquatic systems.
开发了稳健的分析方法，用于测定污水污泥、废水和河水基质中的8种新兴合成酚类抗氧化剂（SPA）和3种代谢物。采用加速溶剂萃取法从污泥中提取目标分析物，优化后使用二氯甲烷/己烷=3:1（萃取溶剂）和90°C（萃取温度）。选择硅胶填充柱对污泥提取物进行后续净化处理。对于水样分析，采用液液萃取结合硅胶净化。通过优化的高效液相色谱-串联质谱法在负电喷雾电离模式下测定目标物。11种分析物在污水、河水和污泥基质中的方法定量限分别为0.1至23 ng/L、0.1至20 ng/L和0.1至15 ng/g。不同加标水平下，三种基质预处理的总回收率在63%至106%之间，相对标准偏差小于17%。在所采集的样品中鉴定出9种目标物，包括2,6-二叔丁基-4-甲基苯酚（BHT）、3,5-二叔丁基-4-羟基苯甲醛（BHT-CHO）、2,6-二叔丁基-1,4-苯醌（BHT-Q）、2,6-二叔丁基-4-羟基-4-甲基-2,5-环己二烯酮（BHT-对苯二酚）、3-叔丁基-4-羟基苯甲醚（BHA）、4-叔辛基苯酚（4-tOP）、2,2'-亚甲基双（6-叔丁基-4-甲基苯酚）（AO 2246）、4,4'-亚丁基双（2-（1,1-二甲基乙基）-5-甲基苯酚）（AO 44B25）和1,3,5-三甲基-2,4,6-三（3,5-二叔丁基-4-羟基苄基）苯（AO 330），污泥和水样中其浓度分别为1.1-2325 ng/g和0.4-2510 ng/L。污水被认为是某些SPA同系物及其相关代谢物进入受纳水系统的可能污染源。
