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固相萃取-气相色谱-质谱-选择离子法检测污水中壬基酚
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中文关键词  壬基酚  内分泌干扰作用  污水  固相萃取-气相色谱-质谱-选择离子  定量检测
英文关键词  nonylphenol  endocrine disrupter activity  wastewater  SPE-GC-MS-∑SIM  quantitative analysis
作者单位
郝瑞霞 北京工业大学建筑工程学院北京 100022 
梁鹏 北京工业大学建筑工程学院北京 100022 
赵曼 北京工业大学建筑工程学院北京 100022 
王俊安 北京工业大学建筑工程学院北京 100022 
周玉文 北京工业大学建筑工程学院北京 100022 
中文摘要
      壬基酚是城市污水和再生水中的一种痕量污染物,具有内分泌干扰作用. 由于壬基分支程度的不同,污水中有多种同分异构体存在,基体背景复杂,定量检测困难. 采用固相萃取-气相色谱-质谱和选择性离子定量分析方法,对70多个污水和再生水样品中壬基酚同分异构体总量进行了定量检测. 结果表明,亲水-亲脂平衡固相萃取柱对壬基酚有良好选择吸附能力,不同水样的浓缩倍数在50~200倍之间. 在壬基酚各异构体质谱图中,107、121、135、149、163这5种离子的丰度较高,特异性较强,其响应值总和(∑SIM)占总离子流(TIC)的54.4%~73%,以∑SIM(107、121、135、149、163)色谱图的积分面积作为定量检测的依据,既准确地反映各种异构体的组成,又排除了背景离子的干扰,确保了方法的选择性、准确度和精密度.
英文摘要
      Nonylphenol (NP) having endocrine disrupter activity is an ultra trace component in sewage and reuse wastewater. There are many NP isomers in the wastewater because nonyl structure is different. The background impurity of the samples is very complex with many other components. So it is difficulty for quantitative analysis of NP in the samples. About seventy sewages and recycled wastewater samples had been measured for the content of NP isomer mixtures by solid-phase extraction–gas chromatography–mass spectrometry and multi-selected ions monitoring (shortened as SPE-GC-MS-SIM). The results show that hydrophilic-lipophilic-equilibrium solid-phase extraction pole has selective adsorption for NP, so that the samples can be concentrated from 50 to 200 times. The five kinds of mass spectrum ions, i.e. 107, 121, 135, 149, 163, have higher abundance and distinct character. The sum of five selected ion monitoring (∑SIM) is from 54.4 to 73 percent of the total ion current for NP, which can accurately represent different NP isomers. Quantitative analysis base on the spectral integral of the ∑SIM chromatograph can eliminate interference with background signal and ensure selectivity, accuracy and precision of the method.

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