柱前衍生-气相色谱/质谱法测定壬基酚方法研究  

Determination of Nonylphenols in Water by Pre-column Derivatization and Gas Chromatography Coupled with Mass Spectrometry

作　　者：周益奇[1] 马梅[1] 王子健[1] 

机构地区：[1]中国科学院生态环境研究中心环境水质学国家重点实验室,北京100085

出　　处：《分析化学》2005年第8期1109-1112,共4页Chinese Journal of Analytical Chemistry

基　　金：国家863高科技项目(No.2002AA601120);国家自然科学基金项目(No.50378089)

摘　　要：研究了一种利用壬基酚与N,O-双(三甲基硅烷基)三氟乙酰胺(简称BSTFA)柱前衍生气相色谱/质谱法测定污水中壬基酚的分析方法。通过实验确定了最佳的前处理方法,对比衍生和未衍生两种方法,确认该衍生化方法对11种常见壬基酚同分异构体具有更好的分离度(可将11种常见壬基酚同分异构体完全分离),更高的灵敏度。方法检出限为0.55ng/L(以4-N-nonylphenol为标准,信噪比为3时的信号对应4-N-NP的浓度)。本方法能延长分离柱的使用寿命,是一个高重现性和高精密度测定壬基酚的方法。A pre column derivatization technique for gas chromatography/mass spectrometric （GC/MS） analysis of nonylphenols in water was performed. Water sample was preconcentrated with Oasis HLB cartridges. The analytes were silylized with silyl reagent his （trimethylsilyl）trifluoroacetamide （BSTFA） after the sample dehydration. Eleven isomers of nonylphenols could be determined accurately by this method, and furthermore this method can prolong life of capillary column. There was no obvious impurity interfered. Recoveries of nonylphenols varied in 81. 1 ± 1. 0% for spiking experiments. Detection limits of the target compounds could be obtained high sensitivity. It attain 0. 55 ng/L for 4-N-nonylphenol. The reproducibility and precision of the method were expressed as relative standard deviation （ RSD% ）, within 1.0%. The method was applied successfully to the determination of nonylphenols in wastewater sampled from a sewage treatment plant in Beijing.

关 键 词：柱前衍生 气相色谱 质谱法 测定 壬基酚 水体监测 非离子表面活性剂 聚氧乙烯醚 

分 类 号：O657.63[理学—分析化学]