液相色谱-电喷雾质谱法同时测定水体中的壬基酚聚氧乙烯醚及其代谢产物  

Simultaneous Determination of Nonylphenol Ethoxylates and Their Metabolites by Liquid Chromatography-Electrospray Ionisation Mass Spectrometry

作　　者：张晶[1] 张昱[1] 杨敏[1] 金芬[1] 陈梅雪[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：《分析测试学报》2007年第2期178-182,共5页Journal of Instrumental Analysis

基　　金：国家自然科学基金资助项目(20307010;50578153)

摘　　要：利用液相色谱-电喷雾质谱法同时分析水体中的壬基酚聚氧乙烯醚（NPEOs）及其代谢产物壬基酚聚氧乙烯醚乙酸（NPECs）和壬基酚（NP）,用Waters Symmetry Shield^TM RP 18色谱柱,甲醇和乙酸铵溶液作为梯度洗脱的流动相,结果表明3类物质的分离效果良好,并可通过选择离子记录（SIR）模式实现NPEOs和NPECs各单体的定量.仪器的检出限为1～50 pg,选用Oasis HLB小柱进行固相萃取,回收率达75%～98%,平均标准偏差小于12%.该方法用于污水处理厂的水样测定,所取各水样中都测出了NP和NPEOs,并从氧化沟上清液中检测到 NPECs.A reversed-phase liquid chromatography -electrospray ionisation mass spectrometry （LC - ESI MS ） was developed for the simultaneous determination of nonylphenol ethoxylates surfactants （NPEOs） and their biodegradation products, namely nonylphenol （NP） and nonylphenoxy carboxylates （NPECs） in aquatic environment in a single run. After solid-phase extracting （SPE） with a 500 mg of Oasis HLB cartridges, the analytes were separated on a Waters Symmetry Shield^TM RP 18 column using 5 mmol/L NH4Ac in water and CH3OH as binary mobile phase for gradient elution. As a result, a well-shaped peak can be observed on every selected ion chromatogram. Instrumental limits of detection for these compounds were 1 -50 pg, and the SPE recoveries ranged from 75% to 98% and the relative standard deviation（RSD） was below 12%. This method was applied to the analysis of the samples of the sewage treatment plant. NP and NPEOs were found in all three samples while NPECs occurred only in the supernatant of mixed liquid.

关 键 词：壬基酚聚氧乙烯醚 壬基酚聚氧乙烯醚乙酸 壬基酚 固相萃取 液相色谱-电喷雾质谱 

分 类 号：O657.63[理学—分析化学]