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

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 ShieldTMRP 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。

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

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 ShieldTM 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.