固相萃取-高效液相色谱-质谱法测定海水中的烷基酚和烷基酚聚氧乙烯醚

Determination of alkylphenol and alkylphenolpolyethoxylates in brine by solid phase extraction and high performance liquid chromatography-mass spectrometry

建立了固相萃取-高效液相色谱-电喷雾质谱分析海水中辛基酚、壬基酚、辛基酚聚氧乙烯醚和壬基酚聚氧乙烯醚的方法。海水样品经C18固相萃取柱富集净化后,以甲醇-水为流动相,在Hypersil GOLD色谱柱上分离,电喷雾质谱在选择离子监测模式下分析目标化合物,采用外标法定量。结果表明,4种化合物的平均加标回收率为59.6%～104.4%,相对标准偏差(RSD,n=3)为1.0%～13.5%;仪器检出限为0.08～3μg/L。将本方法用于大连海岸6个采样点海水中辛基酚、壬基酚、辛基酚聚氧乙烯醚和壬基酚聚氧乙烯醚的检测发现,样品中壬基酚和壬基酚聚氧乙烯醚均有检出,且油港和海港附近海水中的含量较高。

A simple method based on solid phase extraction（SPE） coupled with high performance liquid chromatography-mass spectrometry（HPLC-MS） was developed for the determination of octylphenol（OP）,nonylphenol（NP）,octylphenol ethoxylates（OPEOs） and nonylphenol ethoxylates（NPEOs） in brine.The extraction and cleanup of brine samples were performed on C18 solid-phase extraction cartridges.The complete separation among OP,NP,OPEOs and NPEOs was achieved on a Hypersil GOLD analytical column with methanol-water as the mobile phase.The determination was achieved using HPLC-MS with electrospray ionization（ESI） in selected ion monitoring mode.The results showed that the average recoveries of target compounds were 59.6%-104.4% and the corresponding relative standard deviations（RSDs,n=3） were 1.0%-13.5%.The instrumental limits of detection for the compounds were 0.08-3 μg/L.This method was applied to the analysis of the samples of seawater near Dalian coast.The results showed that both NP and NPEOs were detected in all samples and their concentrations in seaport and oil port were much higher than those in other sampling sites.