C_(18)膜萃取-超高效液相色谱-串联质谱法测定海水中羟基多环芳烃  

Determination of hydroxylated polycyclic aromatic hydrocarbons in seawater by ultra performance liquid chromatography and mass spectrometry-C_(18) membrane disk extraction

作　　者：刘丹[1] 赫春香[1] 那广水[2] 李瑞婧[2] 高宇航 曹胜凯 LIU Dan;HE Chun-xiang;NA Guang-shui;LI Rui-jing;GAO Yu-hang;CAO Sheng-kai(School of Chemistry and Chemical Engineering;State Oceanic Administration Key Laboratory of Environment Monitoring Center,Dalian 116023;Liaoning Normal University,Dalian 11602;Marine Eeology and Environment,National Marin)

机构地区：[1]辽宁师范大学化学化工学院,大连116029 [2]国家海洋环境监测中心国家海洋局近岸海域生态环境重点实验室,大连116023

出　　处：《分析试验室》2018年第8期884-888,共5页Chinese Journal of Analysis Laboratory

基　　金：国家自然科学基金(41406088;21377032);南北极环境综合考察与评估专项(2017-02-01;03-04;04-01;04-03)资助

摘　　要：建立了C_(18)固相膜萃取-超高效液相色谱/质谱法测定海水中11种羟基多环芳烃(OHPAHs)的方法。利用C_(18)固相膜对4L海水中11种OH-PAHs进行富集,二氯甲烷超声提取,浓缩后进入C_(18)柱色谱,以乙腈-0.02%氨水为流动相梯度淋洗后进入质谱检测,11种OH-PAHs的浓度与其峰面积呈线性关系,方法检出限为0.290~2.04 ng/L,平均回收率为60.8%~96.4%,相对标准偏差均低于13%。利用本方法对河北养殖区海水中11种OH-PAHs进行检测,OH-PAHs的浓度处于1.81~10.0 ng/L之间。本法为远距离、大体积水样中痕量OH-PAHs的提取富集与测定提供了解决方案。A new method for determining 11 hydroxyl polycyclic aromatic hydrocarbons（OH-PAHs）in seawater was established by combining the C（18） membrane disk extraction with ultra performance liquid chromatography and mass spectrometry（UPLC-MS/MS）. 11 OH-PAHs from 4 L seawater were enriched by C（18） membrane, and then ultrasonic extracted by dichloromethane. After being concentrated,compounds were separated by C（18） column and were detected by mass spectrometry with CH3 CN/NH3·H2 O（0. 2%） as mobile phase gradient elution. The peak areas of 11 OH-PAHs were linearly dependent with their concentrations and the detection limit were 0. 290 ~ 2. 04 ng/L. The average recoveries were 60. 8% ~ 96. 4% and the relative standard deviations were less than 13%.This method was applied to analyze the concentration of 11 OH-PAHs in the seawater of Hebei aquaculture area,and the results showed that the concentration of OH-PAHs was 1. 81 ~ 10. 0 ng/L.The method is applicable to determine the concentration of OH-PAHs in large volume of water samples.

关 键 词：羟基多环芳烃 C18固相膜萃取 超高效液相色谱/质谱法 海水 

分 类 号：X826[环境科学与工程—环境工程]