A novel method through solid phase extraction combined with gradient elution for concentration and separation of 66(ultra)trace persistent toxic pollutants in Antarctic waters  

作　　者：Li Zhang Guang-Shui Na Chun-Xiang He Rui-Jing Li Hui Gao Lin-Ke Ge Yan-Jie Wang Yao Yao 

机构地区：[1]School of Chemistry and Chemical Engineering,Liaoning Normal University [2]Key Laboratory for Ecological Environment in Coastal Areas (SOA),National Marine Environmental Monitoring Center

出　　处：《Chinese Chemical Letters》2016年第3期405-411,共7页中国化学快报（英文版）

基　　金：financially supported by the National Natural Science Foundation of China(No.21377032);the Chinese Polar Environment Comprehensive Investigation and Assessment Program(Nos.2014-02-01,2014-03-04,2014-04-01,2014-04-03);the Marine Public Welfare Scientific Research Projects(No.201105013);the Foundation of Polar Science Key Laboratory,SOA,China(No.KP201208)

摘　　要：This study developed a method to perform the simultaneous concentration and selective separation of 66 （ultra） trace persistent toxic substances in Antarctic waters. The substances included 30 polychlorinated biphenyls, 17 organochlorine pesticides, 16 polycyclic aromatic hydrocarbons, 3 hexabromocyclododecanes. Solid phase extraction was performed using a C18 membrane and silica gel column. Gradient elution was conducted using organic solvents with different polarities; as a result, the efficiency of the C18 film is improved and the interferences from impurities and target compounds are eliminated. Extracts were subsequently analyzed through gas chromatography or liquid and gas chromatography coupled to tandem mass spectrometry. Method validation yielded the following values： recoveries of all target analytes in the Antarctic water ranged from 87.3% to 117.6% and reproducibility as percent relative standard deviation was lower than 5%. Quantification limits ranged from 0.004 μg L^-1 to 0.030 μg L^-1. The established method improved the recoveries and reduced the limits of detection. Results indicated the method exhibited good performance in the simultaneous concentration and selective separation of 66 （ultra） trace organic pollutants; Therefore, the proposed sample pretreatment can potentially eliminate the effects of various classes of impurities to some extent.This study developed a method to perform the simultaneous concentration and selective separation of 66 （ultra） trace persistent toxic substances in Antarctic waters. The substances included 30 polychlorinated biphenyls, 17 organochlorine pesticides, 16 polycyclic aromatic hydrocarbons, 3 hexabromocyclododecanes. Solid phase extraction was performed using a C18 membrane and silica gel column. Gradient elution was conducted using organic solvents with different polarities; as a result, the efficiency of the C18 film is improved and the interferences from impurities and target compounds are eliminated. Extracts were subsequently analyzed through gas chromatography or liquid and gas chromatography coupled to tandem mass spectrometry. Method validation yielded the following values： recoveries of all target analytes in the Antarctic water ranged from 87.3% to 117.6% and reproducibility as percent relative standard deviation was lower than 5%. Quantification limits ranged from 0.004 μg L^-1 to 0.030 μg L^-1. The established method improved the recoveries and reduced the limits of detection. Results indicated the method exhibited good performance in the simultaneous concentration and selective separation of 66 （ultra） trace organic pollutants; Therefore, the proposed sample pretreatment can potentially eliminate the effects of various classes of impurities to some extent.

关 键 词：Polychlorinated biphenyls（PCBs） Organochlorine pesticides（OCPs） Polycyclic aromatic hydrocarbons（PAHs） Hexabromocyclododecanes（HBCDs） Solid phase extraction（SPE） Gradient elution 

分 类 号：X830[环境科学与工程—环境工程] O658.2[理学—分析化学]