固相萃取-气相色谱质谱法测定水体中氯代多环芳烃
|
摘要
本研究建立了固相萃取-气相色谱质谱联用测定水体中6种Cl-PAHs的分析方法。采用poly-sery HLB固相萃取小柱对水样进行富集浓缩,用大体积采样器以2 mL/min的流速过柱,用6 mL的正己烷-二氯甲烷(4∶1,V/V)洗脱,气相色谱-质谱联用、选择离子扫描方式进行定性和定量分析,并采用内标定量法。在对应Cl-PAHs线性范围内的线性相关系数为0.9952~0.9997,检出限与定量限分别为0.013~0.592 ng/L和0.051~0.257 ng/L。除9-Cl Flu(加标回收率为34.4%~45.6%)外,其它Cl-PAHs的加标回收率为77.8%~105.4%。将本方法用于测定南京工业园区及周边水体中Cl-PAHs分析,测得其总浓度为23.594~106.374 ng/L。
In this work,a solid phase extraction( SPE) coupled with gas chromatography-mass spectrometry(SPE-GC-MS) method was developed for determination of 6 kinds of typical Cl-PAHs in water. The targets in water sample were concentrated by poly-sery HLB SPE cartridge and passed through the cartridge with a bulk sampler at a flow rate of 2 mL/min,and then eluted by 6 mL of n-hexane/dichloromethane(4∶ 1,V/V). The Cl-PAHs were qualified and quantified by GC-MS in selective ion scan monitoring method( SIM). Good linearity was observed in the range of 1 to 1000 ng/mL Cl-PAHs with correlation coefficients of 0.9952-0.9997. The limits of detection and limits of quantification ranged from 0.013 to 0. 592 ng/L and 0. 051 to0.257 ng/L,respectively. Spiked recoveries in pure water ranged from 77. 8% to 105. 4%,with the rlative standard deviations of less than 10%,except 9-Cl Flu,with the spiked recoveries ranging from 34. 4% to 45.6%. The results indicated that the SPE-GC-MS analytical method established here was sensitive and accurate for determination of Cl-PAHs in surface water samples. Then the method was applied to analyze Cl-PAHs in water samples collected from Nanjing industrial Park and surrounding areas,and it was found that the total concentration of Cl-PAHs was ranging from 23.594 ng/L to 106.374 ng/L.
In this work,a solid phase extraction( SPE) coupled with gas chromatography-mass spectrometry(SPE-GC-MS) method was developed for determination of 6 kinds of typical Cl-PAHs in water. The targets in water sample were concentrated by poly-sery HLB SPE cartridge and passed through the cartridge with a bulk sampler at a flow rate of 2 mL/min,and then eluted by 6 mL of n-hexane/dichloromethane(4∶ 1,V/V). The Cl-PAHs were qualified and quantified by GC-MS in selective ion scan monitoring method( SIM). Good linearity was observed in the range of 1 to 1000 ng/mL Cl-PAHs with correlation coefficients of 0.9952-0.9997. The limits of detection and limits of quantification ranged from 0.013 to 0. 592 ng/L and 0. 051 to0.257 ng/L,respectively. Spiked recoveries in pure water ranged from 77. 8% to 105. 4%,with the rlative standard deviations of less than 10%,except 9-Cl Flu,with the spiked recoveries ranging from 34. 4% to 45.6%. The results indicated that the SPE-GC-MS analytical method established here was sensitive and accurate for determination of Cl-PAHs in surface water samples. Then the method was applied to analyze Cl-PAHs in water samples collected from Nanjing industrial Park and surrounding areas,and it was found that the total concentration of Cl-PAHs was ranging from 23.594 ng/L to 106.374 ng/L.
引文
1 YANG Yong-Liang,PAN Jing,ZHU Xiao-Hua,LIU Xian-De,CHEN Da-Zhou.Chinese J.Environ.Chem.,2009,28(2):276-283杨永亮,潘静,朱晓华,刘咸德,陈大舟.环境化学,2009,28(2):276-283
2 Ishaq R,Nf C,Zebühr Y,Broman D,Jrnberg U.Chemosphere,2003,50(9):1131-1150
3 Fernando S,Jobst K J,Taguchi V Y,Helm P A,Reiner E J,Mccarry B E.Environ.Sci.Technol.,2014,48(18):10656-10663
4 Nishimura C,Horii Y,Tanaka S,Asante K A,Ballesteros F,Viet P H,Itai T K,Takigami H,Tanabe S,Fujimori T.Environ.Pollut.,2017,225:252-260
5 Jin R,Liu G,Zheng M,Jiang X,Zhao Y,Yang L,Wu X,Xu Y.Environ.Sci.Technol.,2017,51(14):7945-7953
6 Pinto M,Rebola M,Louro H,Antunes A M M,JoséS S,Rocha M.Polycyclic Aromat.Compd.,2014,34(4):356-371
7 Ohura T.Sci.World J.,2007,7:372-380
8 Sun J L,Zeng H,Ni H G.Chemosphere,2013,90(6):1751-1759
9 SUN Jian-Lin,CHANG Wen-Jing,CHEN Zheng-Xia,ZENG Hui.Chinese J.Environ.Sci.,2015,36(5):1513-1522孙建林,常文静,陈正侠,曾辉.环境科学,2015,36(5):1513-1522
10 Jin R,Zheng M H,Yang H B,Yang L L,Wu X L,Xu Y,Liu G R.Environ.Pollut.,2017,231:1601-1608
11 Oyler A R,Liukkonen R J,Lukasewycz M T,Heikkila K E,Cox D A,Carlson R M.Environ.Sci.Technol.,1983,17(6):334-342
12 Shiraishi H,Pilkington N H,Otsuki A,Fuwa K.Environ.Sci.Technol.,1985,19(7):585-590
13 Li J,Yu N,Zhang B,Jin L,Li M,Hu M,Zhang X,Wei S,Yu H.Water Res.,2014,54:53-61
14 Zimmers S M,Browne E P,O’Keefe P W,Anderton D L,Kramer L,Reckhow D A,Arcaro K F.Chemosphere,2014,104:237-243
15 ZHENG Ji-San,MA Jing,Horii Y,Kannan K,Ohura T,XU Gang,WU Ming-Hong.Chinese J.Environ.Chem.,2012,31(7):1101-1107郑继三,马静,Horii Y,Kannan K,Ohura T,徐刚,吴明红.环境化学,2012,31(7):1101-1107
16 Horii Y,Ohura T,Yamashita N,Kannan K.Arch.Environ.Contam.Toxicol.,2009,57(4):651-660
17 Tue N M,Goto A,Takahashi S,Itai T,Asante K A,Nomiyama K,Tanabe S,Kunisue T.J.Mater.Cycles Waste Manage.,2017,19(4):1324-1332
18 MO Li-Gui,MA Sheng-Tao,LI Hui-Ru,YU Zhi-Qiang,SHENG Guo-Ying,FU Jia-Mo.Chinese J.Anal.Chem.,2013,41(12):1825-1830莫李桂,马盛韬,李会茹,于志强,盛国英,傅家谟.分析化学,2013,41(12):1825-1830
19 WANG Shu-Tao,ZHENG Ya-Nan,WANG Zhi-Fang,YUAN Yuan-Yuan,MA Xiao-Qing,YANG Xue-Ying.Chinese J.Luminescence,2017,38(6):807-813王书涛,郑亚南,王志芳,苑媛媛,马晓晴,杨雪莹.发光学报,2017,38(6):807-813
20 Wang X,Kang H,Wu J.J.Sep.Sci.,2016,39(9):1742-1748
2 Ishaq R,Nf C,Zebühr Y,Broman D,Jrnberg U.Chemosphere,2003,50(9):1131-1150
3 Fernando S,Jobst K J,Taguchi V Y,Helm P A,Reiner E J,Mccarry B E.Environ.Sci.Technol.,2014,48(18):10656-10663
4 Nishimura C,Horii Y,Tanaka S,Asante K A,Ballesteros F,Viet P H,Itai T K,Takigami H,Tanabe S,Fujimori T.Environ.Pollut.,2017,225:252-260
5 Jin R,Liu G,Zheng M,Jiang X,Zhao Y,Yang L,Wu X,Xu Y.Environ.Sci.Technol.,2017,51(14):7945-7953
6 Pinto M,Rebola M,Louro H,Antunes A M M,JoséS S,Rocha M.Polycyclic Aromat.Compd.,2014,34(4):356-371
7 Ohura T.Sci.World J.,2007,7:372-380
8 Sun J L,Zeng H,Ni H G.Chemosphere,2013,90(6):1751-1759
9 SUN Jian-Lin,CHANG Wen-Jing,CHEN Zheng-Xia,ZENG Hui.Chinese J.Environ.Sci.,2015,36(5):1513-1522孙建林,常文静,陈正侠,曾辉.环境科学,2015,36(5):1513-1522
10 Jin R,Zheng M H,Yang H B,Yang L L,Wu X L,Xu Y,Liu G R.Environ.Pollut.,2017,231:1601-1608
11 Oyler A R,Liukkonen R J,Lukasewycz M T,Heikkila K E,Cox D A,Carlson R M.Environ.Sci.Technol.,1983,17(6):334-342
12 Shiraishi H,Pilkington N H,Otsuki A,Fuwa K.Environ.Sci.Technol.,1985,19(7):585-590
13 Li J,Yu N,Zhang B,Jin L,Li M,Hu M,Zhang X,Wei S,Yu H.Water Res.,2014,54:53-61
14 Zimmers S M,Browne E P,O’Keefe P W,Anderton D L,Kramer L,Reckhow D A,Arcaro K F.Chemosphere,2014,104:237-243
15 ZHENG Ji-San,MA Jing,Horii Y,Kannan K,Ohura T,XU Gang,WU Ming-Hong.Chinese J.Environ.Chem.,2012,31(7):1101-1107郑继三,马静,Horii Y,Kannan K,Ohura T,徐刚,吴明红.环境化学,2012,31(7):1101-1107
16 Horii Y,Ohura T,Yamashita N,Kannan K.Arch.Environ.Contam.Toxicol.,2009,57(4):651-660
17 Tue N M,Goto A,Takahashi S,Itai T,Asante K A,Nomiyama K,Tanabe S,Kunisue T.J.Mater.Cycles Waste Manage.,2017,19(4):1324-1332
18 MO Li-Gui,MA Sheng-Tao,LI Hui-Ru,YU Zhi-Qiang,SHENG Guo-Ying,FU Jia-Mo.Chinese J.Anal.Chem.,2013,41(12):1825-1830莫李桂,马盛韬,李会茹,于志强,盛国英,傅家谟.分析化学,2013,41(12):1825-1830
19 WANG Shu-Tao,ZHENG Ya-Nan,WANG Zhi-Fang,YUAN Yuan-Yuan,MA Xiao-Qing,YANG Xue-Ying.Chinese J.Luminescence,2017,38(6):807-813王书涛,郑亚南,王志芳,苑媛媛,马晓晴,杨雪莹.发光学报,2017,38(6):807-813
20 Wang X,Kang H,Wu J.J.Sep.Sci.,2016,39(9):1742-1748
© 2004-2018 中国地质图书馆版权所有 京ICP备05064691号 京公网安备11010802017129号 地址：北京市海淀区学院路29号 邮编：100083 电话：办公室：(+86 10)66554848；文献借阅、咨询服务、科技查新：66554700 |