以ZIF-8为固相微萃取涂层分析环境水样中痕量多溴联苯醚
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摘要
将沸石咪唑酯骨架材料(ZIF-8)制成固相微萃取涂层,结合气相色谱-三重四极杆串联质谱联用仪(GC-MS/MS),建立了一种快速灵敏分析环境水样中6种痕量多溴联苯醚的方法。采用单因素优化实验得到的最优条件为:不添加Na Cl,萃取温度为50℃,萃取时间为50 min,p H值为7.0,解吸时间和解吸温度分别为5 min和280℃。在最优条件下,该方法测定水样中多溴联苯醚的线性范围为1~1 000 ng/L,检出限为0.08~2.29 ng/L,定量下限为0.23~7.32 ng/L。日内和日间相对标准偏差分别为4.3%~6.5%和6.9%~9.3%。将该方法应用于4种实际环境水样(自来水、泉水、池塘水和垃圾填埋场废水)中多溴联苯醚的检测,回收率为81.6%~109%。
A rapid and sensitive method was developed for the analysis of 6 polybrominated biphenyl ethers( PBDEs) at trace levels in environmental water samples by gas chromatography-tandem mass spectrometry( GC-MS/MS) with a synthesized zeolite imidazolate framework-8( ZIF-8) as solid phase microextraction coating.The experimental conditions were optimized with single factor tests,and the optimal conditions were as follows:extraction time:50 min,extraction temperature:50 ℃,p H value:7.0,desorption temperature:280 ℃,desorption time:5 min,and without salt addition.Under the optimized conditions,the calibration curves for 6 PBDEs were linear in the range of1-1 000 ng/L with limits of detection and limits of quantitation of 0.08-2.29 ng/L and 0.23-7.32 ng/L,respectively.The intra-day and inter-day RSDs were in the range of 4.3%-6.5% and6.9%-9.3%,respectively.This method was successfully applied in the analysis of PBDEs in 4 environmental water samples( tap water,spring water,pond water and landfill waste water) with recoveries of 81.6%-109%.
A rapid and sensitive method was developed for the analysis of 6 polybrominated biphenyl ethers( PBDEs) at trace levels in environmental water samples by gas chromatography-tandem mass spectrometry( GC-MS/MS) with a synthesized zeolite imidazolate framework-8( ZIF-8) as solid phase microextraction coating.The experimental conditions were optimized with single factor tests,and the optimal conditions were as follows:extraction time:50 min,extraction temperature:50 ℃,p H value:7.0,desorption temperature:280 ℃,desorption time:5 min,and without salt addition.Under the optimized conditions,the calibration curves for 6 PBDEs were linear in the range of1-1 000 ng/L with limits of detection and limits of quantitation of 0.08-2.29 ng/L and 0.23-7.32 ng/L,respectively.The intra-day and inter-day RSDs were in the range of 4.3%-6.5% and6.9%-9.3%,respectively.This method was successfully applied in the analysis of PBDEs in 4 environmental water samples( tap water,spring water,pond water and landfill waste water) with recoveries of 81.6%-109%.
引文
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[3]Shang X H,Dong G X,Zhang H X,Zhang L,Yu X W,Li J G,Wang X Y,Yue B,Zhao Y F,Wu Y N.Food Control,2016,67:240-246.
[4]Sun J D,Pan L L,Zhan Y,Lu H N,Tasang D C,Liu W X,Wang X L,Li X D,Zhu L Z.Sci.Total Environ.,2016,544:670-676.
[5]Fontana A R,Silva M F,Mart2Nez L D,Wuilloud R G,Altamirano J C.J.Chromatogr.A,2009,1216(20):4339-4346.
[6]PietrońW J,Mańagocki P.Talanta,2017,167:411-427.
[7]Li J X,Sun M Y,Hu X Y,Wu X Q,Chang Q Y,Fan C L.J.Instrum.Anal.(李建勋,孙梦园,胡雪艳,吴兴强,常巧英,范春林.分析测试学报),2017,36(11):1339-1345.
[8]He J,Li T,Dong M Y,Dong N.J.Instrum.Anal.(何静,李涛,董美玉,董南.分析测试学报),2017,36(10):1185-1190.
[9]Zhao R S,Wang X,Yan J P,Wang X D.J.Sep.Sci.,2009,32(4):630-636.
[10]Jiang X Y,Zhang H,Chen X Q.Microchem.Acta,2011,175:341-346.
[11]Li Q L,Wang X,Liu Y L,Chen X F,Wang M L,Zhao R S.J.Chromatogr.A,2014,1374:58-65.
[12]Gong S X,Wang X,Chen Y,Cheng C G,Wang M L,Zhao R S.J.Chromatogr.A,2015,1401:17-23.
[13]Shi Q,Chen Z,Song Z,Li J,Dong J.Angew.Chem.Int.Ed.,2011,123(3):698-701.
[14]Phan A,Doonan C J,Uriberomo F J,Knobler C B,O'Keeffe M,Yaghi O M.Acc.Chem.Res.,2010,43(1):58-67.
[15]Seoane B,Zamaro J M,Tellez C,Coronas J.Cryst Eng Comm.,2012,4(9):3103-3107.
[16]Ge D,Lee H K.J.Chromatogr.A,2011,1218(47):8490-8495.
[17]Huang J,Ou C,Lv F,Cao Y,Tang H,Zhou Y,Gan N.Talanta,2017,65:326-331.
[18]Lan H,R9nkk9 T,Parshintsev J,Hartonen K,Ning G,Sakeye M,Sarfraz J,Riekkola M L.J.Chromatogr.A,2016,1486:76-85.
[19]Zhang J,Zhang W,Bao T,Chen Z.J.Chromatogr.A,2015,1388:9-16.
[20]Park K S,Ni Z,C^otéA P,Choi J Y,Huang R,Uribe Romo F J,Chae H K,O'Keeffe M,Yaghi M.Proc.Natl.Acad.Sci.USA,2006,103(27):10186-10191.
[21]Schejn A,Balan L,Falk V,Aranda L,Medjahdi G,Schneider R.Cryst Eng Comm.,2014,16(21):4493-4500.
[22]Hu Y,Kazemian H,Rohani S,Huang Y,Song Y.Chem.Commun.,2011,47(47):12694-12696.
[23]Ouyang G,Vuckovic D,Pawliszyn J.Chem.Rev.,2011,111(4):2784-2814.
[24]Yu H,Zhao Y F,Yang L X,Chen X F.Anal.Methods,2017,48:6808-6813.
[25]Zhang H,Lee H K.J.Chromatogr.A,2011,1218(28):4509-4516.
[26]Naing N N,Li S F,Lee H K.J.Chromatogr.A,2016,1458:25-34.
[27]Wang J X,Jiang D Q,Gu Z Y,Yan X P.J.Chromatogr.A,2006,1137(1):8-14.