基于分子印迹磁性复合材料的基质分散-固相萃取/液相色谱法测定海水中的氯酚类污染物
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摘要
建立了一种快速、高效、灵敏的基质分散-磁性固相萃取/液相色谱(d MSPE-HPLC)方法,用于海水中5种氯酚类(CPs)污染物残留量的测定。样品用五氯酚分子印迹氨基功能化磁性复合材料富集,在C8反相液相色谱柱(250 mm×4.6 mm×5.0μm)上分离,以甲醇-5 mmol/L乙酸铵水溶液(体积比70∶30)为流动相,230 nm处检测。考察了样品p H值、萃取时间和洗脱剂的种类与用量对CPs富集回收率的影响。结果表明,在最佳实验条件下,5种CPs在1~5 000 ng/L浓度范围内呈良好的线性关系,相关系数(r2)均大于0.998 9;平均回收率为86.5%~98.8%,相对标准偏差(RSDs)为0.8%~8.6%;检出限(LODs)为0.18~1.20 ng/L,定量下限(LOQs)为0.6~4.0 ng/L。方法可用于海水中CPs类化合物的快速筛查和确证分析。
A rapid,sensitive and accurate method for the simultaneous determination of 5 kinds of chlorophenols( CPs) in seawater samples by dispersive magnetic solid phase extraction- liquid chromatography( d MSPE- HPLC) was developed. The seawater samples were firstly enriched with pentachlorophenol-imprinted amino-functionalized nano-Fe3O4-polymer magnetic composite material( n Fe3O4@ MIPNH2- polymer),then separated on a C8 analytic column( 250 mm × 4. 6 mm × 5. 0μm) using methanol- NH4 Ac solution( 70 ∶ 30) as mobile phase and detected at 230 nm via UV detector. The results showed that under the optimal condition,the calibration curves were linear in the range of 1- 5 000 ng / L with correlation coefficients( r2) higher than 0. 998 9 for target chlorophenols. The spiked recoveries were between 86. 5% and 98. 8% with relative standard deviations( RSDs) of 0. 8%- 8. 6%. The limits of detection( LODs) were in the range of 0. 18- 1. 20 ng / L and the limits of quantitation( LOQs) were between 0. 6 ng / L and 4. 0 ng / L. The developed method could be applied in the routine analysis of chlorophenols in seawater samples.
A rapid,sensitive and accurate method for the simultaneous determination of 5 kinds of chlorophenols( CPs) in seawater samples by dispersive magnetic solid phase extraction- liquid chromatography( d MSPE- HPLC) was developed. The seawater samples were firstly enriched with pentachlorophenol-imprinted amino-functionalized nano-Fe3O4-polymer magnetic composite material( n Fe3O4@ MIPNH2- polymer),then separated on a C8 analytic column( 250 mm × 4. 6 mm × 5. 0μm) using methanol- NH4 Ac solution( 70 ∶ 30) as mobile phase and detected at 230 nm via UV detector. The results showed that under the optimal condition,the calibration curves were linear in the range of 1- 5 000 ng / L with correlation coefficients( r2) higher than 0. 998 9 for target chlorophenols. The spiked recoveries were between 86. 5% and 98. 8% with relative standard deviations( RSDs) of 0. 8%- 8. 6%. The limits of detection( LODs) were in the range of 0. 18- 1. 20 ng / L and the limits of quantitation( LOQs) were between 0. 6 ng / L and 4. 0 ng / L. The developed method could be applied in the routine analysis of chlorophenols in seawater samples.
引文
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[5]Ding Z Q,Zhang Q Y.Chin.J.Anal.Chem.(丁宗庆,张琼瑶.分析化学),2010,38(10):1400-1404.
[6]Ki M D,Han J,Cho I Y.Anal.Bioanal.Chem.,2013,405(1):377-387.
[7]Zhou C H,Tong S S,Chang Y X,Jia X,Zhou W H.Electrophoresis,2012,33(8):1331-1338.
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[11]Peng L,Wang Y Z,Zeng H,Yuan Y.Analyst,2011,136:756-763.
[12]Oriol B,Montserrat L,Cristina P,Cristina P,Franck L D,Florence P K.Anal.Methods,2013,5:6297-6305.
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[15]Ozkutuk E B,Ersoz A,Denizli A,Say R.J.Hazard.Mater.,2008,157:130-136.
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[20]López-Jiménez F J,Rubio S,Pérez-Bendito D.J.Chromatogr.A,2008,1195:25-33.
[21]Guo L,Lee H K.J.Chromatogr.A,2011,1218:4299-4306.
[22]Marchese S,Gentili A,Perret D,Sergi M,Notari S.Chromatographia,2004,59:411-417.
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[25]Li J,Zhao X,Shi Y,Cai Y,Mou S,Jiang G.J.Chromatogr.A,2008,1180:24-31.
[26]Pan S D,Zhou L X,Zhao Y G,Chen X H,Shen H Y,Cai M Q,Jin M C.J.Chromatogr.A,2014,1362:34-42.