氨基修饰磁性氧化石墨烯固相萃取-高效液相色谱/质谱法测定水中苯脲类除草剂

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英文篇名：Determination of Phenylurea Herbicides Residues in Water by an Amido Modified Magnetic Graphene Oxide Solid Phase Extraction-High Performance Liquid Chromatography/Mass Spectrometry 作者：刘小燕 ; 李欣悦 ; 高仕谦 ; 张占恩 英文作者：LIU Xiao-yan;LI Xin-yue;GAO Shi-qian;ZHANG Zhan-en;School of Environmental Science and Engineering,Suzhou University of Science and Technology;Innovation Center of Water Treatment Technology and Material Suzhou University of Science and Technology; 关键词：氨基修饰磁性氧化石墨烯 ; 苯脲类除草剂 ; 磁性固相萃取 ; 环境水样 英文关键词：Aminoated magnetic graphene oxide composites;;Phenylurea herbicides;;Magnetic solid-phase extraction;;Environmental water sample 中文刊名：FXKX 英文刊名：Journal of Analytical Science 机构：苏州科技大学环境科学与工程学院;苏州科技大学水处理技术与材料协同创新中心; 出版日期：2019-04-20 出版单位：分析科学学报 年：2019 期：v.35 基金：江苏省高校自然科学研究重大项目(No.15KJA610003);; 苏州科技大学青年基金(No.341511201);苏州科技大学人才引进科研项目(No.331511207) 语种：中文; 页：FXKX201902014 页数：5 CN：02 ISSN：42-1338/O 分类号：78-82

摘要

本实验建立了氨基修饰磁性氧化石墨烯固相萃取-高效液相色谱/质谱法测定环境水样中灭草隆、异丙隆、绿麦隆和敌草隆4种苯脲类除草剂的分析方法。采用恒温搅拌法将三乙酸四胺(TETA)修饰在氧化石墨烯(GO)片层上,并用共沉淀法合成磁性三乙酸四胺氧化石墨烯(MTGO),用傅里叶红外(FT-IR)光谱及扫描电镜(SEM)进行表征。磁性固相萃取的最优条件为:以甲醇为洗脱剂,MTGO的用量为15.0 mg,萃取时间为15 min。在最优条件下,4种目标苯脲类除草剂的检出限为0.03～0.05μg/L。用该方法对实际水样进行分析,加标回收率为84.3%～96.4%,相对标准偏差为3.9%～8.6%。本实验方法操作简单,检出限低,可以满足环境水样中痕量苯脲类除草剂的分析测定。
        Aminoated magnetic graphene oxide composites were synthesized and used as the adsorbent for the MSPE of four benzylurea herbicides from environmental water samples prior to HPLC/MS.The tetraocetuacid tetraamine(TETA) was modified on the graprene oxide(GO) layer by constant temperature agitation, and MTGO was synthesized by coprecipitation method,which was characterized by Fourier transform infrared spectroscopy scanning electron microscopy(FT-IR) and SEM.The optimized conditions about this method were as follows: methanol as elution solution, 15.0 mg MTGO as adsorbent, 15 min adsorption time.Under the conditions, the limits of detection of the method ranged from 0.03 to 0.05 μg/L.The method was applied to the analysis of the environmental water samples.The recoveries of the method were in the range from 84.3% to 96.4% and the relative standard deviations were 3.9%-8.6%. Owing to its simple and rapid operation, low detection limit and good reproducibility, this method can meet the determination of the trace residue of benzylurea herbicides in water samples.

引文

[1] LIU E M,SHENG W,HAN J,et al.Food and Machinery(刘恩梅,生威,韩静,等.食品与机械),2011,27(3):160.
    [2] FENG Y B,LI J,YANG S F,et al.Chemical Reagents(冯玉冰,李晶,杨顺风,等.化学试剂),2017,39(5):449.
    [3] Eichelberger J W,Lichtenberg J J.Environmental Science & Technology,1971,5(6):541.
    [4] ZHI J L,OU J F,CHEN M X,et al.China Environmental Monitoring(支建梁,欧菊芳,陈铭学,等.中国环境监测),2007,23(5):10.
    [5] PENG X J,PANG J S,DENG A H.Journal of Instrumental Analysis(彭晓俊,庞晋山,邓爱华.分析测试学报),2011,30(7):784.
    [6] ZHONG Q.Ionic Liauid Based Microwave-assisteel Extration of Triazine and Phenylurea Herbicides from Environmental Medium.Beijing:Beijing University of Chemical Technology(钟秋.离子液体-微波辅助萃取环境基质中的三嗪类和苯脲类除草剂.北京:北京化工大学),2012.
    [7] HUANG H Z,SUN M H,WANG S L,et al.Modern Food Technology(黄智鸿,孙茂红,王素利,等.现代食品科技),2016,(1):266.
    [8] WANG H X,LI Y Q,YONG L,et al.Chinese Journal of Chromatography(王和兴,黎源倩,雍莉,等.色谱),2007,25(4):536.
    [9] WU F,ZHANG Z E,ZHANG L.Modern Chemical Industry(吴飞,张占恩,张磊.现代化工),2016,(5):189.
    [10] XIAO L,WANG Y C,CHENG M R.Journal of Tea Science( 肖亮,王园朝,成美容.茶叶科学),2010,30(1):52.
    [11] LIN K Y A,Lee W D.Applied Surface Science,2016,361:114.