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金属有机骨架纳米材料-固相萃取环境水样中亚硝胺类消毒副产物

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李小蒙, 王旭坤, 吴怡秋, 邵子纯, 邵煜晨, 陈坤, 高仕谦, 张占恩. 金属有机骨架纳米材料-固相萃取环境水样中亚硝胺类消毒副产物[J]. 环境化学, 2019, 38(6): 1258-1265. doi: 10.7524/j.issn.0254-6108.2018120603
引用本文: 李小蒙, 王旭坤, 吴怡秋, 邵子纯, 邵煜晨, 陈坤, 高仕谦, 张占恩. 金属有机骨架纳米材料-固相萃取环境水样中亚硝胺类消毒副产物[J]. 环境化学, 2019, 38(6): 1258-1265. doi: 10.7524/j.issn.0254-6108.2018120603
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LI Xiaomeng, WANG Xukun, WU Yiqiu, SHAO Zichun, SHAO Yuchen, CHEN Kun, GAO Shiqian, ZHANG Zhan. Determination of N-nitrosamines in water samples based on the solid-phase extraction with metal-organic framework[J]. Environmental Chemistry, 2019, 38(6): 1258-1265. doi: 10.7524/j.issn.0254-6108.2018120603
Citation: LI Xiaomeng, WANG Xukun, WU Yiqiu, SHAO Zichun, SHAO Yuchen, CHEN Kun, GAO Shiqian, ZHANG Zhan. Determination of N-nitrosamines in water samples based on the solid-phase extraction with metal-organic framework[J]. Environmental Chemistry, 2019, 38(6): 1258-1265. doi: 10.7524/j.issn.0254-6108.2018120603
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金属有机骨架纳米材料-固相萃取环境水样中亚硝胺类消毒副产物

  • 1.

    苏州科技大学 环境科学与工程学院, 苏州, 215009;

  • 2.

    郑州大学 化学与分子工程学院, 郑州, 450001;

  • 3.

    苏州科技大学天平学院 环境工程系, 苏州, 215009

  • 基金项目:

    江苏省高校自然科学研究重大项目（15KJA610003），苏州科技大学人才引进科研项目（331711204）和江苏省高等学校大学生创新创业训练计划（2018001）资助.

Determination of N-nitrosamines in water samples based on the solid-phase extraction with metal-organic framework

  • 1.

    School of Environmental Science and Engineering, Suzhou University of Science and Technology, Suzhou, 215009, China;

  • 2.

    School of Chemistry and Molecular Engineering, Zhengzhou University, Zhengzhou, 450001, China;

  • 3.

    School of Environmental Engineering, Tianping college of Suzhou University of Science and Technology, Suzhou, 215009, China

  • Fund Project: Supported by Major Projects of Natural Science Research in Universities in Jiangsu Province(15KJA610003), Suzhou University of Science and Technology Talent Introduction Research Project(331711204) and Innovation and Entrepreneurship Training Program for College Students in Jiangsu Province(2018001).

  • 摘要: 将通过水热合成法制备的金属有机骨架材料[MIL-101（Cr）]作为吸附剂应用于吸附环境水样中的亚硝胺类消毒副产物，采用超高效液相色谱-串联质谱法（UHPLC-MS/MS）进行测定.通过SEM、TEM和FT-IR技术对MIL-101（Cr）的表面形态和特征基团进行表征，并对影响萃取效率的主要因素，如MIL-101（Cr）的用量、萃取时间、水样的pH值和解吸条件等进行考察.研究表明，当MIL-101（Cr）用量为6.0 mg，pH=9.0，30℃下9 min内可达吸附平衡，回收率高于63.5%，3种亚硝胺的检出限为0.029-0.283 μg·L-1.将方法应用于环境水样的测定，加标回收率在77.9%-107.2%范围内，相对标准偏差低于5.4%.该方法操作简单快速、准确可靠、检出限低，可用于水样中痕量亚硝胺类消毒副产物的检测.
    Abstract: The metal-organic frameworks[MIL-101(Cr)] was synthesized by hydrothermal method and applied to the absorption of N-nitrosamines (NAs) in environmental water coupled with ultra high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS). The surface morphology was characterized by SEM, TEM and FT-IR. The experimental parameters of solid phase extraction were investigated including the amount of MIL-101(Cr), extraction time, sample pH and desorption conditions. The recoveries of NAs were over 63.5% within 9.0 min when the mass concentration of MIL-101(Cr) was 6.0 mg, the pH value of water sample was 9.0, the desorption temperature was 30℃. The detection limits were in the range of 0.029-0.238 μg·L-1. The developed method was successfully applied to the analysis of NAs in environmental water samples, the recoveries were in the range from 77.9% to 107.2% and the RSDs was within 5.4%. The proposed method was simple, rapid and accurate, which could be applied to the analysis of the trace amount NAs in environmental water samples.
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  • 收稿日期:  2018-12-06
  • 刊出日期:  2019-06-15

金属有机骨架纳米材料-固相萃取环境水样中亚硝胺类消毒副产物

  • 1.  苏州科技大学 环境科学与工程学院, 苏州, 215009;
  • 2.  郑州大学 化学与分子工程学院, 郑州, 450001;
  • 3.  苏州科技大学天平学院 环境工程系, 苏州, 215009
  • 收稿日期:  2018-12-06
基金项目:

江苏省高校自然科学研究重大项目（15KJA610003），苏州科技大学人才引进科研项目（331711204）和江苏省高等学校大学生创新创业训练计划（2018001）资助.

摘要: 将通过水热合成法制备的金属有机骨架材料[MIL-101（Cr）]作为吸附剂应用于吸附环境水样中的亚硝胺类消毒副产物，采用超高效液相色谱-串联质谱法（UHPLC-MS/MS）进行测定.通过SEM、TEM和FT-IR技术对MIL-101（Cr）的表面形态和特征基团进行表征，并对影响萃取效率的主要因素，如MIL-101（Cr）的用量、萃取时间、水样的pH值和解吸条件等进行考察.研究表明，当MIL-101（Cr）用量为6.0 mg，pH=9.0，30℃下9 min内可达吸附平衡，回收率高于63.5%，3种亚硝胺的检出限为0.029-0.283 μg·L-1.将方法应用于环境水样的测定，加标回收率在77.9%-107.2%范围内，相对标准偏差低于5.4%.该方法操作简单快速、准确可靠、检出限低，可用于水样中痕量亚硝胺类消毒副产物的检测.

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