高级搜索

分子印迹-固相萃取-气相色谱-质谱联用测定沉积物中的16种邻苯二甲酸酯

,  ,  ,  ,  ,  , 

downloadPDF

上一篇

下一篇

刘奇鹰, 施航, 郭远明, 孙秀梅, 郭建波, 程鑫, 张露. 分子印迹-固相萃取-气相色谱-质谱联用测定沉积物中的16种邻苯二甲酸酯[J]. 环境化学, 2018, 37(6): 1376-1381. doi: 10.7524/j.issn.0254-6108.2017082301
引用本文: 刘奇鹰, 施航, 郭远明, 孙秀梅, 郭建波, 程鑫, 张露. 分子印迹-固相萃取-气相色谱-质谱联用测定沉积物中的16种邻苯二甲酸酯[J]. 环境化学, 2018, 37(6): 1376-1381. doi: 10.7524/j.issn.0254-6108.2017082301
shu
LIU Qiying, SHI Hang, GUO Yuanming, SUN Xiumei, GUO Jianbo, CHENG Xin, ZHANG Lu. Determination of 16 phthalic acid esters (PAEs) in sediments by molecularly imprinted solid phase extraction coupled with gas chromatography-mass spectrometry[J]. Environmental Chemistry, 2018, 37(6): 1376-1381. doi: 10.7524/j.issn.0254-6108.2017082301
Citation: LIU Qiying, SHI Hang, GUO Yuanming, SUN Xiumei, GUO Jianbo, CHENG Xin, ZHANG Lu. Determination of 16 phthalic acid esters (PAEs) in sediments by molecularly imprinted solid phase extraction coupled with gas chromatography-mass spectrometry[J]. Environmental Chemistry, 2018, 37(6): 1376-1381. doi: 10.7524/j.issn.0254-6108.2017082301
shu

分子印迹-固相萃取-气相色谱-质谱联用测定沉积物中的16种邻苯二甲酸酯

  • 1.

    浙江海洋大学水产学院, 舟山, 310022;

  • 2.

    浙江省海洋水产研究所浙江海洋大学海洋与渔业研究所, 舟山, 316100;

  • 3.

    西部矿业股份有限公司锡铁岎公司, 海西, 816203

  • 基金项目:

    国家自然科学基金青年基金（21407127）和浙江省科技厅院所专项（2016F30021）资助.

Determination of 16 phthalic acid esters (PAEs) in sediments by molecularly imprinted solid phase extraction coupled with gas chromatography-mass spectrometry

  • 1.

    Zhejiang Ocean University, Zhoushan, 310022, China;

  • 2.

    Zhejiang Ocean Fisheries Research Institute, Zhoushan, 316100, China;

  • 3.

    Western Mining Co., Ltd Xitieshan Branch, Haixi, 816203, China

  • Fund Project: Supported by the National Natural Science Foundation of China (21407127)and Institute of Science and Technology of Zhejiang Province Special(2016F30021).

  • 摘要: 采用分子印迹技术，以α甲基丙烯酸（α-MAA）为功能单体，三氯甲烷为致孔剂，邻苯二甲酸二甲酯（dimethyl phthalate，DMP）为模板制备的分子印迹柱（MIPs-SPE）用来富集和净化沉积物中的邻苯二甲酸酯（phthalic acid esters，PAEs）.依次采用5 mL二氯甲烷、5 mL二氯甲烷、10 mL乙酸乙酯对沉积物进行液-固萃取.以分子印迹聚合物（MIPs）填充小柱，5 mL甲醇活化，3 mL甲醇-乙腈（1∶1，V/V）作为淋洗液，3 mL甲醇作为洗脱液，气相色谱-串联质谱方法测定采集的沉积物，外标法定量，宁波市杭州湾沉积物PAEs含量为28.0—125.6 ng·g-1，16种PAEs回收率在68%—109%，相对标准偏差在1.8%—11.2%之间，检出限为0.046—4.280 ng·g-1.
    Abstract: Molecular imprinting (MIP) technique was used to detect 16 PAEs in sediments. MIPs were prepured with functional monomer (α-MAA), porogen (chloroform) and template (dimethyl phthalate,DMP). The MIPs were used to enrich and purify the PAEs in sediments. 5 mL methylene chloride sdution, 5 mL methylene chloride solution, and 10 mL ethyl acetate were used for liqud-solid exlration of the sediment. The maximun recovery (86%-114%) of imprinting solid-phese extration MISPE was achieved using 5 mL methanol as activating solution, 3 mL methanol-acetonitrile (1:1, V/V) as washing solution and 3 mL methanol as elution solution. Then the concentrations of PAEs from the sediments of Hangzhou Bay in Ningbo city were determined to be 28.0-125.6 ng·g-1, respectively, under the optimum conditions of washing and elution, RSD was 1.8%-11.2%, and recovery was 68%-109%. The detection limit was 0.046-4.280 ng·g-1, respectively, indicated good LOD and high precision.
  • 加载中
  • [1] 王立鑫, 杨旭. 邻苯二甲酸酯毒性及健康效应研究进展[J]. 环境与健康杂志, 2010, 27(3):276-281.

    WANG L X, YANG X. Advances in toxicity and health effects of phthalates[J]. Journal of Environment and Health, 2010, 27(3):276-281(in Chinese).

    [2] 赵雅辉, 王小逸, 林兴桃, 等. 邻苯二甲酸酷类化合物的体内代谢及毒性研究进展[J]. 环境与健康杂志, 2010, 27(2):184-187.

    ZAHO Y H, WANG X Y, LIN X T, et al. Advances in studies on in vivo metabolism and toxicity of phthalic acid cool compounds[J]. Journal of Environment and Health, 2010, 27(2):184-187(in Chinese).

    [3] FOX G A. Effects of endocrine disruption chemicals on wild life in Canada:Past, present and future[J]. Water Quality Research Journal of Canada, 2001,36(2):233-251.
    [4] 王超英, 李碧芳, 李攻科. 固相微萃取/高效液相色谱联用分析水样中邻苯二甲酸酯[J]. 分析测试学报, 2005, 24(5):35-38.

    WANG C Y, LI B F, LI G K. Analysis of phthalates in water samples by solid phase microextraction and high performance liquid chromatography[J]. Journal of Analytical Science, 2005, 24(5):35-38(in Chinese).

    [5] 高晨晨. 海水中邻苯二甲酸酯类增塑剂的检测方法及应用研究[D]. 青岛:中国海洋大学, 2015:1-15. GAO C C. Study on the Detection Method and application of phthalate plasticizer in seawater[D]. Qingdao:China Ocean University, 2015:1

    -15(in Chinese).

    [6] 徐善浩, 邬蓓蕾, 袁丽凤等. 气相色谱-质谱法测定洗涤用品中6种邻苯二甲酸酯[J]. 理化检验-化学分册, 2016(3):1-4. XU S H, WU B Q, YUAN L F, et al. Determination of six phthalates in washing products by gas chromatography-mass spectrometry[J].Physical Testing and Chemical Analysis Part B(Chemical Analysis), 2016

    (3):1-4(in Chinese).

    [7] 韦寿莲, 郭小军, 严子君等. 邻苯二甲酸二(2-丙基)庚酯分子印迹固相萃取剂的制备及其应用[J]. 色谱, 2014, 32(5):458-463.

    WEI X L, GUO X J, YAN Y J, et al. Preparation and application of molecular imprinted solid phase extraction agent of Di (2-propyl) heptyl Phthalate[J]. Chinese Journal of Chromatography, 2014, 32(5):458-463(in Chinese).

    [8] 薛敏, 王安, 王瑜等. 分子印迹固相萃取技术检测江水、尿液及牛奶中雌激素残留[J]. 分析化学, 2011, 39(6):793-798.

    XUE M, WANG A, WANG Y, et al. Application of molecularly imprinted solid phase extraction for determination of estrogens in river water,Milk and Urine Samples[J]. Chinese Journal of Analytical Chemistry, 2011, 39(6):793-798(in Chinese).

    [9] 齐沛沛. 分子印迹技术分离纯化痕量环境污染物[D]. 大连:中国科学院大连化学物理研究所,2011:68. QI P P.Separation and purification of trace environmental pollutants with molecular imprinting technique[D]. Dalian:Dalian Institute of Chemical Physics, 2011:68(in Chinese).
    [10] 崔学慧,李炳华,陈鸿汉等. 中国土壤与沉积物中邻苯二甲酸酯污染水平及其吸附研究进展[J]. 生态环境学报,2010,19(2):472-479.

    CUI X H, LI B H, CHEN H H, et al. China phthalates in soil and sediment pollution level and adsorption were reviewed[J]. Ecology and Environmental Sciences,2010,19(2):472-479(in Chinese).

  • 加载中
WeChat 点击查看大图
计量
  • 文章访问数:  1178
  • HTML全文浏览数:  1156
  • PDF下载数:  147
  • 施引文献:  0
出版历程
  • 收稿日期:  2017-08-23
  • 刊出日期:  2018-06-15
刘奇鹰, 施航, 郭远明, 孙秀梅, 郭建波, 程鑫, 张露. 分子印迹-固相萃取-气相色谱-质谱联用测定沉积物中的16种邻苯二甲酸酯[J]. 环境化学, 2018, 37(6): 1376-1381. doi: 10.7524/j.issn.0254-6108.2017082301
引用本文: 刘奇鹰, 施航, 郭远明, 孙秀梅, 郭建波, 程鑫, 张露. 分子印迹-固相萃取-气相色谱-质谱联用测定沉积物中的16种邻苯二甲酸酯[J]. 环境化学, 2018, 37(6): 1376-1381. doi: 10.7524/j.issn.0254-6108.2017082301
shu
LIU Qiying, SHI Hang, GUO Yuanming, SUN Xiumei, GUO Jianbo, CHENG Xin, ZHANG Lu. Determination of 16 phthalic acid esters (PAEs) in sediments by molecularly imprinted solid phase extraction coupled with gas chromatography-mass spectrometry[J]. Environmental Chemistry, 2018, 37(6): 1376-1381. doi: 10.7524/j.issn.0254-6108.2017082301
Citation: LIU Qiying, SHI Hang, GUO Yuanming, SUN Xiumei, GUO Jianbo, CHENG Xin, ZHANG Lu. Determination of 16 phthalic acid esters (PAEs) in sediments by molecularly imprinted solid phase extraction coupled with gas chromatography-mass spectrometry[J]. Environmental Chemistry, 2018, 37(6): 1376-1381. doi: 10.7524/j.issn.0254-6108.2017082301
shu

分子印迹-固相萃取-气相色谱-质谱联用测定沉积物中的16种邻苯二甲酸酯

  • 1.  浙江海洋大学水产学院, 舟山, 310022;
  • 2.  浙江省海洋水产研究所浙江海洋大学海洋与渔业研究所, 舟山, 316100;
  • 3.  西部矿业股份有限公司锡铁岎公司, 海西, 816203
  • 收稿日期:  2017-08-23
基金项目:

国家自然科学基金青年基金（21407127）和浙江省科技厅院所专项（2016F30021）资助.

摘要: 采用分子印迹技术，以α甲基丙烯酸（α-MAA）为功能单体，三氯甲烷为致孔剂，邻苯二甲酸二甲酯（dimethyl phthalate，DMP）为模板制备的分子印迹柱（MIPs-SPE）用来富集和净化沉积物中的邻苯二甲酸酯（phthalic acid esters，PAEs）.依次采用5 mL二氯甲烷、5 mL二氯甲烷、10 mL乙酸乙酯对沉积物进行液-固萃取.以分子印迹聚合物（MIPs）填充小柱，5 mL甲醇活化，3 mL甲醇-乙腈（1∶1，V/V）作为淋洗液，3 mL甲醇作为洗脱液，气相色谱-串联质谱方法测定采集的沉积物，外标法定量，宁波市杭州湾沉积物PAEs含量为28.0—125.6 ng·g-1，16种PAEs回收率在68%—109%，相对标准偏差在1.8%—11.2%之间，检出限为0.046—4.280 ng·g-1.

English Abstract

    全文HTML

参考文献 (10)

返回顶部

目录

/

返回文章
返回

Copyright © 2019 中国科学院生态环境研究中心