广西师范大学学报（自然科学版） ›› 2015, Vol. 33 ›› Issue (4): 108-114.doi: 10.16088/j.issn.1001-6600.2015.04.018

• • 上一篇    下一篇

磁固相萃取快速测定环境水样中莠去津和扑草净

李云荣, 吴昊, 田婷婷, 袁晋, 刘莉芳, 米伟, 常银霞, 杜黎明   

  1. 山西师范大学化学与材料科学学院,山西临汾041004
  • 收稿日期:2015-06-01 出版日期:2015-12-25 发布日期:2018-09-21
  • 通讯作者: 杜黎明(1949—),男,山西临猗人,山西师范大学教授,博导。E-mail: lmd@dns.sxnu.edu.cn
  • 基金资助:
    国家自然科学基金资助项目(81402895);山西省青年科学基金资助项目(2014021018-3)

Fast Determination of Atrazine and Prometryn in Environmental Water Sample by Magnetic Solid Phase Extraction

LI Yun-rong, WU Hao, TIAN Ting-ting, YUAN Jin, LIU Li-fang, MI Wei, CHANG Yin-xia, DU Li-ming   

  1. School of Chemistry and Material Science, Shanxi Normal University, Linfen Shanxi 041004, China
  • Received:2015-06-01 Online:2015-12-25 Published:2018-09-21

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摘要： 采用溶剂热法一步合成得到硅藻土-还原石墨烯-四氧化三铁磁性材料,并将其作为磁固相萃取的吸附剂,结合高效液相色谱对环境水样中的莠去津和扑草净进行测定。对磁性材料的种类、样品溶液pH、磁性材料的用量、吸附时间、解析液的种类以及解析时间等对萃取率的影响因素进行了优化。在最佳条件下,莠去津和扑草净的线性相关系数分别为0.999 5和0.999 6,线性范围分别为0.5~120 μg/L和1~120 μg/L,检出限分别为0.055 μg/L和0.04 μg/L,样品的加标回收率是95.2%~103%。实验结果表明该方法可以成功地用于环境水样中的莠去津和扑草净的准确测定。

关键词: 磁固相萃取, 莠去津, 扑草净, 高效液相色谱, 环境水样

Abstract: Diatomite/reduced graphene oxide/ magnetite composites were synthesized by a new method and were used as an adsorbent for the magnetic solid phase extraction. Combing with high-performance liquid chromatography-UV, atrazine and prometryn were measured in environmented water. The effects of various experimental parameters, such as the kinds and amount of magnetic materials, sample pH, extraction time, selection of desorption solvent and etc, were optimized. Under optimal conditions, Atrazine and Prometryn exhibited good linearity, with correlation coefficients of 0.999 5 and 0.999 6, linear range of 0.5~120 μg/L and 1~120 μg/L, and limit of detection of 0.055 and 0.04 μg/L, respectively. The spiked recovery for samples was in the range of 95.23%~102.56%. The experimental results indicate that the proposed method was successfully applied to the analysis of triazine herbicides in environmental water.

Key words: magnetic solid phase extraction, atrazine, prometryn, high-performance liquid chromatography, environmental water

中图分类号: 

  • O656.3
[1] BOYD R A. Herbicides and herbicide degradates in shallow groundwater and the Cedar River near a municipal well field, Cedar Rapids, Iowa[J]. Sci Total Environ, 2000, 248: 241-253.
[2] DONNA A, CROSIGNANI P, ROBUTTI F, et al. Triazine herbicides and ovarian epithelial neoplasms. Scand[J]. J Work Environ Health, 1989, 15(1): 47-53.
[3] 李竺,陈玲,郜洪文,等. 固相萃取-高效液相色谱测定环境水样中的三嗪类化合物[J]. 色谱,2006, 24(3): 267-270.
[4] 张贵江,臧晓欢,周欣,等. 磁性石墨烯纳米粒子固相萃取与气相色谱-质谱相结合测定环境水样中的三嗪类除草剂[J]. 色谱, 2013, 31(11): 1071-1075.
[5] ZHOU Qing-xiang, GAO Yuan-yuan. Combination of ionic liquid dispersive liquid-phase microextraction and high performance liquid chromatography for the determination of triazine herbicides in water samples[J]. Chinese Chemical Letters, 2014, 25: 745-748.
[6] 左海英,张琳,刘菲. 固相萃取—液相色谱/质谱法测定地下水中三嗪类和酰胺类除草剂残留[J]. 岩矿测试, 2014, 33 (1): 96-101.
[7] 郭利辉, 田一方, 梅晓芸, 等. 苯唑西林分子印迹聚合物的制备及其分子识别特性研究[J]. 广西师范大学学报:自然科学版, 2015, 33 (1): 86-92.
[8] ŠAFARÍKOVÁM, ŠAFARÍK I. Magnetic solid-phase extraction[J]. J Magn Magn Mater, 1999, 194: 108-112.
[9] 胡晓芳,郭卫民,鲁佳铭,等. 环境水体中三嗪类除草剂的SPME-GCMS联用仪测定[J]. 环境科学与技术, 2011, 34 (12): 160-163.
[10] ZHAO Guang-ying, SONG Shuang-ju, WANG Chun, et al. Determination of triazine herbicides in environmental water samples by high-performance liquid chromatography using graphene-coated magnetic nanoparticles as adsorbent[J]. Analytica Chimica Acta, 2011, 708: 155-159.
[11] GAO Nan-nan, WU Hao, CHANG Ya-fen, et al. Mixed micelle cloud point-magnetic dispersive μ-solid phase extraction of doxazosin and alfuzosin[J]. Spectrochim Acta A, 2015, 134: 10-16.
[12] WU Hao, TIAN Hong, CHEN Ming-fei, et al. Anionic surfactantmicelle-mediated extraction coupled with dispersive magnetic microextraction for the determination of phthalate esters[J]. Journal of Agricultural and Food Chemistry, 2014, 62: 7682-7689.
[13] 黄倩,何蔓, 陈贝贝,等. 磁固相萃取-气相色谱-火焰光度检测联用测定果汁中的有机磷农药[J]. 色谱,2014, 32(10): 1131-1137.
[14] 白沙沙, 李芝, 臧晓欢, 等. 磁性石墨烯固相萃取-分散液液微萃取-气相色谱法测定水和绿茶中酰胺类除草剂残留[J]. 分析化学, 2013, 41(8): 1177-1182.
[15] HE Ze-ying, WANG Peng, LIU Dong-hui, et al. Hydrophilic-lipophilic balanced magnetic nanoparticles: preparation and application in magnetic solid-phase extraction of organochlorine pesticides and triazine herbicides in environmental water samples[J]. Talanta, 2014, 127: 1-8.
[16] YUAN Peng, YANG Dan, LIN Zhong-yu, et al. Influences of pretreatment temperature on the surface silylation of Diatomaceous amorphous silica with trimethylchlorosilane[J]. J Non Cryst Solids, 2006, 352: 3762-3771.
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