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多壁碳纳米管作为固相萃取吸附剂用于气相色谱-质谱法测定水和土壤样品中的阿特拉津及其主要代谢物

Multi-walled carbon nanotubes as solid-phase extraction adsorbents for determination of atrazine and its principal metabolites in water and soil samples by gas chromatography-mass spectrometry.

作者信息

Min Guang, Wang Shuo, Zhu Huaping, Fang Guozhen, Zhang Yan

机构信息

Key Laboratory of Food Nutrition and Safety, Ministry of Education of China, Tianjin, China.

出版信息

Sci Total Environ. 2008 Jun 15;396(1):79-85. doi: 10.1016/j.scitotenv.2008.02.016. Epub 2008 Mar 26.

Abstract

A novel, simple, cost-effective, and sensitive method was developed for the determination of atrazine and its principal metabolites namely deisopropyl-atrazine (DIA) and deethyl-atrazine (DEA) in water and soil samples using multi-walled carbon nanotubes as solid-phase extraction (SPE) adsorbents coupled with gas chromatography-mass spectrometry (GC-MS). Several condition parameters, such as sample loading flow-rate, eluent and elution volume, extractant and ratio of extraction solvent to sample, were optimized to achieve good sensitivity and precision for the extraction and elution of analytes. A methanol/water solution (50%, v/v) was used to extract atrazine, DIA and DEA from soil. After the extracts went through SPE cartridges (packed with multi-walled carbon nanotubes) at a flow-rate of 4 mL min(-1), the analytes were eluted by 4 mL ethyl acetate at the rate of 1 mL min(-1) under a vacuum pump. The limit of detection (S/N=3) of the proposed method was 0.02 microg kg(-1) for atrazine in water and 0.3 microg kg(-1) in soil; 0.04 microg kg(-1) for DIA in water and 1.0 microg kg(-1) in soil; 0.05 microg kg(-1) for DEA in water and 0.8 microg kg(-1) in soil. Mean recoveries were in the range of 72.27-109.68%, and the reproducibility was accepted (RSD <13%) under the optimum conditions. This developed method was applied to determine the analytes in real environmental samples, and the concentrations of atrazine were 0.77-10.83 microg kg(-1), while DEA and DIA were not detected.

摘要

开发了一种新颖、简单、经济高效且灵敏的方法,用于测定水和土壤样品中的阿特拉津及其主要代谢物,即去异丙基阿特拉津(DIA)和去乙基阿特拉津(DEA)。该方法使用多壁碳纳米管作为固相萃取(SPE)吸附剂,并结合气相色谱 - 质谱联用(GC-MS)。对几个条件参数进行了优化,如样品加载流速、洗脱剂和洗脱体积、萃取剂以及萃取溶剂与样品的比例,以实现对分析物萃取和洗脱的良好灵敏度和精密度。采用甲醇/水溶液(50%,v/v)从土壤中萃取阿特拉津、DIA和DEA。提取物以4 mL min⁻¹的流速通过装有多壁碳纳米管的SPE小柱后,在真空泵作用下,用4 mL乙酸乙酯以1 mL min⁻¹的流速洗脱分析物。该方法的检测限(S/N = 3)为:水中阿特拉津0.02 μg kg⁻¹,土壤中0.3 μg kg⁻¹;水中DIA 0.04 μg kg⁻¹,土壤中为1.0 μg kg⁻¹;水中DEA 0.05 μg kg⁻¹,土壤中0.8 μg kg⁻¹。在最佳条件下,平均回收率在72.27% - 109.68%范围内,重现性良好(RSD < 13%)得到认可。该方法应用于实际环境样品中分析物的测定,阿特拉津的浓度为每千克0.77 - 10.83微克,而未检测到DEA和DIA。

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