Min Guang, Wang Shuo, Zhu Huaping, Fang Guozhen, Zhang Yan
Key Laboratory of Food Nutrition and Safety, Ministry of Education of China, Tianjin, China.
Sci Total Environ. 2008 Jun 15;396(1):79-85. doi: 10.1016/j.scitotenv.2008.02.016. Epub 2008 Mar 26.
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.
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。