Li Cheng, Lu Anxiang, Wang Jihua, Li Jie, Ping Hua, Luan Yunxia, Chen Jiayi, Ha Xuejiao
Beijing Research Center for Agricultural Standards and Testing, Beijing, China.
J Sep Sci. 2014 Dec;37(24):3714-21. doi: 10.1002/jssc.201400797. Epub 2014 Nov 12.
A fast and novel analytical method was developed for the determination of trace levels of sulfonylurea herbicides in water and soil samples. Graphene was used as a sorbent for extraction, and ultra high performance liquid chromatography with tandem mass spectrometry was used for quantification. Five sulfonylurea herbicides were preconcentrated from water samples using a graphene-loaded packed cartridge, while extraction from soil samples was performed in a single step using graphene-supported matrix solid-phase dispersion. Under the optimized conditions, the calibration plots were linear in the range between 5 and 1000 ng/L for water samples, and between 1 and 200 ng/g for soil samples. All correlation coefficients (R) were >0.99. The limits of detection for water and soil samples were 0.28-0.53 ng/L and 0.08-0.26 ng/g, respectively. This method was successfully applied to the analysis of spiked samples of environmental water and soil, with recoveries ranging from 84.2-109.3 and 86.12-103.2%, respectively, all with relative standard deviations of <10%.
开发了一种快速、新颖的分析方法,用于测定水和土壤样品中痕量磺酰脲类除草剂。采用石墨烯作为萃取吸附剂,超高效液相色谱-串联质谱法进行定量分析。使用装填有石墨烯的固相萃取柱对水样中的5种磺酰脲类除草剂进行预富集,而对于土壤样品,则采用石墨烯负载的基质固相分散法一步完成萃取。在优化条件下,水样的校准曲线在5至1000 ng/L范围内呈线性,土壤样品在1至200 ng/g范围内呈线性。所有相关系数(R)均>0.99。水和土壤样品的检测限分别为0.28 - 0.53 ng/L和0.08 - 0.26 ng/g。该方法成功应用于环境水样和土壤加标样品的分析,回收率分别为84.2 - 109.3%和86.12 - 103.2%,相对标准偏差均<10%。