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使用石墨烯萃取后,通过超高效液相色谱-串联质谱法测定环境水和土壤中的五种磺酰脲类除草剂

Determination of five sulfonylurea herbicides in environmental waters and soil by ultra high performance liquid chromatography with tandem mass spectrometry after extraction using graphene.

作者信息

Li Cheng, Lu Anxiang, Wang Jihua, Li Jie, Ping Hua, Luan Yunxia, Chen Jiayi, Ha Xuejiao

机构信息

Beijing Research Center for Agricultural Standards and Testing, Beijing, China.

出版信息

J Sep Sci. 2014 Dec;37(24):3714-21. doi: 10.1002/jssc.201400797. Epub 2014 Nov 12.

Abstract

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%.

摘要

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%。

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