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磁性固相萃取-超高效液相色谱-串联质谱法快速检测环境水体中痕量全氟化合物

发表时间:2016-09-15  浏览量:1724  下载量:297
全部作者: 周雨笋,陶 芸,周廷廷,沈小丽,梅素容
作者单位: 华中科技大学同济医学院公共卫生学院;青岛大学附属医院检验科
摘 要: 以实验室制备的磁性纳米复合材料(Fe3O4@SiO2-NH2&F13)为吸附剂,建立了简便、快速、高效的磁性固相萃取(magnetic solid-phase extraction,MSPE)技术,用于环境水体中9种全氟化合物(perfluorinated compounds,PFCs)的选择性分离与富集,利用超高效液相色谱-串联质谱法(ultra high-performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)对PFCs进行定量分析。在最优的MSPE条件下,500 mL水样中痕量PFCs经磁性材料富集后,重新溶解于0.5 mL甲醇:水(7:3,体积比)中,实现了1 000倍的富集效率。该方法的线性范围在0.5~100 ng•L-1之间,R2≥0.991 7,检测限(limit of detection,LOD)介于0.029~0.099 ng•L-1;在0.5~50 ng•L-1的加标浓度下,PFCs的加标回收率为90.05%~106.67%,相对标准偏差(relative standard deviation,RSD)≤12.62%(n=3),实现了水样中痕量PFCs的快速、准确、灵敏检测。与其他常规方法相比,该方法分析速度快、线性范围宽、灵敏度高、准确性好,可进一步用于环境水体中痕量PFCs的监测和污染状况分析。
关 键 词: 卫生检验学;全氟化合物;磁性固相萃取;环境水体;快速检测
Title: Rapid determination of trace perfluorinated compounds in environmental water sample by magnetic solid-phase extraction coupled with ultra high-performance liquid chromatography-tandem mass spectrometry
Author: ZHOU Yusun, TAO Yun, ZHOU Tingting, SHEN Xiaoli, MEI Surong
Organization: School of Public Health, Tongji Medical College, Huazhong University of Science and Technology; Department of Clinical Laboratory, The Affiliated Hospital of Qingdao University
Abstract: In this study, using a novel magnetic nanocomposite (Fe3O4@SiO2-NH2&F13) prepared in our laboratory, a convenient, rapid and effective magnetic solid-phase extraction (MSPE) procedure was established for selective separation and concentration of nine perfluorinated compounds (PFCs) in environmental water sample, and then an ultra high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) system was employed for the detection of PFCs. Under the optimized MSPE conditions, an enrichment factor of 1 000 was achieved by extracting trace PFCs from 500 mL of water sample and redissolving the analytes in 0.5 mL of methanol:water (7:3, volume ratio). Good linearity of the developed analytical method was in the range of 0.5-100 ng•L-1 with R2≥0.991 7, and the limits of detection (LOD) ranged from 0.029 to 0.099 ng•L-1. At three different fortified concentrations of 0.5-50 ng•L-1, the spiked recoveries of PFCs in the range of 90.05%-106.67% were obtained with RSD≤12.62% (n=3), indicating good accuracy and precision. Compared with other reported methods, the proposed technique has many advantages ranging from fast analytical efficiency, wide linearity range, high sensitivity to good stability, which made it more practical for trace PFCs monitoring and its occurrence investigation in environmental water sample.
Key words: sanitary inspection; perfluorinated compounds; magnetic solid-phase extraction; environmental water sample; rapid determination
发表期数: 2016年9月第17期
引用格式: 周雨笋,陶 芸,周廷廷,等. 磁性固相萃取-超高效液相色谱-串联质谱法快速检测环境水体中痕量全氟化合物[J]. 中国科技论文在线精品论文,2016,9(17):1827-1833.
 
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