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采用金属有机框架材料MIL-101(Cr)进行固相萃取并结合实时直接分析质谱法对三嗪类除草剂进行快速分析。

Solid-phase extraction with the metal-organic framework MIL-101(Cr) combined with direct analysis in real time mass spectrometry for the fast analysis of triazine herbicides.

作者信息

Li Xianjiang, Xing Jiawei, Chang Cuilan, Wang Xin, Bai Yu, Yan Xiuping, Liu Huwei

机构信息

Beijing National Laboratory for Molecular Sciences, the Key Laboratory of Bioorganic Chemistry and Molecular Engineering of Ministry of Education, Institute of Analytical Chemistry, College of Chemistry and Molecular Engineering, Peking University, Beijing, China.

出版信息

J Sep Sci. 2014 Jun;37(12):1489-95. doi: 10.1002/jssc.201400151. Epub 2014 Apr 27.

Abstract

MIL-101(Cr) is an excellent metal-organic framework with high surface area and nanoscale cavities, making it promising in solid-phase extraction. Herein, we used MIL-101(Cr) as a solid-phase extraction packing material combined with fast detection of direct analysis in real time mass spectrometry (DART-MS) for the analysis of triazine herbicides. After systematic optimization of the operation parameters, including the gas temperature of DART, the moving speed of the 1D platform, solvent for desorption, amount of MIL-101(Cr) extraction time, eluent volume and salt concentration, this method can realize the simultaneous detection of five kinds of triazine herbicides. The limits of detection were 0.1∼0.2 ng/mL and the linear ranges covered more than two orders of magnitude with the quantitation limits of 0.5∼1 ng/mL. Moreover, the developed method has been applied for the analysis of lake water samples and the recoveries for spiked analytes were in the range of 85∼110%. These results showed that solid-phase extraction with metal-organic frameworks is an efficient sample preparation approach for DART-MS analysis and could find more applications in environmental analysis.

摘要

MIL-101(Cr)是一种具有高比表面积和纳米级孔洞的优秀金属有机框架材料,使其在固相萃取方面具有应用前景。在此,我们将MIL-101(Cr)用作固相萃取填充材料,并结合实时直接分析质谱法(DART-MS)快速检测技术来分析三嗪类除草剂。在对包括DART气体温度、一维平台移动速度、解吸溶剂、MIL-101(Cr)用量、萃取时间、洗脱液体积和盐浓度等操作参数进行系统优化后,该方法可实现五种三嗪类除草剂的同时检测。检测限为0.1∼0.2 ng/mL,线性范围覆盖两个以上数量级,定量限为0.5∼1 ng/mL。此外,所开发的方法已应用于湖水样品分析,加标分析物的回收率在85∼110%范围内。这些结果表明,金属有机框架材料的固相萃取是一种用于DART-MS分析的高效样品制备方法,并且在环境分析中可能会有更多应用。

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