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亚临界水萃取结合分子印迹技术用于三嗪类除草剂检测中的样品制备

Subcritical water extraction combined with molecular imprinting technology for sample preparation in the detection of triazine herbicides.

作者信息

Zhao Fengnian, Wang Shanshan, She Yongxin, Zhang Chao, Zheng Lufei, Jin Maojun, Shao Hua, Jin Fen, Du Xinwei, Wang Jing

机构信息

Institute of Quality Standards & Testing Technology for Agro-Products, Chinese Academy of Agricultural Sciences, Beijing 100081, PR China; Key Laboratory of Agro-Product Safety and Quality, Ministry of Agriculture, Beijing 100081, PR China.

Institute of Quality Standards & Testing Technology for Agro-Products, Chinese Academy of Agricultural Sciences, Beijing 100081, PR China; Key Laboratory of Agro-Product Safety and Quality, Ministry of Agriculture, Beijing 100081, PR China.

出版信息

J Chromatogr A. 2017 Sep 15;1515:17-22. doi: 10.1016/j.chroma.2017.06.011. Epub 2017 Jul 8.

Abstract

A selective, environmentally friendly, and cost-effective sample extraction method based on a combination of subcritical water extraction (SWE) and molecularly imprinted solid-phase extraction (MISPE) was developed for the determination of eight triazine herbicides in soil samples by liquid chromatography-tandem mass spectrometry (LC-MS/MS). In SWE, the highest extraction yields of triazine herbicides were obtained under 150°C for 15min using 20% ethanol as the organic modifier. Addition of MIP during SWE increased the extraction efficiency, and using MIP as a selective SPE sorbent improved the enrichment capability. Soil samples were treated with the optimized extraction MIP/SWE-MISPE method and analyzed by LC-MS/MS. The novel technique was then applied to soil samples for the determination of triazine herbicides, and better recoveries (78.9%-101%) were obtained compared with using SWE-MISPE (30%-67%). Moreover, this newly developed method displayed good linearity (R>0.99) and precision (2.7-9.8%), and low enough detection limits (0.4-3.3μgkg). This combination of SWE and MIP technology is a simple, effective and promising method to selectively extract class-specific compounds in complex samples.

摘要

建立了一种基于亚临界水萃取(SWE)和分子印迹固相萃取(MISPE)相结合的选择性、环境友好且经济高效的样品萃取方法,用于通过液相色谱-串联质谱(LC-MS/MS)测定土壤样品中的8种三嗪类除草剂。在SWE中,以20%乙醇作为有机改性剂,在150℃下萃取15分钟可获得三嗪类除草剂的最高萃取率。在SWE过程中添加分子印迹聚合物(MIP)可提高萃取效率,且使用MIP作为选择性固相萃取吸附剂可提高富集能力。采用优化后的萃取方法MIP/SWE-MISPE处理土壤样品,并通过LC-MS/MS进行分析。然后将该新技术应用于土壤样品中三嗪类除草剂的测定,与使用SWE-MISPE(30%-67%)相比,回收率更高(78.9%-101%)。此外,这种新开发的方法具有良好的线性(R>0.99)和精密度(2.7%-9.8%),以及足够低的检测限(0.4-3.3μg/kg)。SWE和MIP技术的这种结合是一种简单、有效且有前景的方法,可用于选择性萃取复杂样品中的特定类别化合物。

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