Zhao Fengnian, Wang Shanshan, She Yongxin, Zhang Chao, Zheng Lufei, Jin Maojun, Shao Hua, Jin Fen, Du Xinwei, Wang Jing
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.
J Chromatogr A. 2017 Sep 15;1515:17-22. doi: 10.1016/j.chroma.2017.06.011. Epub 2017 Jul 8.
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.
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。