Li Na, Wang Zhibing, Zhang Liyuan, Nian Li, Lei Lei, Yang Xiao, Zhang Hanqi, Yu Aimin
College of Chemistry, Jilin University, Qianjin Street 2699, Changchun 130012, PR China.
College of Chemistry and Life Science, Changchun University of Technology, Yanan Street 2055, Changchun 130012, PR China.
Talanta. 2014 Oct;128:345-53. doi: 10.1016/j.talanta.2014.04.084. Epub 2014 May 9.
Liquid-phase extraction coupled with metal-organic frameworks-based dispersive solid phase extraction was developed and applied to the extraction of pesticides in high fatty matrices. The herbicides were ultrasonically extracted from peanut using ethyl acetate as extraction solvent. The separation of the analytes from a large amount of co-extractive fat was achieved by dispersive solid-phase extraction using MIL-101(Cr) as sorbent. In this step, the analytes were adsorbed on MIL-101(Cr) and the fat remained in bulk. The herbicides were separated and determined by high-performance liquid chromatography. The experimental parameters, including type and volume of extraction solvent, ultrasonication time, volume of hexane and eluting solvent, amount of MIL-101(Cr) and dispersive solid phase extraction time, were optimized. The limits of detection for herbicides range from 0.98 to 1.9 μg/kg. The recoveries of the herbicides are in the range of 89.5-102.7% and relative standard deviations are equal or lower than 7.0%. The proposed method is simple, effective and suitable for treatment of the samples containing high content of fat.
开发了液相萃取结合基于金属有机框架的分散固相萃取方法,并将其应用于高脂肪基质中农药的萃取。以乙酸乙酯为萃取溶剂,从花生中超声萃取除草剂。以MIL-101(Cr)为吸附剂,通过分散固相萃取实现了分析物与大量共萃取脂肪的分离。在此步骤中,分析物吸附在MIL-101(Cr)上,脂肪则留在主体相中。除草剂经分离后采用高效液相色谱法测定。对萃取溶剂的类型和体积、超声时间、己烷和洗脱溶剂的体积、MIL-101(Cr)的用量以及分散固相萃取时间等实验参数进行了优化。除草剂的检测限为0.98至1.9 μg/kg。除草剂的回收率在89.5%至102.7%之间,相对标准偏差等于或低于7.0%。该方法简单、有效,适用于处理高脂肪含量的样品。