College of Chinese Materia Medica, Tianjin University of Traditional Chinese Medicine, Tianjin, P. R. China.
College of Food Science and Technology, Henan Agricultural University, Zhengzhou, P. R. China.
J Sep Sci. 2020 Nov;43(21):4058-4066. doi: 10.1002/jssc.202000567. Epub 2020 Sep 24.
A new extraction method, microwave absorption medium-assisted extraction coupled with reversed-phase dispersive liquid-liquid microextraction, was developed for the determination of triazine herbicides in corn and soybean samples. Triazine herbicides were extracted with hexane and then directly enriched into the ionic liquid phase. The purification of sample and concentration of target analytes were performed simultaneously. The method combines the advantages of nonpolar solvent dynamic microwave extraction and reversed-phase dispersive liquid-liquid microextraction, which could greatly simplify the operation and reduce the whole pretreatment time. The Box-Behnken design was used to the optimization of experimental factors involved in the dynamic microwave-assisted extraction. In the present study, good linearity in the range of 5.00-500.00 µg/kg was obtained. The limits of detection and quantification varying from 1.3 to 4.2 and 4.1 to 13.9 µg/kg were achieved, respectively. The intra- and interday precisions were between 2.7 and 6.9%. The present method was applied to the analysis of corn and soybean samples, and the recoveries of analytes ranged from 80.7 to 106.9% with the relative standard deviations of 2.1-7.8%. The present method shows the potentials of practical applications in the treatment of the complex fatty solid samples.
一种新的萃取方法,即微波吸收介质辅助萃取结合反相分散液液微萃取,被开发用于玉米和大豆样品中三嗪类除草剂的测定。三嗪类除草剂用正己烷萃取,然后直接富集到离子液相中。同时完成样品的净化和目标分析物的浓缩。该方法结合了非极性溶剂动态微波萃取和反相分散液液微萃取的优点,可大大简化操作并减少整个预处理时间。采用 Box-Behnken 设计对动态微波辅助萃取中涉及的实验因素进行优化。在本研究中,在 5.00-500.00 µg/kg 的范围内获得了良好的线性。检测限和定量限分别为 1.3-4.2 和 4.1-13.9 µg/kg。日内和日间精密度在 2.7-6.9%之间。该方法应用于玉米和大豆样品的分析,分析物的回收率在 80.7-106.9%之间,相对标准偏差为 2.1-7.8%。该方法在处理复杂的含脂固体样品方面具有实际应用的潜力。