Key Laboratory of Analytical Chemistry for Biology and Medicine (Ministry of Education), Department of Chemistry, Wuhan University , Wuhan 430072, People's Republic of China.
J Agric Food Chem. 2013 Jun 5;61(22):5397-403. doi: 10.1021/jf400870m. Epub 2013 May 28.
This article presents a novel application of dispersive microextraction based on "magnetic water" (m-water) for the purification of organophosphorus pesticides (methamidophos, omethoate, monocrotophos) from cold-pressed vegetable oils. In the present study, a trace amount of water (extractant) was adsorbed on bare Fe₃O₄ by hydrophilic interaction to form m-water. Rapid extraction can be achieved while the m-water is dispersed in the sample solution with the aid of a vigorous vortex. After extraction, the analyte-adsorbed m-water can be readily isolated from the sample solution by a magnet, which could greatly simplify the operation and reduce the whole pretreatment time. Several parameters affecting the extraction efficiency were investigated, and under the optimized conditions, a simple and effective method for pesticide analysis was established by coupling with gas chromatography/mass spectrometry (GC/MS). The linearity range of the proposed method was 2-100 ng/g with satisfactory correlation coefficients (R) of 0.9997-0.9998, and the limits of quantification (LOQ) for the target compounds were in the range of 0.70-1.27 ng/g. In addition, the reproducibility was obtained by evaluating the intra- and interday precisions with relative standard deviations (RSDs) less than 7.2% and 6.5%, respectively. Finally, the established "magnetic water" microextraction method was successfully applied for the determination of pesticide residues in several kinds of cold-pressed vegetable oils.
本文提出了一种基于“磁水”(m-water)的分散微萃取方法,用于从冷榨植物油中净化有机磷农药(甲胺磷、氧乐果、久效磷)。在本研究中,通过亲水相互作用将痕量的水(萃取剂)吸附在裸露的 Fe₃O₄ 上,形成 m-water。在剧烈涡旋的作用下,m-water 可以分散在样品溶液中,从而实现快速萃取。萃取后,用磁铁很容易将吸附有分析物的 m-water 从样品溶液中分离出来,这可以大大简化操作并减少整个预处理时间。考察了影响萃取效率的几个参数,并在优化条件下,通过与气相色谱/质谱(GC/MS)联用,建立了一种简单有效的农药分析方法。该方法的线性范围为 2-100ng/g,相关系数(R)为 0.9997-0.9998,目标化合物的定量限(LOQ)在 0.70-1.27ng/g 范围内。此外,通过评估日内和日间精密度,得到的重复性相对标准偏差(RSD)分别小于 7.2%和 6.5%。最后,将建立的“磁水”微萃取方法成功应用于几种冷榨植物油中农药残留的测定。