Department of Chemistry, Beijing Key Laboratory of Microanalytical Methods and Instrumentation, Tsinghua University, Beijing, China.
J Sep Sci. 2013 Aug;36(15):2522-9. doi: 10.1002/jssc.201201091.
A quick, easy, cheap, effective, rugged, and safe (QuEChERS) sample pretreatment method coupled with LC-MS was developed for the determination of 11 pesticides in tobacco. Sample pretreatment parameters and instrumental parameters of LC-MS were investigated, and the optimal conditions were selected. Under the optimized conditions, the 11 pesticides were detected simultaneously with a good linear relationship (r(2) = 0.9993-0.9999) and high precisions (less than 5% of the RSD of peak areas). The LODs were in the range of 0.1-5.0 μg/L. Compared with SPE clean-up, QuEChERS greatly simplified the sample pretreatment with simple solvent extraction system. After QuEChERS pretreatment, no serious matrix effects were observed. Used for the analysis of real samples, metalaxyl was found in cigarette and tobacco samples at 63.47 and 132.27 ng/g, respectively. The recoveries for 11 pesticides were in the range of 70.03-118.69%, and RSDs were less than 10%. The proposed method is simple, low cost, and has good reproducibility.
建立了一种快速、简便、廉价、有效、耐用、安全(QuEChERS)的样品前处理方法,并结合 LC-MS 用于测定烟草中的 11 种农药。考察了 LC-MS 的样品前处理参数和仪器参数,选择了最佳条件。在优化条件下,11 种农药得到了很好的线性关系(r²=0.9993-0.9999)和高精密度(峰面积的 RSD 小于 5%),检测限在 0.1-5.0 μg/L 范围内。与 SPE 净化相比,QuEChERS 大大简化了样品预处理,采用简单的溶剂萃取体系。QuEChERS 预处理后,未观察到严重的基质效应。用于分析实际样品,在香烟和烟草样品中分别发现了金属酰胺,含量为 63.47 和 132.27 ng/g。11 种农药的回收率在 70.03-118.69%之间,RSD 小于 10%。该方法简单、成本低、重现性好。