Baotou Medical College, Baotou, Inner Mongolia 014060, China.
Anal Methods. 2020 Jun 4;12(21):2747-2756. doi: 10.1039/d0ay00288g.
A rapid and simple analytical method based on magnetic solid-phase extraction with magnetic amino modified multiwalled carbon nanotubes with ultra-high performance liquid chromatography-tandem mass spectrometry is reported for the determination of seven pesticides (futriafol, metalaxyl, myclobutanil, napropamide, epoxiconazole, fipronil and diniconazole) in water samples. In this study, magnetic amino modified multi-walled carbon nanotubes were synthesized and selected as a new kind of material to adsorb pesticides in the water samples. Various magnetic solid-phase extraction parameters, such as the amount and type of adsorbent, extraction methods, extraction time, the type and volume of desorption solvent, desorption time and solution ionic strength, were systematically optimized. Under optimum conditions, the method validation results showed good linearity and recoveries. The calibration curves were in the range of 1.0-100 ng mL-1 for napropamide, epoxiconazole, metalaxyl, and fipronil, while they were 5.0-500 ng mL-1 for futriafol, myclobutanil, and diniconazole, with determination coefficients (R2) higher than 0.9909. The limits of quantification were 1.0-5.0 ng mL-1 and the limits of detection were 0.3-1.5 ng mL-1. The recoveries of the seven pesticides ranged from 80.4% to 103.2%. This developed method, which is more convenient and effective in comparison with traditional methods, has been successfully applied for the analysis of pesticides in water samples qualitatively and quantitatively.
基于磁性固相萃取与超高效液相色谱-串联质谱联用的快速简便分析方法,用于测定水样中的七种农药(氟噻唑、甲霜灵、戊菌隆、萘普胺、烯唑醇、氟虫腈和烯唑醇)。本研究合成了磁性氨基修饰多壁碳纳米管,并将其作为一种新型材料用于吸附水样中的农药。系统优化了各种磁性固相萃取参数,如吸附剂的用量和类型、萃取方法、萃取时间、解吸溶剂的类型和体积、解吸时间和溶液离子强度等。在最佳条件下,方法验证结果表明具有良好的线性和回收率。萘普胺、烯唑醇、甲霜灵和氟虫腈的校准曲线范围为 1.0-100ng mL-1,而氟噻唑、戊菌隆和烯唑醇的校准曲线范围为 5.0-500ng mL-1,测定系数(R2)均高于 0.9909。七种农药的检出限为 1.0-5.0ng mL-1,定量限为 0.3-1.5ng mL-1。七种农药的回收率在 80.4%-103.2%之间。与传统方法相比,该方法更方便、更有效,已成功用于定性和定量分析水样中的农药。