College of Chemistry, Jilin University, Qianjin Street 2699, Changchun, 130012, China.
School of Chemistry and Chemical Engineering, Shandong Provincial Key Laboratory of Chemical Energy Storage and Novel Cell Technology, Liaocheng University, Liaocheng, 252059, China.
Talanta. 2020 May 1;211:120676. doi: 10.1016/j.talanta.2019.120676. Epub 2019 Dec 28.
In the presented work, we proposed the use of polyvinylidene difluoride (PVDF) as a coupling agent to load MIL-101(Cr) and carboxylated multi-walled carbon nanotubes (MWCNTs) on the skeleton of melamine sponge (MeS) for the preparation of novel extraction media with high-efficiency. The morphology and structure of this composite were characterized by scanning electron microscopy (SEM) analyses. The obtained MIL-101(Cr)/MWCNTs functionalized MeS(MIL/M-MeS) cube was used as a sorbent for the solid-phase extraction (SPE) of six triazines (Atraton, Simetryne, Prometon, Ametryn, Propazine, and Prometryn) spiked corn samples. Several parameters that may affect the extraction efficiencies, including type and volume of extraction solvent, times of ultrasonic extraction, adsorption, and desorption; type and volume of desorption solvent, were optimized. This was followed by elution containing the herbicides, which were quantified using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Under optimum conditions, the analytical method for the preparation of MIL/M-MeS cube produced satisfactory recoveries and repeatability. The LODs of the method when applied to spiked corn samples were in the range of 0.01-0.04 ng g (LODs = 3δ/k). The relative intra- and inter-day recoveries ranged from 90.30 to 116.50% and 92.38-116.24%, respectively, and relative standard deviations ranged from 1.08 to 12.32% and 5.36-16.23%, respectively.
在本工作中，我们提出使用聚偏二氟乙烯（PVDF）作为偶联剂，将 MIL-101(Cr)和羧基化多壁碳纳米管（MWCNTs）负载到三聚氰胺海绵（MeS）骨架上，制备高效新型萃取介质。通过扫描电子显微镜（SEM）分析对这种复合材料的形态和结构进行了表征。所得的 MIL-101(Cr)/MWCNTs 功能化 MeS（MIL/M-MeS）立方体被用作固相萃取（SPE）的吸附剂，用于萃取受污染玉米样品中的六种三嗪类除草剂（阿特拉津、西玛津、扑灭通、莠去津、扑灭津和敌草隆）。优化了可能影响萃取效率的几个参数，包括萃取溶剂的类型和体积、超声萃取的次数、吸附和解吸；解吸溶剂的类型和体积。然后，用高效液相色谱-串联质谱（HPLC-MS/MS）法对含有除草剂的洗脱液进行洗脱并定量。在最佳条件下，用于制备 MIL/M-MeS 立方体的分析方法具有令人满意的回收率和重复性。该方法应用于受污染玉米样品时，方法的检出限（LOD）在 0.01-0.04 ng g（LOD=3δ/k）范围内。日内和日间相对回收率分别在 90.30-116.50%和 92.38-116.24%之间，相对标准偏差分别在 1.08-12.32%和 5.36-16.23%之间。
