Marzi Khosrowshahi Elnaz, Farajzadeh Mir Ali, Tuzen Mustafa, Afshar Mogaddam Mohammad Reza, Nemati Mahboob
Food and Drug Safety Research Center, Tabriz University of Medical Sciences, Tabriz, Iran.
Anal Methods. 2021 Aug 28;13(32):3592-3604. doi: 10.1039/d1ay00861g. Epub 2021 Jul 26.
A dispersive solid-phase microextraction method based on magnetic carbon nano-onions (MCNOs) was developed for the extraction and preconcentration of some pesticides from water and vegetable samples. For more cleanup and preconcentration, a dispersive liquid-liquid microextraction (DLLME) method was employed after performing the first step. In this method, firstly, MCNOs were prepared and then used for adsorption of the analytes from the sample solution. After that, the adsorbed analytes were eluted with an appropriate water-miscible organic solvent and used as a dispersive solvent in the following DLLME procedure. The extracted analytes were quantified by gas chromatography-mass spectrometry (GC-MS) in selected ion monitoring (SIM) mode. Various factors affecting the method efficiency such as sorbent weight, salt effect, pH, temperature, and type and volume of eluent and extraction solvent were optimized. This method showed wide linear ranges with a coefficient of determination ≥ 0.994, and low limits of detection (0.001-0.005 ng mL) and quantification (0.003-0.019 ng mL) under optimal conditions. Also, a good precision (relative standard deviation ≤ 8.6%) for five replicates and a satisfactory accuracy (mean relative recoveries between 82 and 99%) were obtained. It can be considered as an efficient and environment friendly method for the extraction of analytes from vegetable and fruit juices and water samples.
开发了一种基于磁性碳纳米洋葱（MCNOs）的分散固相微萃取方法，用于从水和蔬菜样品中萃取和预富集某些农药。为了实现更多的净化和预富集，在第一步之后采用了分散液液微萃取（DLLME）方法。在该方法中，首先制备MCNOs，然后用于从样品溶液中吸附分析物。之后，用适当的与水混溶的有机溶剂洗脱吸附的分析物，并将其用作后续DLLME程序中的分散溶剂。通过气相色谱 - 质谱联用仪（GC-MS）在选择离子监测（SIM）模式下对萃取的分析物进行定量。对影响方法效率的各种因素，如吸附剂重量、盐效应、pH值、温度以及洗脱剂和萃取溶剂的类型和体积进行了优化。该方法在最佳条件下显示出宽线性范围，测定系数≥0.994，检测限低（0.001 - 0.005 ng/mL）和定量限低（0.003 - 0.019 ng/mL）。此外，五次重复测定具有良好的精密度（相对标准偏差≤8.6%）和令人满意的准确度（平均相对回收率在82%至99%之间）。它可被认为是一种从蔬菜汁、果汁和水样中萃取分析物的高效且环境友好的方法。
