Costa Dos Reis Luciana, Vidal Lorena, Canals Antonio
Departamento de Química Analítica, Nutrición y Bromatología e Instituto Universitario de Materiales, Universidad de Alicante, P.O. Box 99, 03080, Alicante, Spain.
Anal Bioanal Chem. 2017 Apr;409(10):2665-2674. doi: 10.1007/s00216-017-0211-3. Epub 2017 Feb 10.
A fast, simple, economical, and environmentally friendly magnetic solid-phase extraction (MSPE) procedure has been developed to preconcentrate 2,4,6-trinitrotoluene (TNT) from water samples prior to determination by liquid chromatography-UV-Vis employing graphene oxide/FeO nanocomposite as sorbent. The nanocomposite synthesis was investigated, and the MSPE was optimized by a multivariate approach. The optimum MSPE conditions were 40 mg of nanocomposite, 10 min of vortex extraction, 1 mL of acetonitrile as eluent, and 6 min of desorption in an ultrasonic bath. Under the optimized experimental conditions, the method was evaluated to obtain a preconcentration factor of 153. The linearity of the method was studied from 1 to 100 μg L (N = 5), obtaining a correlation coefficient of 0.994. The relative standard deviation and limit of detection were found to be 12% (n = 6, 10 μg L) and 0.3 μg L, respectively. The applicability of the method was investigated, analyzing three types of water samples (i.e., reservoir and drinking water and effluent wastewater) and recovery values ranged between 87 and 120% (50 μg L spiking level), showing that the matrix had a negligible effect upon extraction. Finally, the semiquantitative Eco-Scale metrics confirmed the greenness of the developed method.
已开发出一种快速、简单、经济且环保的磁性固相萃取(MSPE)方法,用于在采用氧化石墨烯/FeO纳米复合材料作为吸附剂通过液相色谱 - 紫外 - 可见分光光度法测定之前,对水样中的2,4,6 - 三硝基甲苯(TNT)进行预富集。研究了纳米复合材料的合成,并通过多变量方法对MSPE进行了优化。最佳MSPE条件为40 mg纳米复合材料、10分钟涡旋萃取、1 mL乙腈作为洗脱剂以及在超声浴中6分钟解吸。在优化的实验条件下,评估该方法获得的预富集因子为153。研究了该方法在1至100 μg L范围内的线性(N = 5),相关系数为0.994。相对标准偏差和检测限分别为12%(n = 6,10 μg L)和0.3 μg L。研究了该方法的适用性,分析了三种类型的水样(即水库水、饮用水和废水),加标水平为50 μg L时回收率在87%至120%之间,表明基质对萃取的影响可忽略不计。最后,半定量的生态尺度指标证实了所开发方法的绿色性。