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基于深共晶溶剂和氮化碳的微型化基质固相分散与高效液相色谱联用:一种新的萃取和测定土壤样品中痕量硝基甲苯污染物的可行性。

Miniaturized matrix solid-phase dispersion based on deep eutectic solvent and carbon nitride associated with high-performance liquid chromatography: A new feasibility for extraction and determination of trace nitrotoluene pollutants in soil samples.

机构信息

Faculty of Chemical Engineering, School of Engineering, University of Tehran, Tehran, Iran.

Department of Chemistry, Faculty of Chemistry and Chemical Engineering, Malek Ashtar University of Technology, Tehran, Iran.

出版信息

J Chromatogr A. 2019 Sep 13;1601:35-44. doi: 10.1016/j.chroma.2019.05.008. Epub 2019 May 10.

Abstract

In this research, a miniaturized version of matrix solid phase dispersion (MSPD) method was developed for successful extraction of five nitrotoluenes from soil samples. The terpene based deep eutectic solvent (DES) composed of borneol and DL-menthol was used simultaneously as extraction solvent and dispersing liquid. Graphitic-carbon nitride (g-CN) as sorbent was prepared by pyrolysis of melamine at a muffle furnace. The MSPD mixture was obtained by grinding soil, DES, and g-CN. Minimum amount of acetonitrile was used in the elution step. Some experimental variables including type and volume of DES, type of dispersant, mass ratio of dispersant to sample, volume of elution solvent, grinding time, and ultrasonication time were evaluated. Analysis of extracted samples was performed by high performance liquid chromatography-ultra violet detection. Under the optimized conditions; the limits of detection were achieved in the range of 0.12-0.33 μg g, and the relative standard deviations were equal to or lower than 9.3%. The extraction recoveries were ranged from 78 to 96%. This straightforward and fast method is effective for environmentally friendly extraction of nitrotoluenes from soil samples.

摘要

本研究开发了一种微型化的基质固相分散(MSPD)方法,成功地从土壤样品中提取了五种硝基甲苯。萜烯基深共晶溶剂(DES)由龙脑和 DL-薄荷醇组成,同时用作提取溶剂和分散液。石墨相氮化碳(g-CN)通过在马弗炉中热解三聚氰胺制备。MSPD 混合物通过研磨土壤、DES 和 g-CN 获得。在洗脱步骤中仅使用最小量的乙腈。评估了一些实验变量,包括 DES 的类型和体积、分散剂的类型、分散剂与样品的质量比、洗脱溶剂的体积、研磨时间和超声时间。通过高效液相色谱-紫外检测对提取的样品进行分析。在优化的条件下;检测限在 0.12-0.33μg g 范围内,相对标准偏差等于或低于 9.3%。萃取回收率在 78%至 96%之间。这种简单快速的方法可有效地从土壤样品中环保地提取硝基甲苯。

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