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Development of a dispersive liquid-liquid microextraction coupled with magnetic dispersive microsolid phase extraction for determination of triazines in wastewater samples.
Analytical and Bioanalytical Chemistry ( IF 4.3 ) Pub Date : 2020-01-10 , DOI: 10.1007/s00216-019-02354-4
Karina Aguilar-Arteaga 1 , Cynthia Hernández-Mera 1 , Luis Díaz-Batalla 1 , Araceli Castañeda-Ovando 2 , Alida Elizabeth Cruz-Pérez 3 , Enrique Barrado-Esteban 4 , Manuel Carrillo-Cárdenas 5
Affiliation  

The combination of two microextraction techniques (dispersive liquid-liquid microextraction [DLLME] and magnetic dispersive microsolid phase extraction [MDMSPE]) was developed and reported for atrazine and simazine preconcentration from wastewater samples. The proposal methodology involved the use of magnetite supports functionalized with different alkyl or phenyl groups. The magnetic adsorbents were synthesized by the solvothermal method assisted by microwave, characterized, and used in the sample preconcentration of atrazine and simazine. The method validation included parameters such as the wastewater matrix effect, repeatability, and recovery. The analyte separation and quantification were performed by high-performance liquid chromatography with ultraviolet detection (HPLC-DAD). Parameters, such as the polarity and mass of magnetic solids and pH, were evaluated to provide better extraction performance. The highest recoveries (> 95%) were obtained with 50 mg of the phenyl group support (CS2) at pH 5, using 5 mL of the sample and carbon tetrachloride and methanol, as extraction and dispersive solvents, respectively. The lowest limits of detection (LOD) achieved were 13.16 and 13.86 ng L-1, and the limits of quantification (LOQ) were 43.89 and 46.19 ng L-1 for simazine and atrazine, respectively, with repeatability (expressed as %RSD) below 5% in all cases. The developed method is simple, easy, and low cost for the analysis of two herbicides potentially dangerous for environmental and human health. Graphical abstract.

中文翻译:

分散液-液微萃取与磁性分散微固相萃取相结合用于测定废水样品中的三嗪的开发。

开发了两种微萃取技术(分散液-液微萃取[DLLME]和磁分散微固相萃取[MDMSPE])的组合,并报道了废水样品中阿特拉津和辛嗪的预浓缩。提议的方法论涉及使用磁铁矿载体,其被不同的烷基或苯基官能化。通过微波辅助溶剂热法合成了磁性吸附剂,并对其进行了表征,并将其用于样品中阿特拉津和西玛津的富集。方法验证包括废水基质效应,可重复性和回收率等参数。通过高效液相色谱和紫外检测(HPLC-DAD)进行分析物的分离和定量。参数,对诸如磁性固体的极性和质量以及pH进行了评估,以提供更好的提取性能。使用5 mg样品,四氯化碳和甲醇分别作为萃取溶剂和分散溶剂,在pH 5下使用50 mg苯基载体(CS2)可获得最高的回收率(> 95%)。最低的检测限(LOD)为13.16和13.86 ng L-1,定量限(LOQ)分别为simazine和atrazine分别为43.89和46.19 ng L-1,重复性(表示为%RSD)低于在所有情况下均为5%。所开发的方法简单,容易且成本低,可用于分析两种可能对环境和人体健康构成危险的除草剂。图形概要。分别使用5 mL样品和四氯化碳和甲醇分别作为萃取溶剂和分散溶剂,在pH 5下使用50 mg苯基载体(CS2)得到95%的苯基。最低的检测限(LOD)为13.16和13.86 ng L-1,定量限(LOQ)分别为simazine和atrazine分别为43.89和46.19 ng L-1,重复性(表示为%RSD)低于在所有情况下均为5%。所开发的方法简单,容易且成本低,可用于分析两种可能对环境和人体健康构成危险的除草剂。图形概要。分别使用5 mL样品和四氯化碳和甲醇分别作为萃取溶剂和分散溶剂,在50 pH值为5的苯基载体(CS2)中获得95%的苯甲酸。最低的检测限(LOD)为13.16和13.86 ng L-1,定量限(LOQ)分别为simazine和atrazine分别为43.89和46.19 ng L-1,重复性(表示为%RSD)低于在所有情况下均为5%。所开发的方法简单,容易且成本低,可用于分析两种可能对环境和人体健康构成危险的除草剂。图形概要。辛嗪和阿特拉津的定量限(LOQ)分别为43.89和46.19 ng L-1,所有情况下的重复性(表示为%RSD)均低于5%。所开发的方法简单,容易且成本低,可用于分析两种可能对环境和人体健康构成危险的除草剂。图形概要。辛嗪和阿特拉津的定量限(LOQ)分别为43.89和46.19 ng L-1,所有情况下的重复性(表示为%RSD)均低于5%。所开发的方法简单,容易且成本低,可用于分析两种可能对环境和人体健康构成危险的除草剂。图形概要。
更新日期:2020-01-11
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