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在紫外可见分光光度法测定钴之前,利用新型周边四取代镍(II)酞菁作为传感器的分散液液微萃取方法。

Dispersive Liquid-Liquid Microextraction Method Utilizing a Novel Peripherally Tetra-Substituted Ni(II) Phthalocyanine as a Sensor Prior to UV-Visible Spectrophotometry for the Determination of Co.

作者信息

Çağlar Yasemin, Saka Ece Tuğba

机构信息

Department of Genetic and Bioengineering, Giresun University, Giresun 28200, Türkiye.

Department of Chemistry, Karadeniz Technical University, Trabzon 61080, Türkiye.

出版信息

Molecules. 2025 Jun 11;30(12):2548. doi: 10.3390/molecules30122548.

Abstract

Dispersive liquid-liquid microextraction (DLLME) is an economical, rapid, sensitive, and environmentally friendly miniaturized liquid-liquid extraction format. It has been successfully applied in trace element analysis since 2006 when it was first proposed. This article describes a new dispersive liquid-liquid microextraction method for the determination of trace amounts of Co. In brief, this method involves the extraction of Co from the sample to the trichloromethane phase by the dispersive action of methanol after the formation of a complex with a novel 9-(methylaminomethyl)anthracene-Ni(II) phthalocyanine (MAMA Ni(II)Pc ) as a sensor. The first step in this study was the synthesis and characterisation of the sensor. Later, the proposed method was optimized with respect to various parameters such as extraction and dispersive solvents and their amounts, pH, sensor concentration, and centrifugation time and rate. The calibration graph was linear between 0.40 and 260 µg/L, with an R of 0.9978. The limit of detection and limit of quantification were found to be 0.19 µg/L and 0.46 µg/L, respectively. To evaluate the precision of this method, the analysis of a 50 µg/L Co solution was carried out. The intra-day and inter-day relative standard deviation values were calculated as 1.7% and 2.4%, respectively (n = 7). The accuracy of the proposed method was investigated by means of a standard addition/recovery test.

摘要

分散液液微萃取(DLLME)是一种经济、快速、灵敏且环保的微型液液萃取方法。自2006年首次提出以来,它已成功应用于微量元素分析。本文描述了一种用于测定痕量钴的新型分散液液微萃取方法。简而言之,该方法涉及在与新型9-(甲氨基甲基)蒽-Ni(II)酞菁(MAMA Ni(II)Pc)作为传感器形成络合物后,通过甲醇的分散作用将样品中的钴萃取到三氯甲烷相中。本研究的第一步是传感器的合成与表征。随后,针对萃取溶剂、分散溶剂及其用量、pH值、传感器浓度、离心时间和速率等各种参数对所提出的方法进行了优化。校准曲线在0.40至260 µg/L之间呈线性,R为0.9978。检测限和定量限分别为0.19 µg/L和0.46 µg/L。为评估该方法的精密度,对50 µg/L的钴溶液进行了分析。日内和日间相对标准偏差值分别计算为1.7%和2.4%(n = 7)。通过标准加入/回收率试验研究了所提出方法的准确性。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/3d0d/12195804/915e5b7d2350/molecules-30-02548-g001.jpg

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