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通过液相微萃取对水样和土壤提取物中的极性酚类化合物进行预浓缩,并采用液相色谱-紫外检测法进行测定。

Preconcentration of polar phenolic compounds from water samples and soil extract by liquid-phase microextraction and determination via liquid chromatography with ultraviolet detection.

作者信息

Dolatto Rafael Garrett, Messerschmidt Iara, Pereira Betânia Fraga, Martinazzo Rosane, Abate Gilberto

机构信息

Departamento de Química, Universidade Federal do Paraná, CP 19032, CEP 81531-990, Curitiba, PR, Brazil.

FAPEG/Embrapa Clima Temperado, BR 392, Km 78, CEP 96010-971, Pelotas, RS, Brazil.

出版信息

Talanta. 2016;148:292-300. doi: 10.1016/j.talanta.2015.11.004. Epub 2015 Nov 3.

Abstract

This work proposes a liquid-phase microextraction (LPME) method to extract the highly polar compounds phenol (Ph), o-cresol (o-Cr), m-cresol (m-Cr), p-cresol (p-Cr), and 2,4-dimethylphenol (2,4-DMP) from aqueous matrices. The first extraction step of the LPME method employed a common volumetric flask and n-octanol, and the second extraction step used NaOH as the acceptor phase. The optimized extraction conditions were 900 μL of n-octanol as the extraction solvent, NaOH at 0.60 mol L(-1) as the acceptor phase, an extraction time of 5.0 min, HCl at 0.01 mol L(-1) and NaCl at 20.0% as the donor phase, and an extraction temperature of 20.0°C. The analysis of 50.0 mL of aqueous sample, pretreated under the optimized LPME conditions, afforded a limit of detection (LOD) between 0.3 and 3.5 μg L(-1), a limit of quantification (LOQ) between 1.2 and 11.6 μg L(-1), and a linear range from 2.50 to 50.0 μg L(-1) for Ph, o-Cr, m-Cr and p-Cr and from 12.5 to 250 μg L(-1) for 2,4-DMP. The proposed LPME method was a successful sample preparation strategy, and allowed for precise and accurate quantification of polar phenolic compounds in aqueous matrices such as tap water, river water, groundwater, and seawater, and also in a soil extract. The recovery values ranged from 72.5% to 126.0%, and the relative standard deviation was between 0.3 and 11.5%.

摘要

本研究提出了一种液相微萃取(LPME)方法,用于从水性基质中萃取高极性化合物苯酚(Ph)、邻甲酚(o-Cr)、间甲酚(m-Cr)、对甲酚(p-Cr)和2,4-二甲基苯酚(2,4-DMP)。LPME方法的第一步萃取采用普通容量瓶和正辛醇,第二步萃取使用NaOH作为接受相。优化后的萃取条件为:900 μL正辛醇作为萃取溶剂,0.60 mol L(-1)的NaOH作为接受相,萃取时间为5.0分钟,0.01 mol L(-1)的HCl和20.0%的NaCl作为供体相,萃取温度为20.0°C。对50.0 mL在优化的LPME条件下预处理的水样进行分析,得到的检测限(LOD)在0.3至3.5 μg L(-1)之间,定量限(LOQ)在1.2至11.6 μg L(-1)之间,Ph、o-Cr、m-Cr和p-Cr的线性范围为2.50至50.0 μg L(-1),2,4-DMP的线性范围为12.5至250 μg L(-1)。所提出的LPME方法是一种成功的样品制备策略,可对自来水、河水、地下水和海水等水性基质以及土壤提取物中的极性酚类化合物进行精确和准确的定量分析。回收率在72.5%至126.0%之间,相对标准偏差在0.3%至11.5%之间。

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