采用Keggin型磷钨酸插层铜铬层状双氢氧化物增强多孔中空纤维作为吸附剂,对所选氯酚进行固相微萃取,并对其进行高效液相色谱定量分析

IF 3.8 2区 化学 Q1 BIOCHEMICAL RESEARCH METHODS Journal of Chromatography A Pub Date : 2023-05-24 DOI:10.1016/j.chroma.2023.463993
Fatemeh Darvishnejad , Jahan Bakhsh Raoof , Milad Ghani , Reza Ojani
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引用次数: 4

摘要

本文采用共沉淀法合成了一种铜铬层状双氢氧化物(Cu/Cr-LDH)。将Cu/Cr-LDH插入到keggin型多金属氧酸盐(H3PW12O40)上。将改性LDH置于中空纤维(HF)的孔中,制备HF-固相微萃取法(HF- spme)的萃取装置。该方法用于自来水、河水和茶叶样品中4-氯酚、2,4-二氯酚和2,4,6-三氯酚的提取。提取的目标物通过高效液相色谱-紫外检测进行定量分析。根据得到的最优条件确定了该方法的线性动态范围(ldr)、检出限(lod)和定量限(loq)等指标。结果表明,LDR在1 ~ 500 μg L−1之间,r2 > 0.9960。lod范围为0.28 ~ 0.36µg L−1,loq范围为0.92 ~ 1.1µg L−1。在(2和10 μg L−1)和(5和10 μg L−1)两种不同浓度下,计算出该方法提取目标分析物的相对标准偏差(rsd %)分别在3.70% ~ 5.30%和3.50% ~ 5.70%之间。富集因子在57 ~ 61之间。为考察该方法的准确性,获得了相对回收率在93 ~ 105%之间的结果。最后,将该方法用于不同水和茶样品中所选分析物的提取。
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Keggin type phosphotungstic acid intercalated copper-chromium-layered double hydroxide reinforced porous hollow fiber as a sorbent for hollow fiber solid phase microextraction of selected chlorophenols besides their quantification via high performance liquid chromatography

Herein, a copper-chromium-layered double hydroxide (Cu/Cr-LDH) was synthesized by the co-precipitation method. The Cu/Cr-LDH was intercalated to the Keggin-type polyoxometalate (H3PW12O40). The modified LDH accommodated in the pores of hollow fiber (HF), to prepare the extracting device for the HF-solid phase microextraction method (HF-SPME). The method was used for the extraction of 4-chlorophenol, 2,4-dichlorophenol, and 2,4,6- trichlorophenol from tap water, river water, and tea sample. The extracted target analytes were quantified via high-performance liquid chromatography-UV detection. The figures of merit of the method such as, linear dynamic ranges (LDRs), limit of detections (LODs) and, limit of quantifications (LOQs), were determined based on the obtained optimum condition. Based on the results, the LDR was between 1 and 500 μg L  1 and r2 higher than 0.9960. The LODs and LOQs were obtained in the ranges of 0.28–0.36 µg L  1 and 0.92–1.1 µg L  1, respectively. The relative standard deviations ((RSDs% for inter-and intra-day) of the method for the extraction of target analytes were calculated in two different concentrations of (2 and 10 μg L  1) and (5 and 10 μg L  1) between 3.70% - 5.30% and 3.50% - 5.70%-respectively. The enrichment factors were obtained between 57 and 61. In order to investigate the accuracy of the method, also the relative recovery was obtained, between 93 and 105%. Finally, the proposed method was used for the extraction of the selected analytes in different water and tea samples.

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来源期刊
Journal of Chromatography A
Journal of Chromatography A 化学-分析化学
CiteScore
7.90
自引率
14.60%
发文量
742
审稿时长
45 days
期刊介绍: The Journal of Chromatography A provides a forum for the publication of original research and critical reviews on all aspects of fundamental and applied separation science. The scope of the journal includes chromatography and related techniques, electromigration techniques (e.g. electrophoresis, electrochromatography), hyphenated and other multi-dimensional techniques, sample preparation, and detection methods such as mass spectrometry. Contributions consist mainly of research papers dealing with the theory of separation methods, instrumental developments and analytical and preparative applications of general interest.
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