{"title":"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","authors":"Fatemeh Darvishnejad , Jahan Bakhsh Raoof , Milad Ghani , Reza Ojani","doi":"10.1016/j.chroma.2023.463993","DOIUrl":null,"url":null,"abstract":"<div><p>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 (H<sub>3</sub>PW<sub>12</sub>O<sub>40</sub>). 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 <em>L</em> <sup>−</sup> <sup>1</sup> and r<sup>2</sup> higher than 0.9960. The LODs and LOQs were obtained in the ranges of 0.28–0.36 µg <em>L</em> <sup>−</sup> <sup>1</sup> and 0.92–1.1 µg <em>L</em> <sup>−</sup> <sup>1</sup>, 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 <em>L</em> <sup>−</sup> <sup>1</sup>) and (5 and 10 μg <em>L</em> <sup>−</sup> <sup>1</sup>) 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.</p></div>","PeriodicalId":347,"journal":{"name":"Journal of Chromatography A","volume":null,"pages":null},"PeriodicalIF":3.8000,"publicationDate":"2023-05-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"4","resultStr":"{\"title\":\"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\",\"authors\":\"Fatemeh Darvishnejad , Jahan Bakhsh Raoof , Milad Ghani , Reza Ojani\",\"doi\":\"10.1016/j.chroma.2023.463993\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<div><p>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 (H<sub>3</sub>PW<sub>12</sub>O<sub>40</sub>). 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 <em>L</em> <sup>−</sup> <sup>1</sup> and r<sup>2</sup> higher than 0.9960. The LODs and LOQs were obtained in the ranges of 0.28–0.36 µg <em>L</em> <sup>−</sup> <sup>1</sup> and 0.92–1.1 µg <em>L</em> <sup>−</sup> <sup>1</sup>, 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 <em>L</em> <sup>−</sup> <sup>1</sup>) and (5 and 10 μg <em>L</em> <sup>−</sup> <sup>1</sup>) 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.</p></div>\",\"PeriodicalId\":347,\"journal\":{\"name\":\"Journal of Chromatography A\",\"volume\":null,\"pages\":null},\"PeriodicalIF\":3.8000,\"publicationDate\":\"2023-05-24\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"4\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Journal of Chromatography A\",\"FirstCategoryId\":\"1\",\"ListUrlMain\":\"https://www.sciencedirect.com/science/article/pii/S0021967323002194\",\"RegionNum\":2,\"RegionCategory\":\"化学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"\",\"PubModel\":\"\",\"JCR\":\"Q1\",\"JCRName\":\"BIOCHEMICAL RESEARCH METHODS\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Journal of Chromatography A","FirstCategoryId":"1","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/S0021967323002194","RegionNum":2,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q1","JCRName":"BIOCHEMICAL RESEARCH METHODS","Score":null,"Total":0}
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.
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.