{"title":"Fe3O4@氮掺杂碳@钯核双壳纳米管作为新型纳米吸附剂用于超声波辅助分散磁性固相萃取有机磷农药。","authors":"Zolfaghar Aladaghlo, Ali Sahragard, Alireza Fakhari, Neda Salarinejad, Siyavash Kazemi Movahed, Minoo Dabiri","doi":"10.1016/j.talanta.2024.126911","DOIUrl":null,"url":null,"abstract":"<p><p>In this study, an ultrasonic assisted dispersive magnetic solid phase extraction leveraging Fe<sub>3</sub>O<sub>4</sub>@nitrogen-doped carbon@Pd core-double shell nanotubes was developed for the extraction of organophosphorus pesticides (OPPs) in trace levels from real samples. Incorporation of Pd species into the structure of the nanosorbent could enhance its interactions with sulfur groups in the structure of OPPs. X-ray photoelectron spectroscopy and X-ray diffraction, brunauer-emmett-teller, field emission scanning electron microscopy, and high-resolution transmission electron microscopy were used to characterize the nanosorbent after its synthesis. Then, effective variables on the extraction efficiency of OPPs using the nanosorbent were optimized. These parameters included 2-propanol as the adsorption solvent; the sample pH of 7.0; the sorbent quantity of 10 mg; and the extraction and desorption times of 3 min. Under optimized conditions, linear ranges with determination coefficients (R<sup>2</sup>) higher than 0.99, low detection limits of 0.30 ng mL<sup>-1</sup>, high preconcentration factors (423-470) and relatively high extraction recoveries (84-94 %) were obtained. The proposed extraction system was then successfully applied to the analysis of OPPs in fruits, vegetables, water, and agricultural soil samples, yielding relative recoveries from 90.4 to 107 %.</p>","PeriodicalId":435,"journal":{"name":"Talanta","volume":"281 ","pages":"126911"},"PeriodicalIF":5.6000,"publicationDate":"2025-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":"{\"title\":\"Fe<sub>3</sub>O<sub>4</sub>@nitrogen-doped carbon@Pd core-double shell nanotubes as a novel nanosorbent for ultrasonic assisted dispersive magnetic solid phase extraction of organophosphorus pesticides.\",\"authors\":\"Zolfaghar Aladaghlo, Ali Sahragard, Alireza Fakhari, Neda Salarinejad, Siyavash Kazemi Movahed, Minoo Dabiri\",\"doi\":\"10.1016/j.talanta.2024.126911\",\"DOIUrl\":null,\"url\":null,\"abstract\":\"<p><p>In this study, an ultrasonic assisted dispersive magnetic solid phase extraction leveraging Fe<sub>3</sub>O<sub>4</sub>@nitrogen-doped carbon@Pd core-double shell nanotubes was developed for the extraction of organophosphorus pesticides (OPPs) in trace levels from real samples. Incorporation of Pd species into the structure of the nanosorbent could enhance its interactions with sulfur groups in the structure of OPPs. X-ray photoelectron spectroscopy and X-ray diffraction, brunauer-emmett-teller, field emission scanning electron microscopy, and high-resolution transmission electron microscopy were used to characterize the nanosorbent after its synthesis. Then, effective variables on the extraction efficiency of OPPs using the nanosorbent were optimized. These parameters included 2-propanol as the adsorption solvent; the sample pH of 7.0; the sorbent quantity of 10 mg; and the extraction and desorption times of 3 min. Under optimized conditions, linear ranges with determination coefficients (R<sup>2</sup>) higher than 0.99, low detection limits of 0.30 ng mL<sup>-1</sup>, high preconcentration factors (423-470) and relatively high extraction recoveries (84-94 %) were obtained. The proposed extraction system was then successfully applied to the analysis of OPPs in fruits, vegetables, water, and agricultural soil samples, yielding relative recoveries from 90.4 to 107 %.</p>\",\"PeriodicalId\":435,\"journal\":{\"name\":\"Talanta\",\"volume\":\"281 \",\"pages\":\"126911\"},\"PeriodicalIF\":5.6000,\"publicationDate\":\"2025-01-01\",\"publicationTypes\":\"Journal Article\",\"fieldsOfStudy\":null,\"isOpenAccess\":false,\"openAccessPdf\":\"\",\"citationCount\":\"0\",\"resultStr\":null,\"platform\":\"Semanticscholar\",\"paperid\":null,\"PeriodicalName\":\"Talanta\",\"FirstCategoryId\":\"92\",\"ListUrlMain\":\"https://doi.org/10.1016/j.talanta.2024.126911\",\"RegionNum\":1,\"RegionCategory\":\"化学\",\"ArticlePicture\":[],\"TitleCN\":null,\"AbstractTextCN\":null,\"PMCID\":null,\"EPubDate\":\"2024/9/18 0:00:00\",\"PubModel\":\"Epub\",\"JCR\":\"Q1\",\"JCRName\":\"CHEMISTRY, ANALYTICAL\",\"Score\":null,\"Total\":0}","platform":"Semanticscholar","paperid":null,"PeriodicalName":"Talanta","FirstCategoryId":"92","ListUrlMain":"https://doi.org/10.1016/j.talanta.2024.126911","RegionNum":1,"RegionCategory":"化学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"2024/9/18 0:00:00","PubModel":"Epub","JCR":"Q1","JCRName":"CHEMISTRY, ANALYTICAL","Score":null,"Total":0}
引用次数: 0
摘要
本研究开发了一种超声波辅助分散磁性固相萃取技术,利用Fe3O4@氮掺杂碳@Pd核双壳纳米管从实际样品中萃取痕量有机磷农药(OPPs)。在纳米吸附剂结构中加入钯元素可增强其与 OPPs 结构中硫基团的相互作用。纳米吸附剂合成后,采用了 X 射线光电子能谱和 X 射线衍射、布伦纳-埃米特-泰勒、场发射扫描电子显微镜和高分辨率透射电子显微镜对其进行了表征。然后,对使用纳米吸附剂萃取 OPPs 的有效变量进行了优化。这些参数包括:吸附溶剂为 2-丙醇;样品 pH 值为 7.0;吸附剂用量为 10 毫克;萃取和解吸时间为 3 分钟。在优化条件下,萃取的线性范围和测定系数(R2)均大于 0.99,检出限低至 0.30 ng mL-1,预浓缩倍数高(423-470),萃取回收率相对较高(84-94 %)。随后,该萃取系统被成功应用于水果、蔬菜、水和农业土壤样品中 OPPs 的分析,相对回收率为 90.4% 至 107%。
Fe3O4@nitrogen-doped carbon@Pd core-double shell nanotubes as a novel nanosorbent for ultrasonic assisted dispersive magnetic solid phase extraction of organophosphorus pesticides.
In this study, an ultrasonic assisted dispersive magnetic solid phase extraction leveraging Fe3O4@nitrogen-doped carbon@Pd core-double shell nanotubes was developed for the extraction of organophosphorus pesticides (OPPs) in trace levels from real samples. Incorporation of Pd species into the structure of the nanosorbent could enhance its interactions with sulfur groups in the structure of OPPs. X-ray photoelectron spectroscopy and X-ray diffraction, brunauer-emmett-teller, field emission scanning electron microscopy, and high-resolution transmission electron microscopy were used to characterize the nanosorbent after its synthesis. Then, effective variables on the extraction efficiency of OPPs using the nanosorbent were optimized. These parameters included 2-propanol as the adsorption solvent; the sample pH of 7.0; the sorbent quantity of 10 mg; and the extraction and desorption times of 3 min. Under optimized conditions, linear ranges with determination coefficients (R2) higher than 0.99, low detection limits of 0.30 ng mL-1, high preconcentration factors (423-470) and relatively high extraction recoveries (84-94 %) were obtained. The proposed extraction system was then successfully applied to the analysis of OPPs in fruits, vegetables, water, and agricultural soil samples, yielding relative recoveries from 90.4 to 107 %.
期刊介绍:
Talanta provides a forum for the publication of original research papers, short communications, and critical reviews in all branches of pure and applied analytical chemistry. Papers are evaluated based on established guidelines, including the fundamental nature of the study, scientific novelty, substantial improvement or advantage over existing technology or methods, and demonstrated analytical applicability. Original research papers on fundamental studies, and on novel sensor and instrumentation developments, are encouraged. Novel or improved applications in areas such as clinical and biological chemistry, environmental analysis, geochemistry, materials science and engineering, and analytical platforms for omics development are welcome.
Analytical performance of methods should be determined, including interference and matrix effects, and methods should be validated by comparison with a standard method, or analysis of a certified reference material. Simple spiking recoveries may not be sufficient. The developed method should especially comprise information on selectivity, sensitivity, detection limits, accuracy, and reliability. However, applying official validation or robustness studies to a routine method or technique does not necessarily constitute novelty. Proper statistical treatment of the data should be provided. Relevant literature should be cited, including related publications by the authors, and authors should discuss how their proposed methodology compares with previously reported methods.