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用于食品和水样中痕量金属离子固相萃取和预富集的功能化多孔碳微球填充柱

Functionalized porous carbon microspheres packed column for solid phase extraction and preconcentration of trace metal ions in food and water samples.

作者信息

Ali Syed Ghazanfar, Kapoor Sakshi, Khan Rais Ahmad, Haseen Uzma, Khan Haris Manzoor

机构信息

Department of Microbiology, Jawaharlal Nehru Medical College, Aligarh Muslim University Aligarh-202002 U.P India.

Nanoscale Research Facility, Indian Institute of Technology Delhi Hauz Khas New Delhi-110016 India.

出版信息

RSC Adv. 2024 Oct 29;14(47):34556-34564. doi: 10.1039/d4ra06137c.

Abstract

Porous materials play a crucial role in the extraction of trace analytes; yet, the attainment of high selectivity and efficient regeneration continues to pose a considerable problem. In this study, we employed a green method to synthesize porous carbon microspheres. These microspheres were subsequently functionalized with aminophosphonic acid to facilitate the extraction of heavy metal ions from real samples. A comprehensive analysis of the aminomethylphosphorylated carbon microspheres was conducted using FTIR, SEM, EDX, TEM, BET and water contact angle measuring techniques. The potential optimization of analyte enrichment can be accomplished by the proposed solid-phase extraction (SPE) approach, which notably reduces spectrum interferences following sample purification. Following the IUPAC equation, the detection limit of the proposed method was found to be 0.04 ng mL, after running 20 replicate blank tests. The primary focus of sequestration of trace metal ions is the formation of metal-ligand chelates within the carbon spheres, resulting in enhanced selectivity and extraction rates exceeding 99.9% from samples with low concentrations. The present studies show a significant preconcentration limit of 0.4 ng mL and a substantial preconcentration factor of 500. The method was implemented to examine real food and water samples, and the obtained data exhibit significant accuracy with a relative standard deviation (RSD) of less than 5%.

摘要

多孔材料在痕量分析物的萃取中起着至关重要的作用;然而,实现高选择性和高效再生仍然是一个相当大的问题。在本研究中,我们采用绿色方法合成了多孔碳微球。随后用氨基膦酸对这些微球进行功能化处理,以促进从实际样品中萃取重金属离子。使用傅里叶变换红外光谱(FTIR)、扫描电子显微镜(SEM)、能量色散X射线光谱(EDX)、透射电子显微镜(TEM)、比表面积分析仪(BET)和水接触角测量技术对氨基甲基磷酸化碳微球进行了全面分析。所提出的固相萃取(SPE)方法可以实现分析物富集的潜在优化,该方法在样品净化后显著降低了光谱干扰。根据国际纯粹与应用化学联合会(IUPAC)方程,在进行20次重复空白试验后,所提出方法的检测限为0.04 ng/mL。痕量金属离子螯合的主要重点是在碳球内形成金属 - 配体螯合物,从而提高选择性,并且从低浓度样品中的萃取率超过99.9%。本研究显示了0.4 ng/mL的显著预富集限和500的显著预富集因子。该方法用于检测实际食品和水样,获得的数据具有显著的准确性,相对标准偏差(RSD)小于5%。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/eed8/11521043/d3229721eb76/d4ra06137c-f1.jpg

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