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基于分子印迹的溶胶-凝胶纳米纤维固相微萃取与高效液相色谱在线联用选择性测定乙酰磺胺酸钾。

Molecularly imprinted sol-gel nanofibers based solid phase microextraction coupled on-line with high performance liquid chromatography for selective determination of acesulfame.

机构信息

Department of Chemistry, Amirkabir University of Technology, Hafez, Tehran, Iran.

Department of Chemistry, Amirkabir University of Technology, Hafez, Tehran, Iran.

出版信息

Talanta. 2015 Mar;134:340-347. doi: 10.1016/j.talanta.2014.11.011. Epub 2014 Nov 14.

DOI:10.1016/j.talanta.2014.11.011
PMID:25618677
Abstract

Sol-gel based molecularly imprinted polymer (MIP) nanofiber was successfully fabricated by electrospinning technique on the surface of a stainless steel bar. The manufactured tool was applied for on-line selective solid phase microextraction (SPME) and determination of acesulfame (ACF) as an artificial sweetener with high performance liquid chromatography (HPLC). The selective ability of method for the extraction of ACF was investigated in the presence of some selected sweeteners such as saccharine (SCH), aspartame (ASP) and caffeine (CAF). Electrospinning of MIP sol-gel solution on the stainless steel bar provided an unbreakable sorbent with high thermal, mechanical, and chemical stability. Moreover, application of the MIP-SPME tool revealed a unique approach for the selective microextraction of the analyte in beverage samples. In this work, 3-(triethoxysilyl)-propylamine (TMSPA) was chosen as a precursor due to its ability to imprint the analyte by hydrogen bonding, Van der Walls, and dipole-dipole interactions. Nylon 6 was also added as a backbone and support for the precursor in which sol could greatly growth during the sol-gel process and makes the solution electrospinable. Various effective parameters in the extraction efficiency of the MIP-SPME tool such as loading time, flow rate, desorption time, selectivity, and the sample volume were evaluated. The linearity for the ACF in beverage sample was in the range of 0.78-100.5 ng mL(-1). Limit of detection (LOD) and quantification (LOQ) were 0.23 and 0.78 ng mL(-1) respectively. The RSD values (n=5) were all below 3.5%at the 20 ng mL(-1) level.

摘要

基于溶胶-凝胶的分子印迹聚合物(MIP)纳米纤维通过静电纺丝技术成功地在不锈钢棒表面制造。所制造的工具用于在线选择性固相微萃取(SPME)和高效液相色谱法(HPLC)测定人工甜味剂乙酰磺胺酸钾(ACF)。在存在一些选定的甜味剂(如糖精(SCH)、阿斯巴甜(ASP)和咖啡因(CAF))的情况下,研究了方法对 ACF 提取的选择性能力。MIP 溶胶-凝胶溶液在不锈钢棒上的静电纺丝提供了一种具有高热、机械和化学稳定性的不可破坏的吸附剂。此外,MIP-SPME 工具的应用为饮料样品中分析物的选择性微萃取提供了一种独特的方法。在这项工作中,选择 3-(三乙氧基硅基)-丙胺(TMSPA)作为前体,因为它能够通过氢键、范德华力和偶极-偶极相互作用对分析物进行印迹。还添加了尼龙 6 作为前体的骨架和支撑物,其中溶胶在溶胶-凝胶过程中可以大大生长,并使溶液可静电纺丝。评估了 MIP-SPME 工具萃取效率的各种有效参数,如加载时间、流速、解吸时间、选择性和样品体积。饮料样品中 ACF 的线性范围为 0.78-100.5ngmL(-1)。检测限(LOD)和定量限(LOQ)分别为 0.23 和 0.78ngmL(-1)。在 20ngmL(-1)水平时,RSD 值(n=5)均低于 3.5%。

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