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基于纳米结构印迹聚合物的涡旋辅助分散微固相萃取:分光光度法和溶液扫描法的比较研究。

Vortex-assisted dispersive micro-solid phase extraction based on nanostructured imprinted polymer: A comparison study between spectrophotometric and solution scanometric techniques.

机构信息

Chemistry Department, Yasouj University, Yasouj 75918-74831, Iran.

Chemistry Department, Yasouj University, Yasouj 75918-74831, Iran.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2022 May 30;1199:123262. doi: 10.1016/j.jchromb.2022.123262. Epub 2022 Apr 26.

DOI:10.1016/j.jchromb.2022.123262
PMID:35489127
Abstract

In the present work, methyl red molecularly imprinted polymeric (MR-MIP) nanostructure was synthesized using the precipitation polymerizations for the separation of MR dye from aqueous media. The as-prepared MIP was characterized using colorimetry, infrared (IR) spectroscopy, and scanning electron microscopy (SEM). In addition, vortex-assisted dispersive micro-solid phase extraction (VAD-µSPE) based on MIP nanostructure was accomplished as a simple and efficient method for selective preconcentration of low amounts of MR from aqueous solutions. The effects of important parameters such as pH, adsorbent dose, eluent volume, and vortex adsorption-desorption time on the extraction efficiency were investigated. Two techniques including UV-Vis absorption spectroscopy and solution scanometry were applied for the analysis of MR content, comparatively. In spectrophotometric determination, the highest recovery was observed at pH 3.5 after 5 and 3 min of vortex time in the adsorption and desorption steps. The preconcentration factor of 75 and a wide linear concentration range (0.010 and 2.0 mg.L; R = 0.996) and low detection limit (LOD = 5.0 µg.L) with an acceptable precision (RSD = 3.4 %) was observed, too. Under optimum conditions in scanometric determination, a high preconcentration factor (i.e. 500) and similar linearity (0.010-2.0 mg.L; R = 0.989) and a low LOD of 3.1 µg.L, with the relative standard deviation of 1.4% was observed. Both techniques were used for MR recovery from various aqueous samples, successfully.

摘要

在本工作中,采用沉淀聚合方法合成了甲基红分子印迹聚合物(MR-MIP)纳米结构,用于从水介质中分离 MR 染料。所制备的 MIP 采用比色法、红外(IR)光谱法和扫描电子显微镜(SEM)进行了表征。此外,基于 MIP 纳米结构的涡旋辅助分散微固相萃取(VAD-µSPE)作为一种从水溶液中选择性预浓缩低浓度 MR 的简单高效方法得到了实现。考察了 pH 值、吸附剂剂量、洗脱剂体积和涡旋吸附-解吸时间等重要参数对萃取效率的影响。应用紫外可见吸收光谱法和溶液扫描法两种技术对 MR 含量进行了分析,进行了比较。在分光光度法测定中,在吸附和解吸步骤中涡旋时间为 5 和 3 分钟时,在 pH 3.5 下观察到最高的回收率。观察到 75 的预浓缩因子和较宽的线性浓度范围(0.010 和 2.0 mg.L; R = 0.996)和低检测限(LOD = 5.0 µg.L),具有可接受的精密度(RSD = 3.4 %)。在扫描测定的最佳条件下,观察到 500 的高预浓缩因子(即)和类似的线性度(0.010-2.0 mg.L; R = 0.989)和低 LOD 为 3.1 µg.L,相对标准偏差为 1.4%。两种技术均成功用于从各种水样品中回收 MR。

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