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基于多壁碳纳米管的磁性分子印迹聚合物作为一种高选择性的固相微萃取吸附剂,用于超声辅助分散固相微萃取生物流体中的索他洛尔。

A multi-walled carbon nanotube-based magnetic molecularly imprinted polymer as a highly selective sorbent for ultrasonic-assisted dispersive solid-phase microextraction of sotalol in biological fluids.

机构信息

Department of Analytical Chemistry, Faculty of Chemistry, University of Kashan, Kashan, Iran.

出版信息

Analyst. 2018 Jun 11;143(12):2862-2875. doi: 10.1039/c7an02077e.

Abstract

A modified multiwalled carbon nanotube-based magnetic molecularly imprinted polymer (MWCNT-MMIP) was synthesized and applied for selective extraction and preconcentration of sotalol (SOT) in biological fluid samples by using ultrasonic-assisted dispersive solid-phase microextraction (UA-DSPME). The synthetic particles were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), Brunauer-Emmett-Teller (BET) analysis, vibrating sample magnetometry (VSM) and Fourier transform infrared spectroscopy (FTIR). The screening of UA-DSPME was preliminarily performed by Plackett-Burman design (PBD) and, subsequently, central composite design (CCD) under response surface methodology (RSM) was used individually for evaluation of the significant factors and their possible interaction effects on the adsorption process. Batch mode adsorption studies were performed to evaluate the adsorption kinetics, adsorption isotherms, and selective recognition of MWCNT-MMIPs. The adsorption equilibrium of SOT using MWCNT-MMIPs could be well-defined with the Langmuir isotherm model and the maximum adsorption capacity was calculated to be 79.36 mg g-1. Under optimized conditions, the SOT was selectively and effectively extracted in real biological samples and good linearity was obtained with correlation coefficients (R2) over 0.996 and the detection limit (S/N = 3) was 0.31 ng mL-1. The average recoveries of the spiked human urine and plasma samples at four concentration levels of SOT ranged from 94.60-102.50 and 97.40-101.60 percent, respectively, and the relative standard deviation was found to be lower than 4.50%. The results illustrated that the proposed MWCNT-MMIPs@UA-DSPME extraction method coupled with HPLC-UV determination could be applied for sensitive and selective analysis of trace SOT in biological fluid samples.

摘要

一种改良的基于多壁碳纳米管的磁性分子印迹聚合物(MWCNT-MMIP)被合成,并通过超声辅助分散固相微萃取(UA-DSPME)用于选择性提取和预浓缩生物流体样品中的索他洛尔(SOT)。通过扫描电子显微镜(SEM)、透射电子显微镜(TEM)、BET 分析、振动样品磁强计(VSM)和傅里叶变换红外光谱(FTIR)对合成颗粒进行了表征。通过 Plackett-Burman 设计(PBD)对 UA-DSPME 进行了初步筛选,随后在响应面法(RSM)下分别使用中心复合设计(CCD)来评估对吸附过程有显著影响的因素及其可能的相互作用。批量吸附研究用于评估 MWCNT-MMIPs 的吸附动力学、吸附等温线和选择性识别。MWCNT-MMIPs 对 SOT 的吸附平衡可以用 Langmuir 等温线模型很好地定义,最大吸附容量计算为 79.36mg g-1。在优化条件下,MWCNT-MMIPs 可以有效地选择性提取真实生物样品中的 SOT,相关系数(R2)大于 0.996,检测限(S/N = 3)为 0.31ng mL-1。在 SOT 的四个浓度水平下,人尿和血浆样品的平均回收率分别为 94.60-102.50%和 97.40-101.60%,相对标准偏差低于 4.50%。结果表明,所提出的 MWCNT-MMIPs@UA-DSPME 萃取方法与 HPLC-UV 测定相结合,可用于生物流体样品中痕量 SOT 的灵敏选择性分析。

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