Monolithic capillary electrochromatographic system based on gold nanoparticles and chitosan chiral molecularly imprinted polymers for enantioseparation of metolachlor and separation of structural analogs

IF 5.3 2区化学 Q1 CHEMISTRY, ANALYTICAL Microchimica Acta Pub Date : 2025-04-09 DOI:10.1007/s00604-025-07142-9

Ziyun Bu, Qiankang Si, Xiaolin Lu, Pei Wang, Dezhen Wu, Yingying Mei

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Abstract

A novel monolithic capillary column (AuNPs@CMIP(poly-Chitosan)@capillary) with hybridized chiral molecular imprinted polymers (CMIPs) as stationary phase was prepared using S-metolachlor (S-MET) as template, chitosan as functional monomer, glutaraldehyde as cross-linker, and aminated-gold nanoparticles (NH₂-AuNPs) as nanocarriers. The capillary electrochromatography (CEC) system constructed by AuNPs@CMIP(poly-Chitosan)@capillary achieved the efficient chiral separation of MET (resolution (Rs) = 9.83) as well as separation of its various structural analogs (Rs > 1.58). In addition, AuNPs@CMIP(poly-Chitosan)@capillary exhibits satisfactory reproducibility and stability. The relative standard deviations (RSDs) of migration times and Rs for intra-day, inter-day, and inter-column were all less than 6.1%, and no significant decline in separation performance was observed after 21 days of storage. NH₂-AuNPs, with their large specific surface area and stable structure, can provide abundant binding sites and play a supporting role, reducing the deformation and collapse of CMIPs’ cavities, and further ensuring the structural stability and separation performance of the stationary phase. Finally, parameters such as imprinting factor and selectivity factor were calculated by adsorption experiments, and the CEC separation mechanism was discussed. The chitosan CMIPs-based capillary monolithic column developed in this work has rarely been reported and is an innovative attempt, providing a feasible and promising approach for the development of CEC chiral monolithic stationary phases.

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基于金纳米颗粒和壳聚糖手性分子印迹聚合物的整体毛细管电色谱系统用于异甲草胺对映体分离和结构类似物分离

以s-甲草胺（S-MET）为模板，壳聚糖为功能单体，戊二醛为交联剂，氨基化金纳米颗粒（NH2-AuNPs）为纳米载体，制备了以杂化手性分子印迹聚合物（CMIPs）为固定相的新型整体毛细管柱（AuNPs@CMIP（poly-壳聚糖）@毛细管）。AuNPs@CMIP（聚壳聚糖）@毛细管构建的毛细管电色谱（CEC）体系实现了MET的高效手性分离（分辨率(Rs) = 9.83）及其各种结构类似物的分离（Rs > 1.58）。此外，AuNPs@CMIP（聚壳聚糖）@毛细管具有良好的重现性和稳定性。日内、日间、柱间迁移时间和Rs的相对标准偏差（rsd）均小于6.1%，贮藏21 d后分离效果未见明显下降。NH2-AuNPs具有较大的比表面积和稳定的结构，可以提供丰富的结合位点并发挥支撑作用，减少CMIPs空腔的变形和坍塌，进一步保证固定相的结构稳定性和分离性能。最后通过吸附实验计算了印迹因子和选择性因子等参数，并对CEC的分离机理进行了探讨。本文所研制的壳聚糖cmips基毛细管整体柱在国内外报道较少，是一种创新的尝试，为开发CEC手性整体固定相提供了一种可行而有前景的方法。图形抽象

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来源期刊

Microchimica Acta 化学-分析化学

CiteScore

9.80

自引率

5.30%

发文量

410

审稿时长

2.7 months

期刊介绍： As a peer-reviewed journal for analytical sciences and technologies on the micro- and nanoscale, Microchimica Acta has established itself as a premier forum for truly novel approaches in chemical and biochemical analysis. Coverage includes methods and devices that provide expedient solutions to the most contemporary demands in this area. Examples are point-of-care technologies, wearable (bio)sensors, in-vivo-monitoring, micro/nanomotors and materials based on synthetic biology as well as biomedical imaging and targeting.