Facile synthesis of Cu2+-immobilized magnetic covalent organic frameworks for highly efficient enrichment and sensitive determination of five phthalate monoesters from mouse plasma with HPLC-MS/MS.
Facile synthesis of Cu2+-immobilized magnetic covalent organic frameworks for highly efficient enrichment and sensitive determination of five phthalate monoesters from mouse plasma with HPLC-MS/MS.
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DOI：
10.1016/j.talanta.2022.123923
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发表时间：
2022-09
期刊：
影响因子：
6.1
通讯作者：
Akang Dan;Shasha Zhang;Zhongliang Chen;Jinghan Dong;Wenjun Zheng;Yuxin Tu;Zian Lin;Zongwei Cai-Zongw
中科院分区：
文献类型：
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作者：
Akang Dan;Shasha Zhang;Zhongliang Chen;Jinghan Dong;Wenjun Zheng;Yuxin Tu;Zian Lin;Zongwei Cai-Zongw
由于生物样品的复杂性，开发一种简单、高选择性和灵敏的邻苯二甲酸单酯(MPAE)分析方法仍然是一个挑战。为了解决这一问题，制备了具有核-壳结构的Cu2+固定磁性共价有机骨架(Fe3O4@TtDt@Cu2+复合材料)，通过在Fe3O4NPs表面合成带有固有双功能基团的COFS壳并进一步固定化Cu2+来提高mPAEs的富集率。该复合材料具有较高的比表面积(348.1 m2g−1)、显著的饱和磁化强度(34.94emu g−1)、有序介孔结构、Cu2+的固载化和良好的热稳定性。在此基础上，建立了基于Cu2+固定COF复合材料的磁性固相萃取(MSPE)前处理技术，并对吸附剂用量、吸附时间、洗脱溶剂等关键参数进行了详细的考察。建立的分析方法线性范围宽(L−1为10-8000 ng)，检出限低(LOD为2-10 ng L−1)，相关系数良好(R2≥为0.9904)。此外，该分析方法还成功地应用于小鼠血浆中代谢物mPAEs的高灵敏检测，表明Fe3O4@TtDt@Cu2+复合材料作为一种快速有效的吸附剂在样品前处理中具有良好的应用前景。
Development of a simple, highly selective, and sensitive analytical method for phthalate monoesters (mPAEs) remains a challenge due to the complexity of biological samples. To address this issue, Cu2+immobilized magnetic covalent organic frameworks (Fe3O4@TtDt@Cu2+composites) with core-shell structures were prepared to enhance the enrichment efficiency of mPAEs by a facile approach synthesis of COFs shells with inherent bifunctional groups on Fe3O4NPs and further Cu2+immobilization. The composites exhibit high specific surface area (348.1 m2g−1), outstanding saturation magnetization (34.94 emu g−1), ordered mesoporous structure, Cu2+immobilization, and excellent thermal stability. Accordingly, a magnetic solid-phase extraction (MSPE) pretreatment technique based on Cu2+immobilized COF composites combined with high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was established, and key parameters including the adsorbent amount, adsorption time, elution solvent, etc. were examined in detail. The developed analytical method showed wide linear ranges (10–8000 ng L−1), low limit of detections (LODs, 2–10 ng L−1), and good correlation coefficients (R2≥ 0.9904) for the five mPAEs. Furthermore, the analytical method was also successfully applied to the highly sensitive detection of metabolite mPAEs in mouse plasma samples, indicating the promising application of the Fe3O4@TtDt@Cu2+composites as a quick and efficient adsorbent in the sample pretreatment.