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Rapid synthesis of three-dimensional sulfur-doped porous graphene via solid-state microwave irradiation for protein removal in plasma sample pretreatment

机译:通过固态微波辐射快速合成三维硫掺杂多孔石墨烯,用于血浆样品预处理中的蛋白质去除

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In this work, we prepared three-dimensional sulfur-doped porous graphene (3D-SPG) via solid-state microwave method and first introduced it to plasma sample pretreatment as adsorbent for the removal of proteins. The efficient heating effect of solid-state microwave irradiation endowed the as-prepared 3D-SPG with large specific surface area, porous structures and sulfur-doped conjugated pi electron surface, thus producing an outstanding adsorbent for proteins adsorption. The adsorption behavior of 3D-SPG towards proteins was explored using bovine serum albumin (BSA) as the model protein and several kinetic models and isotherm models were employed to describe the adsorption process. The results indicated that BSA was adsorbed onto 3D-SPG in a monolayer manner with high adsorption capacity, and chemisorption and intraparticle diffusion was the rate controlling step in proteins adsorption process. By applying 3D-SPG as adsorbent to remove proteins in real rat plasma, we found that 3D-SPG solid phase extraction (SPE) gained exceedingly high protein removal efficiency compared with other plasma pretreatment methods, suggesting that 3D-SPG SPE could effectively prevent the deterioration of column performance and decrease the interference caused by matrix effect in the follow-up analysis. Furthermore, in comparison with the tandem mass spectra results between 3D-SPG SPE and methanol precipitation, 3D-SPG SPE demonstrated the ability to extract the protein-binding metabolites which usually could not be extracted by methanol precipitation. This ability made 3D-SPG SPE of great value in untargeted metabolomics profiling, because 3D-SPG SPE could be a complementary method to methanol precipitation to improve the coverage of metabolites.
机译:在这项工作中,我们通过固态微波法制备了三维硫掺杂多孔石墨烯(3D-SPG),首先将其引入血浆样品预处理作为吸附剂以除去蛋白质。固态微波辐射的有效加热效果赋予具有大的比表面积,多孔结构和硫掺杂缀合的PI电子表面的制备的3D-SPG,从而产生蛋白质吸附的杰出吸附剂。使用牛血清白蛋白(BSA)作为模型蛋白和几种动力学模型和等温模型来探讨3D-SPG朝向蛋白质的吸附行为,并采用几种动力学模型来描述吸附过程。结果表明,BSA以高吸附能力的单层方式吸附到3D-SPG上,化学吸附和骨盆分散是蛋白质吸附过程中的速率控制步骤。通过将3D-SPG作为吸附剂除去真正的大鼠等离子体中的蛋白质,我们发现与其他等离子体预处理方法相比,3D-SPG固相提取(SPE)具有非常高的蛋白质去除效率,表明3D-SPG SPE可以有效地防止列性能的恶化并降低了在随访分析中的基质效应引起的干扰。此外,与3D-SPG SPE和甲醇沉淀的串联质谱相比,3D-SPG SPE证明了提取蛋白质结合代谢物的能力,该代谢物通常不能通过甲醇沉淀提取。这种能力使3D-SPG SPE在未明确的代谢组科分析中的价值大,因为3D-SPG SPE可能是甲醇沉淀的互补方法,以改善代谢物的覆盖率。

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