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管内固相微萃取毛细管柱填充介孔 TiO2 纳米粒子用于磷酸肽分析。

In-tube solid-phase microextraction capillary column packed with mesoporous TiO nanoparticles for phosphopeptide analysis.

机构信息

Beijing Key Laboratory for Green Catalysis and Separation, Department of Chemistry and Chemical Engineering, Beijing University of Technology, Beijing, P. R. China.

出版信息

Electrophoresis. 2019 Aug;40(16-17):2142-2148. doi: 10.1002/elps.201900055. Epub 2019 May 9.

DOI:10.1002/elps.201900055
PMID:31032959
Abstract

In this study, an in-tube solid-phase microextraction column packed with mesoporous TiO nanoparticles, coupled with MALDI-TOF-MS, was applied to the selective enrichment and detection of phosphopeptides in complex biological samples. The mesoporous TiO nanoparticles with high specific surface areas, prepared by a sol-gel and solvothermal method, were injected into the capillary using a slurry packing method with in situ polymerized monolithic segments as frits. Compared with the traditional solid-phase extraction method, the TiO -packed column with an effective length of 1 cm exhibited excellent selectivity (α-casein/β-casein/BSA molar ratio of 1:1:100) and sensitivity (10 fmol of a β-casein enzymatic hydrolysis sample) for the enrichment of phosphopeptides. These performance characteristics make this system suitable for the detection of phosphorylated peptides in practical biosamples, such as nonfat milk.

摘要

在这项研究中,采用介孔 TiO2 纳米粒子填充的管内固相微萃取柱,结合 MALDI-TOF-MS,用于选择性富集和检测复杂生物样品中的磷酸肽。通过溶胶-凝胶和溶剂热法制备的具有高比表面积的介孔 TiO2 纳米粒子,采用原位聚合整体柱段作为烧结片的浆料填充方法注入毛细管中。与传统的固相萃取方法相比,有效长度为 1cm 的 TiO2 填充柱对磷酸肽的富集表现出优异的选择性(α-酪蛋白/β-酪蛋白/BSA 摩尔比为 1:1:100)和灵敏度(10fmolβ-酪蛋白酶解样品)。这些性能特点使该系统适用于实际生物样品中磷酸化肽的检测,如脱脂牛奶。

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