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Synthesis of bifunctional TiO2@SiO2-B(OH)2@Fe3O4@TiO2 sandwich-like nanosheets for sequential selective enrichment of phosphopeptides and glycopeptides for mass spectrometric analysis

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Abstract

In this work, the bifunctional TiO2@SiO2-B(OH)2@Fe3O4@TiO2 sandwich-like nanosheets were designed and synthesized for the sequential selective enrichment of phosphopeptides and glycopeptides. Due to the bifunctional property of the titanium dioxide and the boronic acid group, the nanosheets were successfully applied to the enrichment of phosphopeptides and glycopeptides sequentially, evaluated by capturing phosphopeptides from tryptic digestion of model phosphoprotein bovine β-casein diluted to 0.02 ng/μL (8 × 10−16 mol/μL) and glycopeptides from tryptic digestion of model glycoprotein horseradish peroxidase (HRP) diluted to 0.1 ng/μL (2.5 × 10−15 mol/μL). The enrichment selectivity of the bifunctional nanosheets was evaluated by capturing phosphopeptides from a peptide mixture of β-casein and bovine serum albumin (BSA) with the molar ratio of 1:1000 (8.3 × 10−12 mol of β-casein and 8.3 × 10−9 mol of BSA in 100 μL) and glycopeptides from a peptide mixture of HRP and BSA up to the ratio of 1:50 (5.0 × 10−11 mol of HRP and 2.5 × 10−9 mol of BSA in 100 μL).

A workflow of the sequential enrichment strategy for phosphopeptides and glycopeptides by the bifunctional TiO2@SiO2-B(OH)2@Fe3O4@TiO2 sandwich-like nanosheets

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Acknowledgments

This work was supported by National Science Foundation of China (No. 21175026) and National Research Projects (2012YQ12004409, 2012CB910604, and 2013CB911201).

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Authors and Affiliations

  1. Department of Chemistry and Institutes of Biomedical Sciences, Fudan University, Shanghai, 200433, China

    Dongpo Xu, Mingxia Gao, Chunhui Deng & Xiangmin Zhang

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  1. Dongpo Xu
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  2. Mingxia Gao
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  3. Chunhui Deng
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  4. Xiangmin Zhang
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Correspondence to Xiangmin Zhang.

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The research followed the tenets of the Declaration of Helsinki, and the use of the human serum and saliva samples for research was approved by the Ethics Committee of Zhongshan Hospital, Fudan University. All individual participants gave informed consent for the use of these samples.

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Xu, D., Gao, M., Deng, C. et al. Synthesis of bifunctional TiO2@SiO2-B(OH)2@Fe3O4@TiO2 sandwich-like nanosheets for sequential selective enrichment of phosphopeptides and glycopeptides for mass spectrometric analysis. Anal Bioanal Chem 408, 5489–5497 (2016). https://doi.org/10.1007/s00216-016-9647-0

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  • DOI: https://doi.org/10.1007/s00216-016-9647-0

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