4.8 Article

Facile Preparation of SiO2/TiO2 Composite Monolithic Capillary Column and Its Application in Enrichment of Phosphopeptides

期刊

ANALYTICAL CHEMISTRY
卷 84, 期 18, 页码 7763-7770

出版社

AMER CHEMICAL SOC
DOI: 10.1021/ac301258q

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资金

  1. Major State Basic Research Development Program of China (973 Program) [2012CB720600, 2012CB720601]
  2. National Natural Science Foundation of China [91017013, 31070327]
  3. Natural Science Fund for Creative Research Groups [20921062]
  4. NSFC
  5. Fundamental Research Funds for the Central Universities

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A novel SiO2/TiO2 composite monolithic capillary column was prepared by sol-gel technology and successfully applied to enrich phosphopeptides as a metal oxide affinity chromatography (MOAC) material. For the monolith preparation, tetramethoxysilane (TMOS) and tetrabutoxytitanium (TBOT) were used as silica and titania source, respectively, and glycerol was introduced to attenuate the activity of titanium precursor, which provided a mild synthetic condition. The prepared monolith was characterized by energy dispersive X-ray spectroscopy (EDX) and X-ray diffraction (XRD). The results revealed an approximate 1/2 molar ratio of titanium to silica as well as an atom-scale homogeneity in the framework. The scanning electron microscopy (SEM) results demonstrated an excellent anchorage between the column and the inner capillary wall, and nitrogen adsorption-desorption experiments showed a bimodal porosity with a narrow mesopore distribution around 3.6 nm. The prepared monolith was then applied for selective enrichment of phosphopeptides from the digestion mixture of phosphoproteins and bovine serum albumin (BSA) as well as human blood serum, nonfat milk, and egg white using an in-tube solid phase microextraction (SPME) system. Our results showed that SiO2/TiO2 composite monolithic capillary column could efficiently enrich the phosphopeptides from complex matrixes. To the best of our knowledge, this is the first attempt for preparing the silica-metal composite monolithic capillary column, which offers the promising application of the monolith on phosphoproteomics study.

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