J. Mater. Sci. Technol. ›› 2020, Vol. 59: 234-242.DOI: 10.1016/j.jmst.2020.02.091
• Research Article • Previous Articles Next Articles
Ruifang Gaoa, Jin Lia, Rui Shia, Yang Zhangb, Fuzhou Ouyanga, Ting Zhanga, Lihua Hua, Guoqiang Xub, Jian Liua,*()
Received:
2020-01-08
Revised:
2020-02-19
Accepted:
2020-02-23
Published:
2020-12-15
Online:
2020-12-18
Contact:
Jian Liu
Ruifang Gao, Jin Li, Rui Shi, Yang Zhang, Fuzhou Ouyang, Ting Zhang, Lihua Hu, Guoqiang Xu, Jian Liu. Highly sensitive detection of phosphopeptides with superparamagnetic Fe3O4@mZrO2 core-shell microspheres-assisted mass spectrometry[J]. J. Mater. Sci. Technol., 2020, 59: 234-242.
Fig. 1. Schematic illustration of synthesis of Fe3O4@mZrO2 microspheres and selective enrichment of phosphorylated peptides for MALDI-TOF analysis. The scheme highlights the difference between the in-situ elution by our approach and the conventional elution method.
Fig. 2. SEM images of (a) Fe3O4 particles, (b) Fe3O4@ZrO2 microspheres, and (c) Fe3O4@mZrO2 microspheres. TEM images of (d) Fe3O4 particles, (e) Fe3O4@ZrO2 microspheres, and (f) Fe3O4@mZrO2 microspheres with an inset for the zoomed-in view. Scale bar: 50 nm. DLS data for (g) Fe3O4 particles, (h) Fe3O4@ZrO2 microspheres, and (i) Fe3O4@mZrO2 microspheres.
Fig. 3. Characterization of different particles. (a) Nitrogen adsorption - desorption isotherms. (b)BJH pore-size distribution curves for Fe3O4@mZrO2 microspheres. (c) Wide-angle X-ray diffraction (XRD) patterns of Fe3O4 particles, Fe3O4 microspheres, and Fe3O4@ZrO2 microspheres. (d)Magnetic hysteresis curves of Fe3O4 particles, Fe3O4@ZrO2 microspheres, and Fe3O4@mZrO2 microspheres.
Fig. 4. Evaluation of the enrichment performance of Fe3O4@mZrO2 microspheres. MALDI-TOF mass spectra for the different concentrations of tryptic digests of β-casein after enrichment using Fe3O4@mZrO2 microspheres. Concentrations of β-casein digests. (a) 140 nM, (b) 14.0 nM (c) 1.40 nM, (d) 140 pM. “*” and “#” indicate phosphorylated peptides and their dephosphorylated homologs, respectively.
Name | Limit of detection (β-Casein digests) | Selectivity (β-Casein/BSA, w/w) | Ref |
---|---|---|---|
Fe3O4-TiNbNS | 200 pM (200 μL) | 1:100 | [ |
Fe3O4@TiO2-ZrO2 | 500 pM (500 μL) | 1:150 | [ |
NC@PMAA@PEGMP-Ti4+ | 500 pM (100 μL) | 1:1500 | [ |
Bi0.15Fe0.15TiO2 | 2 nM (volume N.A.) | 1:1200 | [ |
Fe3O4@mZrO2 | 76 pM (120 μL) | 1:1000 | This work |
Table 1 Performance comparison between Fe3O4@mZrO2 microspheres against the other enrichment materials in the literature reports.
Name | Limit of detection (β-Casein digests) | Selectivity (β-Casein/BSA, w/w) | Ref |
---|---|---|---|
Fe3O4-TiNbNS | 200 pM (200 μL) | 1:100 | [ |
Fe3O4@TiO2-ZrO2 | 500 pM (500 μL) | 1:150 | [ |
NC@PMAA@PEGMP-Ti4+ | 500 pM (100 μL) | 1:1500 | [ |
Bi0.15Fe0.15TiO2 | 2 nM (volume N.A.) | 1:1200 | [ |
Fe3O4@mZrO2 | 76 pM (120 μL) | 1:1000 | This work |
Fig. 5. Evaluation of enrichment specificity of Fe3O4@mZrO2 microspheres. MALDI-TOF mass spectra of Fe3O4@mZrO2 enriched peptides for the different mixing ratios of tryptic digests of β-casein and BSA, (a) 1:1, (b)1:10, (c)1:100, (d)1:1000. The original concentration of β-casein: 70 μM. “*” and “#” indicate phosphorylated peptides and their dephosphorylated homologs, respectively.
Fig. 6. MALDI-TOF mass spectra of the tryptic digest mixture of β-casein and cell extracts (A549) with different concentrations of β-casein. (a) 14.0 μM; (b) 1.40 μM; (c) 140 nM; (d) 14.0 nM. “*” and “#” indicate phosphorylated peptides and their dephosphorylated homologs, respectively.
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