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Functionalized mesoporous sio 2 /tio 2 Composite nano-microsphere solid-phase extraction column and preparation method thereof

A solid-phase extraction small column and solid-phase extraction column technology are applied in the field of preparation of mesoporous SiO2/TiO2 nanocomposite materials, and can solve the problems of low sensitivity, complexity, and low ionization efficiency of phosphate ions in mass spectrometry analysis technology, and achieve The desorption process is simple, the steps are simple, and the stability is good.

Inactive Publication Date: 2017-03-29
NANJING UNIVERSITY OF TRADITIONAL CHINESE MEDICINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[See: (a) Pinkse, M.W.H.; Uitto, P.M.; Hilhorst, M.J.; Ooms, B.; Heck, A.J.R. Anal.Chem.2004, 76, 3935-3943. (b) Yue, G.E.; Roper, M.G.; Balchunas, C.; Pulsipher, A.; Coon, J.J.; Shabanowitz, J.; Hunt, D.F.; .] At present, this method encounters many problems: first, because the digested peptide mixture is too complex, phosphorylation generally occurs in a substoichiometric manner, so the abundance of non-phosphorylated peptides is much higher than that of phosphorylated peptides; second, , the mass spectrometry technique used to detect phosphorylated peptides has low sensitivity; third, under low-lifetime mass spectrometry conditions, the ionization efficiency of phosphate ions becomes lower in terms of detection
Although various enrichment methods have been reported, so far, no related functionalized mesoporous SiO 2 / TiO 2 Composite nanomaterials achieve selective enrichment

Method used

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  • Functionalized mesoporous sio <sub>2</sub> /tio <sub>2</sub> Composite nano-microsphere solid-phase extraction column and preparation method thereof
  • Functionalized mesoporous sio <sub>2</sub> /tio <sub>2</sub> Composite nano-microsphere solid-phase extraction column and preparation method thereof
  • Functionalized mesoporous sio <sub>2</sub> /tio <sub>2</sub> Composite nano-microsphere solid-phase extraction column and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1: Functionalized mesoporous SiO 2 / TiO 2 Preparation of composite nano-microsphere filler

[0029] Experimental materials: cetyltrimethylammonium bromide, batch number: J1315062, purchased from Shanghai Aladdin Reagent Co., Ltd.; sodium oleate, batch number: 20120920, purchased from Sinopharm Chemical Reagent Co., Ltd.; n-tetrabutyl titanate , batch number: 20140121, purchased from Shanghai Aladdin Reagent Co., Ltd.; 1,3,5-trimethylbenzene, batch number: I1329044, purchased from Shanghai Aladdin Reagent Co., Ltd.; tetraethyl silicate, batch number: L1306074, purchased From Shanghai Aladdin Reagent Co., Ltd.; 2,5-dihydroxybenzoic acid, batch number: J1312017, purchased from Nanjing Chemical Reagent Co., Ltd.; 3-mercaptopropionic acid, batch number: 38194, purchased from Shanghai Aladdin Reagent Co., Ltd.; Trypsin (1:250), lot number 20130929, Shanghai Aladdin Reagent Co., Ltd.; β-casein, lot number SLBK9882V, Shanghai Aladdin Reagent Co., Ltd.; 3-aminopropyltr...

Embodiment 2

[0042] Example 2: Mesoporous SiO 2 / TiO 2 Preparation of Composite Nanosphere Solid Phase Extraction Cartridge

[0043] A. Preparation of the extraction column

[0044] 1. Empty column material and specification

[0045] The empty column size of existing solid phase extraction cartridges ranges from 100μL to 1mL. The material of the empty column is polypropylene, and there are polyethylene sieve plates with a pore size of 20 μm on the upper and lower sides of the small column. The above-mentioned empty columns can be used in the present invention. In the following experimental example, the present invention adopts the specification of 1 mL.

[0046] 2. Packing of solid phase extraction column

[0047] The solid-phase extraction column is filled with functionalized mesoporous SiO 2 / TiO 2 Composite Nanospheres, Mesoporous SiO 2 The diameter of the nanospheres is 50-150nm, the average pore size is 4-5nm, and the mesoporous SiO 2 Attachment of TiO on the surface of nano-...

Embodiment 3

[0054] Example 3: Select β-casein as the research target, and test the various performance indicators of the solid-phase extraction cartridge

[0055] Experimental materials: β-casein was purchased from Shanghai Aladdin Reagent Co., Ltd., batch number: SLBK9882V; trypsin (1:250) was purchased from Shanghai Aladdin Reagent Co., Ltd., batch number: 20130929; 2,5-dihydroxy Benzoic acid, batch number: J1312017, was purchased from Nanjing Chemical Reagent Co., Ltd.

[0056] Experimental instruments and equipment: the mass spectrometer is MALDI-TOF-MS (AximaTOF 2 mass spectrometry, Shimadzu, Kyoto, Japan), the functionalized mesoporous SiO prepared in the above-mentioned embodiment 2 2 / TiO 2 Composite nano-microsphere solid phase extraction column.

[0057] experiment procedure:

[0058] (1) Take β-casein and prepare a 1mg / mL standard solution for later use (pH8.0, 50mM ammonium bicarbonate solution as solvent); take trypsin and prepare a 0.05mg / mL standard solution for later u...

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Abstract

The invention provides a functional mesoporous SiO2 / TiO2 nanometer microspheres small solid phase extraction column and a preparation method thereof. The small solid phase extraction column is that functional SiO2 / TiO2 nanometer microspheres are used as a substrate; the small solid phase extraction column is prepared by processing original mesoporous SiO2 / TiO2 nanometer microspheres by amination, TiO2 carboxylation covalently chemical functionalization and then compounding by amidation reaction. The filling height of the functional mesoporous SiO2 / TiO2 nanometer microspheres is (0.2-0.5) centimeter. The small solid phase extraction column is mainly applicable to enriching of biological fluids and phosphopeptide in a complex substrate. The solid phase extraction column has the characteristics that the yield of a target substance is high and up to (92-105%), the preparation cost is low, the materials are easily obtained, the functional process is simple, the adaptability is high, and the mass production is easily carried out. The solid phase extraction column has a good application prospect.

Description

technical field [0001] The invention belongs to the technical field of material enrichment related to proteomics in analytical chemistry, and relates to a mesoporous SiO 2 / TiO 2 The preparation method of the nanocomposite material is mainly used for the selective enrichment and detection of phosphorylated proteins, and the enriched samples are detected by mass spectrometry, thereby greatly improving the detection sensitivity of phosphorylated proteins. Background technique [0002] Phosphorylation, the reversible attachment of a covalent phosphate group to one or more amino acids, is the most common protein modification in cellular regulatory mechanisms. In biological theoretical research, phosphorylation is the most basic, common and important mechanism for regulating and controlling protein activity and function, and it participates in various cell regulatory functions, such as controlling cell cycle, signal transduction, differentiation, proliferation, transformation a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/283B01J20/30G01N30/08
Inventor 朱栋胡玥王军朱俊明顾超前倪雯婷周雪莲
Owner NANJING UNIVERSITY OF TRADITIONAL CHINESE MEDICINE