A preparation method of a macroporous organic-inorganic hybrid monolithic column with a hydrophilic outer surface
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A hydrophilic, monolithic column technology, applied in chemical instruments and methods, separation methods, other chemical processes, etc., can solve the problems of poor interference ability of purification matrix, easy adhesion to the surface, short service life, etc., and achieve uniform skeleton , Not easy to shrink and deform, long service life
Inactive Publication Date: 2015-10-28
HEBEI UNIVERSITY
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[0003] The purpose of the present invention is to provide a method for preparing a hydrophilic macroporous organic-inorganic hybrid monolithic column to solve the problem of protein biomacromolecules in existing monolithic columns, especially when separating complex sample matrices. Adhesion to the surface, easy blockage of pores, high back pressure, slow mass transfer rate, poor interference ability of purification matrix, short service life, etc.
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Embodiment 1
[0023] (1) Mix 2:1 organic precursor methyltrimethoxysilane (MTMS) and inorganic precursor tetraethoxysilane, take 2 mL of the mixture and 0.75 mL of porogen methanol and the molar concentration is 1.0 mol / L The catalyst was mixed with 0.55 mL of concentrated nitric acid solution, ultrasonicated, poured into a stainless steel column, sealed, and stood vertically in a 40°C water bath for 12 h; connected to a high-pressure infusion pump, with a flow rate of 0.05 mL / min, methanol and Rinse with N,N-dimethylformamide for 2 h, and dry at 40°C; then connect the high-pressure infusion pump, and wash with methanol, 0.1 mol / L hydrochloric acid, water, and methanol respectively at a flow rate of 0.05 mL / min for 2 h. h, the remaining solvent was blown dry with nitrogen gas to obtain a macroporous organic-inorganic hybrid monolithic column.
[0024] (2) Connect the dried macroporous organic-inorganic hybrid silica monolithic column to a high-pressure infusion pump, and continuously inject...
Embodiment 2
[0027] In step (1) of Example 1, 1:1 organic precursor methyltrimethoxysilane and inorganic precursor tetraethoxysilane (TEOS) were added, and the others were the same as in Example 1.
Embodiment 3
[0029] In the step (1) of Example 1, a 1:2 ratio of organic precursor methyltrimethoxysilane and inorganic precursor tetraethoxysilane was added, and the others were the same as in Example 1.
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Abstract
The invention relates to a preparation method of a macroporous organic-inorganic hybrid monolithic column with outer surface hydrophilicity, comprising the following steps: A, mixing a precursor mixture, methanol and nitric acid, carrying out ultrasonic treatment, filling the mixture into a stainless steel column, sealing, carrying out water bath, flushing, drying, flushing, blowing nitrogen and blow-drying; B, connecting a high pressure solvent delivery pump, carrying out water bath, blowing methanol and 3-(2,3-epoxy propanolato)propyl trimethoxy silane, completely reacting, flushing and drying; and C, blowing methanol and a solution of perchloric acid for flushing, flushing and drying to obtain the macroporous organic-inorganic hybrid monolithic column with outer surface hydrophilicity. The monolithic column prepared by the preparation method can efficiently adsorb a target and exclude biomacromolecule to be adsorbed on the surface. In addition, the monolithic column has advantages of uniform skeleton, large pore diameter, fast mass transfer, high adsorption capacity, low backpressure and good stability, is not easy for shrinkage deformation, and can directly be used as a precolumn to be combined with a high performance liquid chromatograph so as to realize online solid-phase extraction-liquid chromatograph analysis.
Description
technical field [0001] The invention relates to a preparation method of an online solid-phase extraction monolithic column, in particular to a preparation method of a hydrophilic macroporous organic-inorganic hybrid monolithic column on the outer surface. Background technique [0002] Monolithic column (monolithic column) is a continuous bed stationary phase that uses organic or inorganic polymerization methods to perform in-situ polymerization in the chromatographic column. It has the advantages of good permeability, good stability, and surface structure modification. A new type of separation medium, which plays a very important role in the separation and detection of pharmaceutical, chemical, biological and food drug residues. Based on the different materials in the column, the monolithic column can be roughly divided into three categories: organic polymer monolithic column, silica monolithic column and hybrid monolithic column. Silica gel monolithic column has high colum...
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