Amphoteric hydrophilic organic-silica gel hybrid monolithic column and preparation method thereof
A hydrophilic organic and silica gel hybrid technology, which is applied in chemical instruments and methods, inorganic chemistry, separation methods, etc., can solve the problem that strong polar organic monomers are difficult to dissolve in each other, and achieve mechanical stability and good reproducibility. Variety of surface chemistries to address the effect of swelling or shrinkage
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Embodiment 1
[0022] 1) Capillary pretreatment: take a number of the same capillary columns, pass through water for 0.5h, 1M hydrochloric acid for 1h, water for 0.5h, and 1M sodium hydroxide for 0.5h respectively, plug both ends and react at 100°C for 3h; then pass through water for 0.5h , 0.1M hydrochloric acid for 0.5h, water for 0.5h, methanol for 0.25h, acetone for 0.25h, and nitrogen blowing at 180°C for 3h;
[0023] 2) Column preparation: Accurately weigh 270mg of polyethylene glycol and 100mg of urea and dissolve in 2.5mL of 0.01mol / L acetic acid solution. After complete dissolution, add 900μL of TMOS and 300μL of LVTEO to form a pre-polymerization solution, and then stir at 0°C React for 1 hour to form a uniform and transparent hydrolyzate; then, accurately weigh 10 mg of SPP and 0.5 mg of AIBA, add them to 1 mL of the above hydrolyzate, and ultrasonically dissolve and degas in an ice bath for 10 min; manually push the mixed solution into the pretreated solution with a syringe In th...
Embodiment 2
[0026] In the experiment, factors such as the initiator being AIBA and the amount of urea being 100 mg were kept constant, and the influence of the content of the organic monomer on the performance of the column was investigated. The experimental results are as follows: figure 2 shown;
[0027] It can be seen from the figure that the structure of column D is relatively fluffy and its permeability is too good, resulting in poor chromatographic performance, while column B has a uniform structure and good permeability, while the matrix and wall of column E are shedding, making its permeability poor , the small pores of column F are relatively dense and have poor permeability, so separation cannot be achieved.
Embodiment 3
[0029] Using the amphoteric organic-silica gel hybrid monolithic column prepared in Example 1, under the condition of other experimental conditions being fixed, the pH value of the buffer solution was changed, and the relationship between the electroosmotic flow and the pH value of the buffer solution was measured. In the experiment, the proportion of acetonitrile was kept at 50% (v / v), and the ion concentration of the buffer solution was kept constant at 5 mmol / L. The influence of the pH value of the buffer solution from 3.0 to 9.0 on the electroosmotic flow was investigated. The experimental results are as follows image 3 As shown, the triethylamine phosphate buffer solution is 5.0mmol / L, the acetonitrile content is 50%, the pump pressure is 0.7MPa, the separation voltage is -10kV, and the detection wavelength is 214nm.
[0030] from image 3 It can be seen that under the conditions of pH 3.0 and 4.0, the electroosmotic flow decreases with the increase of pH, and the additi...
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