Method for synthesizing integral bed for cracking solution analysis
A synthesis method and monolithic bed technology, applied in the field of biomolecular analysis technology and chromatographic analysis, can solve the problems of chromatographic columns such as easy pollution, low back pressure, and poor mass transfer performance, and achieve the effects of not easy to be polluted, low back pressure, and low cost
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[0020] The present invention provides a kind of synthetic method for the integral bed of lysate analysis, it is characterized in that the method comprises the steps:
[0021] 1) Mixing methacrylates containing epoxy end groups or acrylate monomers containing epoxy end groups with a crosslinking agent, a porogen and an initiator to obtain a reaction mixture, wherein:
[0022] a. The ratio of the amount of the crosslinking agent to the amount of the monomer is 0.05 to 0.2;
[0023] b. The amount of the porogen accounts for 40% to 80% of the volume content of the reaction mixture;
[0024] c. The ratio of the amount of the initiator to the monomer is 0.005 to 0.03;
[0025] 2) Ultrasonically mix the above reaction mixture evenly, add it into the chromatographic column tube, and polymerize in situ to form a monolithic bed, the polymerization temperature is controlled between 50-60°C, and the reaction time is 12-72 hours;
[0026] 3) after the end of the polymerization reaction, ...
Embodiment 1
[0034]Weigh monomer glycidyl methacrylate, crosslinking agent divinylbenzene and trimerized isocyanurate triallyl urate (1: 0.04: 0.01mol / mol / mol); porogen toluene and n-heptane ( Pore agent / reaction mixture 80vol%, toluene / n-heptane 3: 2vol / vol); Initiator azobisisobutyronitrile (initiator / monomer 0.005: 1mol / mol), mix well, pack into a 50 ×4.6mm stainless steel tube, the other end was sealed, and reacted at 50°C for 72 hours. Connect the monolithic bed to the pump and flush with ethanol. Then diethylamine was used as a modifier, ethanol was used as a solvent, the volume content of diethylamine was 25%, the modification reaction was controlled at 50° C., and the reaction time was 9 hours. After the reaction, the monolithic bed was rinsed with ethanol. More than 75% of pores in the monolithic bed synthesized by the present invention have a diameter of more than ten microns, and the modification density of the monolithic bed is about 1.1 mmol / g monolithic bed.
Embodiment 2
[0036] Weigh monomer epoxy ethylene methacrylate, crosslinking agent ethylene glycol dimethacrylate and trivinylbenzene (1: 0.03: 0.06mol / mol / mol); porogen ethylbenzene and n-octane ( Porogen / reaction mixture 75vol%, ethylbenzene / n-octane 1:1vol / vol); Initiator azobisisobutyronitrile (initiator / monomer 0.01:1mol / mol), mix well, put into one end and seal In a 50×4.6mm stainless steel tube, the other end was sealed and reacted at 55° C. for 36 hours. Connect the monolithic bed to the pump and flush with THF. Then, dimethylamine was used as a modifier, tetrahydrofuran was used as a solvent, the volume content of dimethylamine was 75%, the modification reaction was controlled at 60° C., and the reaction time was 3 hours. After the reaction, the monolithic bed was flushed with tetrahydrofuran. More than 75% of pores in the monolithic bed synthesized by the present invention have a diameter of more than ten microns, and the modification density of the monolithic bed is about 0.5 m...
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