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Method for preparing temperature stimuli responsive intelligent chromatographic column

A chromatographic column and intelligent technology, applied in the field of preparation of temperature-stimulated-responsive intelligent chromatographic columns, can solve the problems of difficult to guarantee separation effect, cumbersome operation in bonding process, affecting separation ability, etc., and achieve low cost of raw materials, environment-friendly, Easy-to-operate effects

Inactive Publication Date: 2012-07-04
HEBEI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this method still has many disadvantages: the bonding process is cumbersome to operate, and the smart gel needs to be prepared before being bonded to the carrier, and factors such as the preparation of the gel, the carrier used, and the bonding conditions will affect the separation. ability, it is more difficult to implement, and the separation effect is difficult to guarantee

Method used

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  • Method for preparing temperature stimuli responsive intelligent chromatographic column
  • Method for preparing temperature stimuli responsive intelligent chromatographic column
  • Method for preparing temperature stimuli responsive intelligent chromatographic column

Examples

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Effect test

Embodiment 1

[0032] A preparation method of a temperature stimulation-responsive intelligent chromatographic column, the steps of which are:

[0033] A. Mix 0.3g N-isopropylacrylamide, 0.20g N,N′-methylenebisacrylamide, 0.08g polyethylene glycol-20000, 10μL 10% w / v ammonium persulfate, 1.4mL deionized Ultrasonic mixing of water;

[0034] Among them, N-isopropylacrylamide is used as polymerized monomer, N, N'-methylenebisacrylamide is used as polymerized crosslinking agent, polyethylene glycol-20000 is used as porogen, 10% w / v ammonium persulfate as an initiator;

[0035] B. Add 10 μL of 10% v / v N, N, N', N'-tetramethylethylenediamine to the reaction product in the previous step after deoxygenation, and mix well;

[0036] Wherein, 10% v / v N, N, N', N'-tetramethylethylenediamine is used as a catalyst;

[0037]C. Pour the reaction product from the previous step into a stainless steel chromatographic column tube and react at -18°C for 24 hours. Install the chromatographic column head at bot...

Embodiment 2

[0041] The difference between the second embodiment of the present invention and the first embodiment is that the amount of each component is: 0.3 g of N-isopropylacrylamide, 0.2 g of N, N'-methylenebisacrylamide, polyethylene glycol Alcohol-20000 0.08 g, 10% w / v ammonium persulfate 10 μL, deionized water 1.4 mL, 10% v / v N,N,N′,N′-tetramethylethylenediamine 10 μL; reaction temperature in Step C The temperature is 25°C, and the reaction time is 24h.

[0042] image 3 From the scanning electron microscope image of the internal morphology of the chromatographic column prepared for this example, it can be seen that the chromatographic column prepared in this example also has micron-sized through holes and a three-dimensional continuous framework.

[0043] Using water as the mobile phase and controlling the temperature, the monolithic chromatographic column prepared in this example can also achieve high-efficiency separation of the six steroid drugs and the three benzene series in...

Embodiment 3

[0045] The difference between the third embodiment of the present invention and the first embodiment is: the amount of each component is: 0.3g of N-isopropylacrylamide, 0.2g of N,N'-methylenebisacrylamide, polyethylene glycol Alcohol-20000 0.01 g, 10% w / v ammonium persulfate 100 μL, deionized water 1.4 mL, 10% v / v N,N,N′,N′-tetramethylethylenediamine 14 μL; reaction temperature in Step C The temperature is 60°C, and the reaction time is 100h.

[0046] Figure 4 From the scanning electron microscope image of the internal morphology of the chromatographic column prepared for this example, it can be seen that the chromatographic column prepared in this example also has micron-sized through holes and a three-dimensional continuous framework.

[0047] Using water as the mobile phase and controlling the temperature, the monolithic chromatographic column prepared in this example can also achieve high-efficiency separation of the six steroid drugs and the three benzene series in Exam...

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Abstract

The invention discloses a method for preparing a temperature stimuli responsive intelligent chromatographic column, which comprises the following steps of: A, uniformly mixing N-Isopropyl acrylamide, N,N'-methylene-bis-acrylamide, polyethylene glycol-20,000, 10 percent w / v ammonium persulfate and deionized water by using ultrasonic waves; B, deoxidizing reaction products in the step A, adding 10 percent v / v N,N,N',N'-tetramethyl ethylene diamine, and uniformly mixing fully; and C, pouring reaction products in the step B into a stainless steel chromatographic column tube, performing reaction at the temperature of between -18 and 60 DEG C for 10 to 100 hours, arranging chromatographic column heads at two ends of the column tube, connecting the column tube to a high pressure pump, and washing the chromatographic column body by using ultrapure water as a mobile phase. The method has the advantage of simple process; the prepared monolithic column has good pore structure, high mechanical strength and high column efficiency; during use, the water is taken as the mobile phase, so the waste and pollution caused by using a large quantity of organic solvent can be avoided; and in the separation process, the action force between reagents and the monolithic column can be controlled only by changing temperature, so the separation is simple and feasible, and the separation effect is good.

Description

technical field [0001] The invention relates to the field of preparation of separation materials, in particular to a preparation method of a temperature stimulation-response intelligent chromatographic column. Background technique [0002] At present, chromatographic columns are usually organic polymer monolithic columns, which are rod-shaped monoliths prepared in situ from monomers, cross-linking agents, initiators, porogens, etc., and have the advantages of simple preparation, good reproducibility, and excellent porosity. Advantages, can achieve rapid and efficient separation of target objects. However, it still has disadvantages such as difficult control of pore size and pore size distribution, inhomogeneous internal structure, and low column efficiency for separating small molecules; pollute the environment. [0003] Stimuli-responsive polymers refer to a class of polymer substances that can respond to subtle changes in the external environment and produce correspondin...

Claims

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Application Information

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IPC IPC(8): B01J20/285B01J20/30
Inventor 刘海燕杨更亮刘名权
Owner HEBEI UNIVERSITY
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