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Preparation method for enrofloxacin molecular imprinting monolithic column

A molecular imprinting and enrofloxacin technology, which is applied in material separation, analysis materials, measuring devices, etc., can solve the problems of unstable polymer backbone, non-recyclable, low separation efficiency, etc., and achieve stable and rapid mass transfer capability, Strong affinity and high separation efficiency

Inactive Publication Date: 2015-04-08
HEBEI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a method for preparing a molecularly imprinted monolithic column that specifically recognizes enrofloxacin antibiotics, so as to solve the problems of unstable polymer skeleton, easy shrinkage and deformation, and easy Problems of peeling off from the tube wall, poor pressure resistance, low separation efficiency, short life, and non-recyclable use

Method used

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  • Preparation method for enrofloxacin molecular imprinting monolithic column
  • Preparation method for enrofloxacin molecular imprinting monolithic column
  • Preparation method for enrofloxacin molecular imprinting monolithic column

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] In a Erlenmeyer flask, weigh 0.5 mmol of enrofloxacin, add 0.4 mL of toluene, 1.6 mL of dodecanol and 0.4 mL of polyethylene glycol-200 (PEG-200), after ultrasonic mixing, add the functional monomer methyl Acrylic acid (MAA) 1.0 mmol and hydroxyethyl methacrylate (HEMA) 1.0 mmol were allowed to interact for 2 h to form a complex. Then add 5.0 mmol of ethylene glycol dimethacrylate (EDMA) and 2.5 mmol of trimethylolpropane trimethacrylate (TMPTA) as crosslinking agents, and 30 mg of initiator azobisisobutyronitrile (AIBN), The solution was ultrasonically degassed for 10 min, deoxygenated by nitrogen for 20 min, and then the mixture was injected into a stainless steel chromatographic column (50 mm × 4.6 mm) and sealed. Stand still vertically in a 55°C water bath for 24 h. After the reaction is finished, cool to room temperature, take out the chromatographic column synthesized, remove the sealing head, connect it to the liquid chromatography pump, and remove the porogen a...

Embodiment 2

[0044] Example 2 Performance testing of molecularly imprinted monolithic columns

[0045] (1) Detection method of dynamic adsorption capacity: connect the molecularly imprinted monolithic columns prepared in Examples and Comparative Examples to a chromatograph, use acetonitrile / water (25 / 75, v / v) as mobile phase at 0.8 mL / min Rinse the column at flow rate and monitor at 280 nm until the baseline is stable; then withdraw the monolithic column from the HPLC system and replace with acetonitrile / water (25 / 75, v / v) containing enrofloxacin 1.0 mg / mL The solution is the mobile phase, fully flush the pipeline from the mobile phase inlet to the chromatographic column; then connect the monolithic column back to the chromatographic system, and continue to use the acetonitrile / water (25 / 75) solution of enrofloxacin as the mobile phase, still Perform chromatographic experiments at a flow rate of 0.8 mL / min, and record the detection signal to obtain dynamic breakthrough. The dynamic adsorp...

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Abstract

The invention relates to a preparation method for an enrofloxacin molecular imprinting monolithic column. The preparation method comprises the steps of a, mixing a template molecule, namely enrofloxacin, a functional monomer and a pore-foaming agent, and performing ultrasonic reaction to obtain a compound; b, adding a crosslinking agent and an initiator into the compound, performing ultrasonic degassing, feeding nitrogen, removing oxygen, injecting a mixed solution into a stainless steel column, sealing the stainless steel column, vertically standing the stainless steel column, and performing water bath heating reaction to obtain a molecular imprinting monolithic column; c, connecting the synthesized molecular imprinting monolithic column to a high-pressure transfusion pump, and cleaning for removing the pore-foaming agent and the template molecule through cleaning liquid to obtain the enrofloxacin molecular imprinting monolithic column. The monolithic column prepared by the preparation method disclosed by the invention has a relatively large aperture structure, a uniform and stable framework and a relatively high fluid dynamic characteristic, and is relatively low in back pressure and stable and quick in mass transfer capacity under a relatively high mass transfer rate; a polymer in the column is unlikely to contract and deform and is difficult to be stripped off from the column wall; the service life is long; the enrofloxacin molecular imprinting monolithic column can be recycled, and batch production, popularization and application are facilitated.

Description

technical field [0001] The invention relates to a preparation method of a solid-phase extraction monolithic column in drug residue analysis, in particular to a preparation method of a molecularly imprinted monolithic column with specific recognition for enrofloxacin antibiotics. Background technique [0002] Quinolones (QNs) antimicrobials refer to a class of broad-spectrum antimicrobials that contain a 4-quinone core, which are artificially synthesized. Currently, the third-generation products are widely used, such as enrofloxacin and ciprofloxacin. , norfloxacin, ofloxacin. Among them, Enrofloxacin (Enrofloxacin), also known as ethyl ciprofloxacin, enrofloxacin, its chemical system is named 1-cyclopropyl-7-(4-ethyl-1-piperazinyl)-6 -Fluoro-1,4-dihydro-4-oxo-3-quinoline carboxylic acid, which belongs to the special antibacterial agent of fluoroquinolones designated by the state, is one of the important drugs for the prevention, diagnosis and treatment of animal diseases ....

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/56
Inventor 秦新英张利萍吕运开杨磊
Owner HEBEI UNIVERSITY
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