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Preparation and application of nano silica-based doxycycline molecularly imprinted polymer

A technology of molecular imprinting and doxycycline, which is applied in the preparation of test samples, other chemical processes, chemical instruments and methods, etc., can solve problems such as oxytetracycline doxycycline residues and the impact on public health

Active Publication Date: 2014-02-05
ANHUI AGRICULTURAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In recent years, some lawbreakers have often abused such drugs for economic benefits, resulting in a large amount of oxytetracycline, chlortetracycline, tetracycline, and doxycycline remaining in animal foods, seriously affecting public health

Method used

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  • Preparation and application of nano silica-based doxycycline molecularly imprinted polymer
  • Preparation and application of nano silica-based doxycycline molecularly imprinted polymer
  • Preparation and application of nano silica-based doxycycline molecularly imprinted polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) By adding 5mL of water, methanol, N,N-dimethylamide, acetonitrile, acetic acid, ethanol, acetone, chloroform, and tetrahydrofuran as solvents, investigate the dissolution effects of different solvents on DOC and MAA, see Table 1. Considering comprehensively, N,N-dimethylformamide was selected as the porogen.

[0023] The dissolving effect of different solvents of table 1 to DOC and MAA

[0024]

[0025] (2) The effect of the ratio of functional monomer MAA, cross-linking agent EDMA, nano-silica and template molecule DOC

[0026] Effect of the ratio of functional monomer MAA to template molecule DOC dosage:

[0027] The experiment fixed the amount of template molecules, changed the amount of functional monomers, and investigated the functional monomers and template molecules when the molar ratio of functional monomers and template molecules was 2:1, 4:1, 6:1, 8:1, and 10:1. After fully combining the template molecule with the functional monomer in the N,N-dimet...

Embodiment 2

[0045] Compare the packing effects of MIP and diatomaceous earth with mass ratios of 1:0, 1:1, 3:2, 2:1, and 3:1. The rate of the sample solution passing through the molecularly imprinted solid phase extraction column (MISPE) and the adsorption effect on the template molecules were compared, and the results are shown in Table 3.

[0046] Table 3 Selection of Preparation Conditions for Molecularly Imprinted Polymer SPE Columns

[0047] Polymer: diatomaceous earth 1:0 1：1 3：2 2：1 3：1

[0048] Filtration rate (mL / min) 0 2.5 1.8 1.2 0.4 Adsorption capacity (μmol / g) 0 19.8 23.3 30.1 35.8

[0049] It can be seen from Table 3 that when the ratio of MIP to diatomaceous earth is 3:1, the adsorption effect of MISPE is better, but the sample loading rate is too slow. When the ratio is 1:1 and 3:2, although the sample passing rate Faster but less effective. Therefore, the optimal ratio is chosen to be 2:1.

[0050] Preparation of DOC mol...

Embodiment 3

[0053] (1) Add 1.0mmol DOC to 20ml DMF, sonicate until it is completely dissolved, add 4mmol MAA, sonicate for 30min to fully interact with DOC and MAA, add 1.0mmol nano-SiO 2 , sonicated for 30min to make nano-SiO 2 Fully dissolve, add 20mmol EDMA and 0.3mmol AIBN, sonicate for 15 minutes, mix evenly, fill with nitrogen and deoxygenate for 10 minutes, seal, react in a water bath at 60°C for 16 hours to obtain a rod-shaped polymer, grind through a 200-mesh sieve, and then pass through a 250-mesh sieve , get the powder between 200-250 meshes, set aside.

[0054] (2) Put the polymer powder obtained in (1) in 20ml of 4% HF, add 3ml of acetone and 3ml of ethanol, stir well, react for 3h, wash the polymer with ultrapure water until the eluent is neutral. The filter residue was oven-dried at 60°C to obtain nano-SiO 2 of polymers.

[0055] (3) Wash the polymer obtained in (2) with (methanol: water: acetic acid = 7: 1.5: 1.5) mixed solution, methanol, and ultrapure water until no D...

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Abstract

The invention relates to a preparation method for a nano SiO2-based doxycycline molecularly imprinted polymer. A doxycycline (DOC) molecularly imprinted polymer with nano silica (nano-SiO2) removed is obtained by using nano-SiO2 as a carrier and DOC as a template molecule, alpha-methylacrylic acid (MAA), ethylene glycol dimethacrylate (EDMA) and 2,2'-azodiisobutyronitrile (AIBN) as functional monomers, a cross-linking agent and an initiator respectively; N,N-dimethylformamide (DMF) as a solvent and through the steps of dissolution, polymerization, SiO2 removal with hydrofluoric acid (HF) and elution. The imprinted polymer is used as a filler for a solid phase extraction column; the obtained solid phase extraction column has good recognizability for the template molecule (DOC) and three template molecule analogues such as tetracycline (TC), oxytetracycline (OTC) and chlortetracycline (CTC); an adsorption rate for DOC can reach 90.2%; an adsorption rate for TC can reach 85.4%; an adsorption rate for OTC can reach 83.7% and an adsorption rate for CTC can reach 86.1%. Therefore, the imprinted polymer can be used for sample pretreatment for residue detections of tetracycline antibiotics in animal derived foods.

Description

technical field [0001] The invention relates to a method for preparing molecularly imprinted polymers; in particular, it relates to a method for preparing molecularly imprinted polymers of tetracycline antibiotics in animal-derived foods. Background technique [0002] Molecular Imprinting Technology (MIT) is a new technology for the preparation of polymer materials with recognition function that has emerged in recent years. It can obtain molecularly imprinted polymers (molecularly imprinted polymers, MIPs). The high selectivity of molecular imprinting recognition comes from a large number of binding sites in the imprinted polymer matrix that match the target molecule in terms of size, shape, and functional groups. This technology has been applied to the preparation of solid-phase extraction column for a single target compound, but there is no report on the preparation method of molecularly imprinted solid-phase extraction column for the separation of multiple compounds of t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F222/14C08F220/06C08J9/26G01N1/34B01J20/26B01J20/30
Inventor 檀华蓉司雄元彭超楼玥
Owner ANHUI AGRICULTURAL UNIVERSITY
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