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Preparation method of a hydrophilic sulfonamide drug molecularly imprinted solid-phase extraction column

A technology of sulfonamide drugs and solid-phase extraction column, which is applied in the preparation of test samples, chemical instruments and methods, ion exchange, etc., can solve the problems that cannot be completely tested with water phase samples, and achieve high price and disposable Use, low cost, solve the effect of large usage

Active Publication Date: 2016-01-20
QILU UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The molecularly imprinted polymers for sulfa drugs prepared in these two inventions can only detect three kinds of sulfa drugs, and they cannot be completely used for the detection of aqueous samples.

Method used

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  • Preparation method of a hydrophilic sulfonamide drug molecularly imprinted solid-phase extraction column
  • Preparation method of a hydrophilic sulfonamide drug molecularly imprinted solid-phase extraction column
  • Preparation method of a hydrophilic sulfonamide drug molecularly imprinted solid-phase extraction column

Examples

Experimental program
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Effect test

Embodiment 1

[0044] (1) Preparation of hydrophilic sulfonamide molecularly imprinted polymer

[0045] First, 0.05 mmol of sulfamethazine and 0.05 mmol of sulfathiazole were dissolved in 6 mL of acetonitrile, and 2 mmol of functional monomer methacrylic acid was added after ultrasonication for 15 min. Oscillate for 3 hours at a speed of 160 rpm on an oscillator to form a pre-polymerization solution. Subsequently, after adding 2 mmol of hydrophilic functional monomer hydroxyethyl methacrylate (HEMA) to the above-mentioned pre-polymerization solution system, shake for 1 h; then add 6 mmol of cross-linking agent (3 mmol of ethylene glycol dimethacrylic acid and 3mmol of 3-(trimethoxysilyl) propyl acrylate), shake for 1h; finally add 25mg of initiator azobisisobutyronitrile (AIBN), shake for 0.5h. Nitrogen gas was passed through to remove oxygen for 5 minutes, and sealed under nitrogen atmosphere; polymerization was initiated by heat in a water bath at 60° C., and the water bath time was 24 h....

Embodiment 2

[0063] Application of the hydrophilic sulfonamide solid-phase extraction column prepared in embodiment 2

[0064] (1) Extraction of ten sulfa drugs from pork

[0065] The purchased pork samples were homogenized in a blender and stored in a -20°C refrigerator. Accurately weigh 1.00 g of pork sample and place it in a 100 mL beaker, and add ten analyte mixed solutions with different concentrations. The protein was denatured by ultrasonication with 3 mL of methanol for 15 min to remove the interference of the protein on the detection of the analyte. repeat three times. The collected supernatant was centrifuged at 3000r / min for 15min. Take the supernatant and filter it through a 0.22 μm filter membrane, transfer it into a 50mL volumetric flask, set the volume to the mark, and wait for purification by solid phase extraction.

[0066] (2) Purification

[0067] Before loading the sample, first activate and equilibrate the solid phase extraction column with 3mL methanol and 3mL de...

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Abstract

The invention belongs to the technical field of chemical detection, and particularly relates to a preparation method of a hydrophilic sulfa drug molecularly imprinted solid-phase extraction column. The preparation method of the hydrophilic sulfa drug molecularly imprinted solid-phase extraction column comprises the following steps: (1) synthesizing a hydrophilic sulfa molecularly imprinted polymer by a bulk polymerization method; (2) characterizing the imprinted polymer obtained in the step (1), and determining the presence of an imprinted binding site; and (3) filling in the polypropylene solid-phase extraction column. The prepared hydrophilic solid-phase extraction column has powerful adsorption function, relatively strong specificity, high recovery rate and relatively low preparation cost, besides, improves the disadvantage of large required solvent amount in a traditional sample pretreatment technology, can be directly used for detection of ten sulfa veterinary drugs in animal-derived foods, and has the characteristics of high selective adsorption and high-efficiency enrichment on the sulfa drugs; and moreover, the solid-phase extraction column can be used for detection of sulfa veterinary drugs in a completely aqueous phase.

Description

technical field [0001] The invention belongs to the technical field of chemical detection, and in particular relates to a preparation method of a hydrophilic sulfonamide drug molecularly imprinted solid-phase extraction column, in particular to its ability to detect sulfamethazine, sulfamethazine, sulfamethazine, and sulfamethazine in animal-derived foods. Enrichment and separation of 10 sulfonamide drugs: thiazole, sulfamerazine, sulfadoxine, sulfachloropyridazine, sulfamethoxine, sulfamethoxazole, sulfamethoxazine and sulfisoxazole. Background technique [0002] Sulfa veterinary drugs are one of the most widely used antibacterial drugs at present. They are widely used to protect and control biological diseases due to their broad-spectrum, high efficiency and low dosage. Residues in edible tissues will cause harm to human health, such as allergic reactions, inhibition of leukocyte production, and urinary system hazards. Therefore, more and more scholars pay high attention ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/285B01J20/30B01D15/08G01N1/34G01N1/40C08F222/14C08F230/08C08F220/06C08F220/28
Inventor 何金兴赵晓磊
Owner QILU UNIV OF TECH
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