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Preparation method of hydrophilic sulfa 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 of incomplete detection of water-phase samples, and achieve high price and disposable Use and solve the effect of large usage and low cost

Active Publication Date: 2014-08-27
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 hydrophilic sulfa drug molecularly imprinted solid-phase extraction column
  • Preparation method of hydrophilic sulfa drug molecularly imprinted solid-phase extraction column
  • Preparation method of hydrophilic sulfa drug molecularly imprinted solid-phase extraction column

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0045] First, dissolve 0.05 mmol of sulfamethazine and 0.05 mmol of sulfathiazole in 6 mL of acetonitrile, and add 2 mmol of functional monomer methacrylic acid after sonication for 15 minutes. Oscillate on a shaker at 160 rpm for 3 hours to form a pre-polymerization solution. Subsequently, after adding 2mmol of the hydrophilic functional monomer hydroxyethyl methacrylate (HEMA) to the above-mentioned prepolymerization solution system, shaking for 1h; then adding 6mmol of crosslinking agent (3mmol 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. Blow in nitrogen to remove oxygen for 5 minutes, and seal under a nitrogen atmosphere; thermally initiate polymerization in a water bath at 60°C, and the water bath time is 24 hours. After the reaction is completed, a bulk polym...

Embodiment 2

[0063] Example 2 Application of the prepared hydrophilic sulfa drug solid phase extraction column

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

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

[0066] (2) Purification

[0067] Before loading the sample, use 3 mL methanol and 3 mL deionized water to activate and equilibrate the solid phase extraction column in sequen...

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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 specifically relates to a preparation method of a hydrophilic sulfa drug molecularly imprinted solid phase extraction column, in particular to its use in animal-derived foods for sulfamethazine, sulfamethazine, and sulfamethazine. The enrichment and separation of 10 sulfa drugs such as thiazole, sulfamethazine, sulfadoxine, sulfachloropyridazine, sulfa-p-methoxypyrimidine, sulfamethoxazole, sulfamethoxazine and sulfisoxazole. Background technique [0002] Sulfonamide veterinary drugs are currently one of the most widely used antibacterial drugs. They are widely used to protect and control biological diseases due to their broad spectrum, high efficiency and low dosage. However, there are currently studies that indicate that excessive use of sulfa veterinary drugs can cause them Residues in edible tissues can cause harm to human health, such as allergic reactions, inhibition of leukocyte ...

Claims

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Application Information

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Patent Type & Authority Applications(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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