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Method for preparing molecular imprinted polymer for recognizing chloromycetin, thiamphenicol and florfenicol simultaneously

The technology of fluorine thiamphenicol and thiamphenicol is applied in the field of preparation of molecularly imprinted polymers, and can solve the problems affecting the wide application of molecularly imprinted solid-phase extraction technology, removing template molecules from polymers, and leakage of template molecules, etc. Achieve the effect of large promotion and application value, improve detection sensitivity and detection efficiency, and strong identification ability

Inactive Publication Date: 2011-07-27
NINGBO UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the current research on molecularly imprinted polymers for chloramphenicol antibiotics is mainly designed based on the specific separation of a single target compound, chloramphenicol, and the template molecules cannot be completely removed from the polymer after conventional elution treatment. , in the subsequent steps of solid phase extraction, including sample loading, rinsing, elution and other operations, the leakage of template molecules is often found. For the detection of trace substances, it increases the system error and directly affects the molecular Wide application of imprinted solid phase extraction technique

Method used

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  • Method for preparing molecular imprinted polymer for recognizing chloromycetin, thiamphenicol and florfenicol simultaneously
  • Method for preparing molecular imprinted polymer for recognizing chloromycetin, thiamphenicol and florfenicol simultaneously
  • Method for preparing molecular imprinted polymer for recognizing chloromycetin, thiamphenicol and florfenicol simultaneously

Examples

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Effect test

Embodiment 1

[0021] Add 1 mmol of functional monomer methacrylic acid (MAA) to 5 ml of porogen acetonitrile, add 25 mmol of cross-linking agent ethylene glycol dimethacrylate (EGDMA), mix well, heat at 40°C for 2 min, and then add template molecules 1 mmol of thiamphenicol was passed through nitrogen for 10-15 minutes, the initiator azobisisobutyronitrile (AIBN) was added, ultrasonic degassed for 5-10 minutes, and sealed under nitrogen or vacuum state. React at 60°C for 36 hours; after the polymerization reaction, take out the synthesized polymer, grind it, sieve it, and use methanol: formic acid (v / v 9 / 1), methanol to remove the template molecule through Soxhlet extraction, and further extract the obtained molecule The imprinted polymer was loaded into a solid-phase extraction column, rinsed with methanol: formic acid (v / v9 / 1) and methanol in sequence, and detected by high-performance liquid chromatography-mass spectrometry until no template molecules were detected; The polymer is vacuum-...

Embodiment 2

[0023] Add 8mmol of functional monomer methacrylic acid (MAA) to 5ml of porogen acetonitrile, add 25mmol of cross-linking agent ethylene glycol dimethacrylate (EGDMA), mix well, heat at 50°C for 2min, and then add template molecules 1 mmol of thiamphenicol was passed through nitrogen for 10-15 minutes, the initiator azobisisobutyronitrile (AIBN) was added, ultrasonic degassed for 5-10 minutes, and sealed under nitrogen or vacuum state. React at 60°C for 36 hours; after the polymerization reaction, take out the synthesized polymer, grind it, sieve it, and use methanol: formic acid (v / v 9 / 1), methanol to remove the template molecule through Soxhlet extraction, and further extract the obtained molecule The imprinted polymer was loaded into a solid-phase extraction column, rinsed with methanol: formic acid (v / v9 / 1) and methanol in sequence, and detected by high-performance liquid chromatography-mass spectrometry until no template molecules were detected; The polymer is vacuum-drie...

Embodiment 3

[0025] Add 1 mmol of functional monomer N, N-diethylaminoethyl methacrylate (DEAEM) to 5 ml of porogen acetonitrile, add 25 mmol of crosslinking agent ethylene glycol dimethacrylate (EGDMA), and mix well , heat at 40°C for 2 minutes, then add 1 mmol of the template molecule thiamphenicol, pass through nitrogen for 10 to 15 minutes, add the initiator azobisisobutyronitrile (AIBN), ultrasonically degas for 5 to 10 minutes, and seal under nitrogen or vacuum state . Reaction at 70°C for 36h; after the polymerization reaction, the synthesized polymer was taken out, ground, sieved, and template molecules were removed by Soxhlet extraction with methanol: formic acid (v / v 9 / 1), methanol, and the obtained molecules were further The imprinted polymer was loaded into a solid-phase extraction column, rinsed with methanol: formic acid (v / v 9 / 1), and methanol in sequence, and detected by high-performance liquid chromatography-mass spectrometry until no template molecules were detected; the ...

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Abstract

The invention relates to a method for preparing a molecular imprinted polymer capable of recognizing chloromycetin, thiamphenicol and florfenicol simultaneously, which belongs to the technical field of bioengineering. The method comprises the following concrete steps: adding a functional monomer and a cross-linking agent into a pore-forming agent, uniformly mixing and heating; then adding template molecule thiamphenicol and an initiating agent, further ultrasonically degassing the mixed solution, sealing in a nitrogen or vacuum pumping state and carrying out polymerization reaction; after thepolymerization reaction is finished, taking the compounded polymer out to grind and screen; eluting by organic solvent to remove template molecules by a combined method of Soxhlet extraction and solid phase-extraction cartridges till the template molecules are not detected by a high performance liquid chromatography-mass spectrometry; finally removing the polymer of the template molecules and drying in vacuum to obtain the molecular imprinted polymer. The polymer can be simultaneously applied to the pre-processing of the antibiotic detection of chloromycetin, thiamphenicol and florfenicol in foods and realizes the specific and selective separation and the efficient enrichment of the chloromycetin, the thiamphenicol and the florfenicol.

Description

technical field [0001] The invention relates to a preparation method of a molecularly imprinted polymer, in particular to a method for preparing a molecularly imprinted polymer that simultaneously recognizes chloramphenicol, thiamphenicol and fluthiamphenicol. Background technique [0002] Chloramphenicol (CAP), Thiamphenicol (TAP) and Fluoramphenicol (Floramphenicol, FF) belong to the chloramphenicol class of antibiotics. Chloramphenicol is decomposed due to the nitro group on its benzene ring. The half-life is long and has serious toxic and side effects. Therefore, chloramphenicol residues in animal foods and aquatic products pose a huge threat to human health. At present, it has been banned from being used in animal-derived foods. 0.1 μg / kg. Thiamphenicol and fluthiamphenicol are widely used as substitutes for chloramphenicol because their toxicity is less than that of chloramphenicol. Existence, the maximum residue limit standard is generally 50 ~ 100μg / kg. Therefore,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F2/44C08F222/14B01J20/30B01J20/26C08J9/26
Inventor 史西志李德祥孙爱丽苏秀榕
Owner NINGBO UNIV
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