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Preparation method and application of magnetic core-hollow porous molecular imprinting polymer satellite assembly for macrolide antibiotics

A macrolide, molecular imprinting technology, applied in the field of analytical chemistry pretreatment, can solve the problems of laborious pretreatment procedures, reduced extraction efficiency, lack of selectivity, etc., and achieves fast mass transfer, large adsorption capacity, and adsorption The effect of capacity

Active Publication Date: 2019-09-06
CHINA PHARM UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these sample pretreatment procedures are laborious and time-consuming
And, due to the lack of selectivity, traditional adsorbents such as C18, hydrophilic-lipophilic equilibrium adsorbents, and strong cation exchangers, are often interfered by coexisting components, reducing the extraction efficiency

Method used

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  • Preparation method and application of magnetic core-hollow porous molecular imprinting polymer satellite assembly for macrolide antibiotics
  • Preparation method and application of magnetic core-hollow porous molecular imprinting polymer satellite assembly for macrolide antibiotics
  • Preparation method and application of magnetic core-hollow porous molecular imprinting polymer satellite assembly for macrolide antibiotics

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Example 1. A method for preparing a magnetic core-hollow porous molecularly imprinted polymer satellite assembly of macrolide antibiotics

[0030] (1) Step 1, Fe 3 O 4 Preparation of @polyDA particles: add 2~6g FeCl 3 ·6H 2 O and 0.5~3g sodium citrate dihydrate are dissolved in 50~100mL ethylene glycol, and then 3~6g sodium acetate are added and stirred. Then, the obtained mixture was sealed in a stainless steel autoclave and heated at 200°C for 10-20h to obtain Fe 3 O 4 NPs. Weigh 10~60mg Fe 3 O 4 NPs were dispersed in 10-20 mL of dopamine tris (Tris) solution (pH 6-9, 10mM Tris-HCl buffer), and stirred at room temperature for 6-15h. Separate the resulting product with a magnet, and then wash it several times to remove excess dopamine to obtain Fe 3 O 4 @polyDA particles.

[0031] (2) Step 2. Synthesis of hollow porous imprinting material: weigh 15-90 mL of acetonitrile and 2-30 mL of methanol to form a mixed solvent. Weigh 0.2-1.3 mmol of template molecules and dissolve ...

Embodiment 2

[0033] Example 2. For the analysis of Fe in macrolide antibiotics 3 O 4 @polyDA-HPMIPs adsorbent effect verification

[0034] (1)Fe 3 O 4 @polyDA(A), HPMIPs(B) and Fe 3 O 4 The electron microscope picture of @polyDA-HPMIPs(C)(D) is as follows figure 1 What you see. figure 1 A nearly spherical Fe with an average size of about 210nm can be seen 3 O 4 Nanoparticles in Fe 3 O 4 The surface of the nanoparticles has a film with a thickness of about 12nm, indicating that the polyDA film was successfully deposited on Fe by oxidative polymerization. 3 O 4 Nanoparticle surface. figure 1 B shows that HPMIPs with a hollow mesoporous structure have been successfully synthesized. Because of their larger specific surface area and pore volume, they have higher adsorption capacity and adsorption rate. figure 1 C and figure 1 D shows Fe 3 O 4 The surface of @polyDA is connected with HPMIPs, indicating that HPMIPs are successfully grafted on Fe 3 O 4 On the surface of @polyDA, a magnetic core-hollow p...

Embodiment 3

[0037] Example 3. Fe 3 O 4 @polyDA-HPMIPs material testing commercially available honey

[0038] (1) Weigh 2~5g honey in a polypropylene centrifuge tube, add 5~10mL macrolide antibiotic buffer of different concentrations, and use 10~20mL K 2 HPO 4 The analytes were extracted with buffer (20mM, pH 8.0), vortexed and centrifuged, and the supernatant was further purified by Dispersive Solid Phase Extraction (DSPE) and spiked for analysis.

[0039] (2) Put the sample solution into a polypropylene centrifuge tube, add 10-20mg Fe 3 O 4 After @polyDA-HPMIPs, shake at constant temperature for 10-20min. Fast separation of Fe with macrolide antibiotics under strong magnetic field 3 O 4 @polyDA-HPMIPs, rinse with deionized water. Finally, use a methanol solution of 1 to 5% ammonia to treat Fe by ultrasound 3 O 4 @polyDA-HPMIPs to elute captured analytes. After desorption, pass the eluted fraction through N 2 The flow is evaporated to dryness, and then reconstituted with 200 μL of mobile phas...

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Abstract

The invention discloses a high-selectivity magnetic core-hollow porous molecular imprinting polymer satellite assembly applied to determining the residual quantity of trace macrolide antibiotics in animal-derived foods and a preparation method of the assembly. With mesoporous silicon as a sacrificial support template, methacrylic acid as a functional monomer and spiromycin as a template molecule,hollow porous molecular imprinting polymers (HPMIPs) are prepared by means of a thermal initiation polymerization method; ferroferric oxide magnetic nanoparticles (Fe3O4NPs) are prepared by means of asolvothermal method. By utilizing the self-polymerization properties of dopamine, polydopamine-coated ferroferric oxide magnetic nanoparticles (Fe3O4@polyDA) are prepared, the HPMIPs are grafted on the surfaces of the polydopamine-coated ferroferric oxide magnetic nanoparticles (Fe3O4@polyDA), synthesized magnetic hollow porous molecular imprinting polymers (Fe3O4@polyDA-HPMIPs) are obtained andserve as a magnetic dispersion solid phase extraction adsorbent, macrolide drugs are selectively enriched and separated, and in combination with HPLC-MS / MS detection, the effect is ideal. The preparedmaterial has the advantages of high affinity, high adsorption capacity, a good magnetic response effect and the like and has broad application prospects in the field of food detection and the like.

Description

Technical field [0001] The invention relates to the field of analytical chemistry pretreatment, in particular to a method for preparing a magnetic core-hollow porous molecularly imprinted polymer satellite assembly with high selectivity for determining the residues of macrolide antibiotics in animal-derived foods and application. Background technique [0002] The macrolide antibiotics isolated from the culture broth of Streptomyces are a kind of weakly polar and basic molecules. They are macrolides formed by deoxysugar and 14-16 carbon atoms through glycosidic bonds. Lactone antibiotics have strong antibacterial activity against most Gram-positive bacteria, some Gram-negative bacteria, and mycoplasma. Such antibiotics have become one of the four most commonly used anti-infective drugs in clinical treatment. In addition, because it can prevent diseases and promote growth, it is also widely used as a feed additive, which may accumulate in the human body through the food chain, cau...

Claims

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Application Information

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IPC IPC(8): C08G83/00C08F222/38C08F222/14C08F226/06C08F220/06B01J20/26G01N30/02G01N30/06
CPCB01J20/26C08F220/06C08F222/1006C08F222/385C08F226/06C08G83/001C08F222/102C08F222/103G01N30/02G01N30/06
Inventor 纪顺利张雨瑞黄佳雯李腾飞丁黎
Owner CHINA PHARM UNIV
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