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Preparation method and application of hollow mesoporous molecularly imprinted polydopamine nanoparticle adsorbent of pomegranate-like structure

A technology of molecular imprinting and polydopamine, which is applied in the field of analytical chemistry pretreatment, can solve the problems of analyte and internal recognition site combined with a single mesoporous structure, complex and lengthy preparation process, poor biocompatibility, etc., to achieve good recognition High performance, high extraction recovery, and low reagent consumption

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

AI Technical Summary

Problems solved by technology

Although the advantages of imprinted mesoporous materials have been described in many previously published works, there are still four main factors that limit their application: (1) strong acid reflux or high temperature heating are indispensable in the process of removing common porogens such as CTAB ; (2) Traditional polymeric monomers such as silane and methacrylic acid are difficult to degrade and have poor biocompatibility; (3) The combination of analyte and internal recognition site is limited by a single mesoporous structure; (4) Complicated and lengthy preparation process
Therefore, it remains a challenge to prepare a mild, biocompatible and broadly applicable imprinted mesoporous material.

Method used

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  • Preparation method and application of hollow mesoporous molecularly imprinted polydopamine nanoparticle adsorbent of pomegranate-like structure
  • Preparation method and application of hollow mesoporous molecularly imprinted polydopamine nanoparticle adsorbent of pomegranate-like structure
  • Preparation method and application of hollow mesoporous molecularly imprinted polydopamine nanoparticle adsorbent of pomegranate-like structure

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Example 1. Preparation method of hollow mesoporous molecularly imprinted polydopamine nanoparticles with pomegranate-like structure

[0028] (1) Step 1. Synthesis of macrolide molecularly imprinted polydopamine particles: first, 0.18 g of F-127 and 0.2085 mL of TMB were dissolved in a mixture of ultrapure water (30 mL) and EtOH (30 mL), and then Sonicate for 30 minutes. Subsequently, 7.4 mg of erythromycin was added under mechanical stirring. After 30 minutes, 45 mg of TRIS was dissolved in 5 mL of ultrapure water to form a mixed solution, and added to the mixture. Then 30 mg of dopamine hydrochloride was added. The reaction mixture was stirred at room temperature for 24 hours, then the product particles were isolated by centrifugation. The centrifuged pellet was washed with ethanol and acetone.

[0029] (2) Step 2. Synthesis of macrolide molecularly imprinted hollow porous polydopamine particles: removal of organic porogen by extraction, wherein the sample is mixed...

Embodiment 2

[0030] Example 2. Validation of the effect of MIMPDA on the enrichment and concentration of macrolides

[0031] (1) SEM photos of MIMPDA and NIMPDA

[0032] Transmission electron microscope pictures of MIMPDA and NIMPDA materials are shown in figure 2 shown. It can be seen that MIMPDA presents a hollow porous structure after the TMB core is removed by the mixture of ethanol and acetone, so it has a larger specific surface area and pore volume, thereby having a higher adsorption capacity and mass transfer rate.

[0033](2) In order to verify the presence of imprinted sites on the prepared pomegranate-like hollow mesoporous molecularly imprinted polydopamine nanomaterials, MIMPDA and NIMPDA were used as dispersed solid-phase extraction materials to dissolve 40 μg / kg of azithromycin (AZI), Milk samples of spiramycin (SPI), tilmicosin (TILM), clarithromycin (CLA), josamycin (JOS), roxithromycin (ROX), and tylosin (TYL) were the above The sample liquid was subjected to a parall...

Embodiment 3

[0034] Example 3. Method validation of pomegranate-like hollow mesoporous molecularly imprinted polydopamine nanoparticle adsorbent for the analysis of macrolide antibiotics

[0035] (1) Based on the linearity of the DSPE-HPLC-MS / MS method of the prepared pomegranate-like structure hollow mesoporous molecularly imprinted polydopamine nanoadsorbent, a series of mixed model macrolide antibiotics were constructed in milk samples. As shown in Table 1, within the linear range of 0.8-80 μg kg-1, the DSPE-HPLC-MS / MS program showed good linearity for all seven macrolide antibiotics, and the correlation coefficient (R2) was higher than 0.992. In antibiotic residue analysis, the sensitivity of the method is usually expressed as the limit of detection (LOD) and limit of quantitation (LOQ). In this study, LOD and LOQ were estimated to be three and ten times the signal-to-noise ratio (S / N), respectively. The data are shown in Table 1, the LOD range of 7 macrolide antibiotics is 0.009-0.0...

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Abstract

The invention discloses a hollow mesoporous molecularly imprinted polydopamine nanoparticle adsorbent of a pomegranate-like structure and a preparation method and application thereof. Dopamine is adopted as a functional monomer, Pluronic F-127 and 1,3,5-trimethylbenzene (TMB) are adopted as organic pore forming agents, and a template molecule is imprinted in a material. An organic-organic self-polymerization approach is adopted, and on the basis of the Pi-Pi interaction between 1,3,5-trimethylbenzene droplets and polydopamine (PDA) particles formed by self-polymerization of the dopamine, a mesoporous molecularly imprinted polymer having a memory function for a stereoscopic structure of the template molecule is obtained through synthesis. The mesoporous molecularly imprinted polymer is usedas a dispersed solid-phase extraction adsorbent and used for enriching and selectively separating an analyte, and in combination with HPLC-MS / MS detection, a good effect is achieved. The preparationmethod is simple, the adsorption capacity and the mass transfer rate are high, the selectivity is great, the service life is long, and the adsorbent has a broad application prospect in the fields of analytical chemistry and environmental analysis.

Description

technical field [0001] The invention relates to the field of analytical chemistry pretreatment, in particular to a pomegranate-like structure hollow mesoporous molecularly imprinted polydopamine nanoparticle adsorbent applied to the highly selective separation of macrolide antibiotic residues in animal-derived foods Preparation method and application. Background technique [0002] Macrolide antibiotics (MACs) are a class of weakly polar and basic molecules with macrolides. Macrolide antibiotics have strong antibacterial activity against most Gram-positive bacteria, some Gram-negative bacteria, and less common pathogens, they have a broader antibacterial spectrum than beta-lactam antibiotics, and Less likely to cause allergic reactions. Therefore, it is often used as a substitute for β-lactam antibiotics. Studies have shown that macrolide antibiotics not only have antibacterial activity, but also have anti-inflammatory and immunomodulatory effects, and are widely used as fe...

Claims

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Application Information

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IPC IPC(8): C08G73/06C08J9/26B01J20/285B01J20/26
CPCB01J20/268B01J20/285C08G73/0672C08J9/26
Inventor 纪顺利黄佳雯张雨瑞范雯嘉杨艺辉
Owner CHINA PHARM UNIV
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