Preparation method and application of thermosensitive macrolide antibiotics molecular-imprinting solid-phase-micro-extracted fibers

A macrolide and molecular imprinting technology, applied in the field of analytical chemistry pretreatment, can solve the problems that have not yet been seen, and achieve the effects of improving repeatability and uniformity, easy control of thickness and high selectivity

Inactive Publication Date: 2018-01-26
CHINA PHARM UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, there has been no report on the preparation and application of molecularly imprinted solid-phase microextraction fibers for thermosensitive macrolide antibiotics

Method used

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  • Preparation method and application of thermosensitive macrolide antibiotics molecular-imprinting solid-phase-micro-extracted fibers
  • Preparation method and application of thermosensitive macrolide antibiotics molecular-imprinting solid-phase-micro-extracted fibers
  • Preparation method and application of thermosensitive macrolide antibiotics molecular-imprinting solid-phase-micro-extracted fibers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Example 1. Preparation method of thermosensitive macrolide antibiotic molecularly imprinted solid-phase microextraction fiber

[0027] (1) A capillary with a length of about 4 cm and an outer diameter of 350 m is burned to remove the outer wall protective layer with a length of 2 cm, and the outer wall is sequentially soaked in 1M sodium hydroxide and 0.1M hydrochloric acid for 1 hour, washed with water until neutral, blown dry with nitrogen, and the volume Silanize the 3-(trimethoxysilyl)propyl acrylate / acetone solution at a ratio of 10%, and dry at 100°C; cut off a glass tube with a length of about 2cm and an inner diameter of 1mm, and dry it; (2) Weigh 0.1mmol of spiramycin, 0.4mmol of N-isopropylacrylamide, and 0.42mmol of methacrylic acid were dissolved in a mixed solvent consisting of 1mL of DMSO and 2mL of chloroform, and the mixed solution was sonicated at room temperature to make the template molecule and the functional unit The body is fully mixed; then add cr...

Embodiment 2

[0029] Example 2. Verification of the effect of MIPs on the enrichment and concentration of macrolides

[0030] (1) The adsorption properties of molecularly imprinted polymers to template molecules were determined at different ratios, see Table 1. Finally established the optimal ratio of template molecule: thermosensitive functional monomer: non-thermosensitive functional monomer: crosslinking agent = 1: 3.5: 4.2: 20, wherein the non-thermosensitive functional monomer is methyl The enrichment effect is best when using acrylic acid. The resulting molecularly imprinted polymers (MIPs) were characterized by infrared spectroscopy, see figure 1 . It can be seen from the infrared spectrum that the MIPs material with eluted template molecules has the same wave number as that contained in non-template imprinted polymers (NIPs), indicating that the template molecules in the obtained MIPs material have been completely removed.

[0031] Table 1 The optimization of the type and ratio o...

example 3

[0037] Example 3. Temperature Sensitivity Characteristics of Thermally Sensitive Molecularly Imprinted Microextraction Fibers

[0038] (1) In order to verify the temperature sensitivity of heat-sensitive molecularly imprinted materials, heat-sensitive molecularly imprinted fibers were used as solid-phase microextraction materials, and spiramycin and tilmicol with a volume of 5 mL and a concentration of 20 μg / mL The solution samples of star and josamycin are the extraction solutions, and the parallel comparative experiments of the extraction amounts at different temperatures are carried out, as shown in Table 2. The results showed that the optimum extraction temperature for different target compounds was different for thermosensitive molecularly imprinted fibers.

[0039] Table 2 Temperature Sensitivity Experiments of Thermosensitive Molecularly Imprinted Fibers

[0040]

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Abstract

The invention discloses high-selectivity molecular-imprinting solid-phase-micro-extracted fibers applied to the determination of residual of trace macrolide antibiotics in animal-derived foods and preparation method of the high-selectivity molecular-imprinting solid-phase-micro-extracted fibers. The molecular-imprinting solid-phase-micro-extracted fibers with controllable synthesized coating thickness, disclosed by the invention, are obtained by taking spiramycin as template molecules by adopting a tube-sleeving thermal-initiated polymerization method. The molecular-imprinting solid-phase-micro-extracted fibers have a memory function on three-dimensional structures of the macrolide antibiotics such as the spiramycin, tilmicosin and josamycin. The molecular-imprinting solid-phase-micro-extracted fibers can be used for carrying out high-selectivity enrichment on the macrolide antibiotics such as the spiramycin, the tilmicosin and the josamycin in sample solutions for residual analysis. The preparation method disclosed by the invention is simple, the prepared extracted fibers are good in chemical and mechanical properties and thermal stability, high in extraction capacity, good in selectivity and long in service life, have temperature sensitivity and have 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 preparation method and application of a molecularly imprinted solid-phase microextraction fiber with high selectivity for the determination of macrolide antibiotic residues in animal source foods. Background technique [0002] The purpose of sample pretreatment is to separate the matrix and coexisting interfering substances, enrich the components to be tested, and improve the detection sensitivity to make up for the lack of existing separation techniques and instrument detection sensitivity. The time required for sample pretreatment accounts for about 60% to 70% of the total analysis time, and the error introduced by the pretreatment process accounts for about 70% to 80% of the entire error. Therefore, the advanced method of sample pretreatment is directly related to the entire analysis. The success or failure of the method. Solid phase microextraction (SPME) i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F222/10C08F220/06C08F220/54C08K9/06C08K3/40C08J9/26B01J20/281B01J20/28G01N30/02G01N30/74
Inventor 纪顺利李腾飞李多丁黎杨文
Owner CHINA PHARM UNIV
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