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Macrolide antibiotic high-selectivity solid-phase micro-extraction probe, preparation method thereof and application of probe

A macrolide, high-selectivity technology, applied in the field of chemistry, can solve the problems of low UV response of macrolide antibiotics, restricting the speed of analysis and detection, and difficult to meet detection requirements, and achieves selectivity and enrichment. Strong ability, good linearity, good linearity effect

Inactive Publication Date: 2018-12-25
GUANGDONG INST OF ANALYSIS CHINA NAT ANALYTICAL CENT GUANGZHOU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

High performance liquid chromatography-tandem mass spectrometry is a commonly used method. However, the pretreatment steps of this method are cumbersome, time-consuming and labor-intensive, which restricts the speed of analysis and detection. Another difficulty in analysis is that the ultraviolet response of macrolide antibiotics is extremely low. The residues in the samples are often at trace levels, so conventional liquid phase methods or spectrophotometric methods are difficult to meet the detection requirements

Method used

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  • Macrolide antibiotic high-selectivity solid-phase micro-extraction probe, preparation method thereof and application of probe
  • Macrolide antibiotic high-selectivity solid-phase micro-extraction probe, preparation method thereof and application of probe
  • Macrolide antibiotic high-selectivity solid-phase micro-extraction probe, preparation method thereof and application of probe

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Experimental program
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Embodiment 1

[0035] 1. Preparation of solid-phase microextraction probes

[0036] figure 1The basic process of making the solid-phase microextraction probe is shown. First cut the wooden stick (birch toothpick) into a length of about 2 cm, and then use a knife to further cut the tip of the wooden stick into a thinner tip (0.1-0.2 mm in outer diameter) to make a solid-phase microextraction probe. Solid substrate for needles. Then, put the wooden stick in a double-necked flask, add 100mL of N,N-dimethylformamide (DMF), and then add 5mL of coupling reagent γ-methacryloxypropyltrimethoxysilane (MPS) Reagents, protected by nitrogen, heated to 110 ° C, stirred and refluxed for 24 hours. After the reaction, wash with absolute ethanol to remove unreacted MPS, and dry naturally to obtain a surface-modified vinyl wooden stick.

[0037] Weigh 0.005 mmol of template molecule roxithromycin in 10 mL of acetonitrile, dissolve it by ultrasonic, add 1 mmol of methacrylic acid (Methacrylic acid, MAA) as...

Embodiment 2

[0060] 1. Preparation of solid-phase microextraction probe (with bamboo stick as solid matrix)

[0061] First cut the bamboo stick (bamboo toothpick), and then use a knife to further cut the tip of the bamboo stick into a thinner one) to make the solid matrix of the solid-phase microextraction probe. Then, put the bamboo stick in a double-necked flask, add 100mL of toluene, then add 2mL of coupling reagent γ-methacryloxypropyltrimethoxysilane (MPS) reagent, protect with nitrogen, heat to 100°C and stir Reflux reaction 20h. After the reaction was finished, it was washed with absolute ethanol to remove unreacted MPS, and the surface-modified vinyl bamboo sticks were obtained by natural drying.

[0062] Weigh 0.001mmol of the template molecule roxithromycin in 10mL of acetonitrile, dissolve it by ultrasonic, add 2mmol of methacrylic acid (Methacrylic acid, MAA) as a functional monomer, and pre-polymerize at room temperature overnight; put bamboo sticks into the mixed solution A...

Embodiment 3

[0069] 1. Preparation of solid-phase microextraction probe (wooden stick as solid substrate)

[0070]First cut the wooden stick (birch toothpick) into a length of about 2 cm, and then use a knife to further cut the tip of the wooden stick into a thinner tip (0.1-0.2 mm in outer diameter) to make a solid-phase microextraction probe. Solid substrate for needles. Then, put the wooden stick in a double-necked flask, add 100mL of dichloromethane, then add 4mL of coupling reagent γ-methacryloxypropyltrimethoxysilane (MPS) reagent, nitrogen protection, heat to 120 °C stirring and reflux reaction for 12h. After the reaction, wash with absolute ethanol to remove unreacted MPS, and dry naturally to obtain a surface-modified vinyl wooden stick.

[0071] Weigh 0.003mmol of the template molecule roxithromycin in 15mL of acetonitrile. After ultrasonically dissolving, add 2mmol of methacrylic acid (Methacrylic acid, MAA) as a functional monomer, pre-polymerize at room temperature overnight...

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Abstract

The invention discloses a macrolide antibiotic high-selectivity solid-phase micro-extraction probe, a preparation method thereof and an application of the probe. The probe takes roxithromycin as a template molecule, silanization reaction between a molecularly imprinted material and a solid substrate with hydroxyl-rich surface is implemented, and the molecularly imprinted material is bonded onto the surface of the solid substrate to prepare the solid-phase micro-extraction probe. High-selectivity and high-enrichment extraction of macrolide antibiotics in various complicated substrates can be directly implemented by the solid-phase micro-extraction probe, electrospray ionization mass spectrometry analysis of an enriched compound in the probe can be directly implemented by the extracted solid-phase micro-extraction probe under normal pressure open conditions, and the probe has ideal sensitivity and repeatability.

Description

technical field [0001] The invention belongs to the field of chemistry, and in particular relates to a macrolide antibiotic high-selectivity solid-phase microextraction probe and its preparation method and application. Background technique [0002] Macrolide antibiotics (Macrolide antibiotics, MALs) include erythromycin, spiramycin, clarithromycin, roxithromycin, josamycin, azithromycin, etc., and their common feature is that they have a macrocyclic structure in the molecule. It also has a lactone structure. Such antibiotics have broad antibacterial spectrum, wide distribution in the body after absorption, high tissue concentration, and long half-life, so they are easier to accumulate and store in the form of the original form or its metabolites in animal foods. At present, macrolide antibiotics are widely used, not only in human clinical medicine and livestock and poultry breeding as therapeutic drugs, but also as feed additives. However, unreasonable or excessive use wil...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/30B01D15/10G01N30/06
CPCB01D15/10B01J20/286G01N30/06G01N2030/009
Inventor 杨运云刘耀慧郭鹏然杨秋霞
Owner GUANGDONG INST OF ANALYSIS CHINA NAT ANALYTICAL CENT GUANGZHOU
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