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Azithromycin detection molecular imprinting monolithic micro column and preparation method thereof

A molecular imprinting and azithromycin technology, applied in the field of material chemistry, can solve the problems affecting the sensitivity and accurate quantification of detection methods, strong matrix effect, lack of selectivity, etc., to overcome cumbersome pretreatment, high selectivity and specificity, high affinity. Peaceful and selective effects

Inactive Publication Date: 2015-08-12
SOUTH CHINA AGRI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the macrocyclic lactone structure of azithromycin itself, there is no characteristic ultraviolet absorbing group, and the ultraviolet detection of high performance liquid chromatography is not sensitive; at present, high performance liquid chromatography-tandem mass spectrometry is generally used to analyze azithromycin residues. Although the sensitivity is greatly improved, the pretreatment Generally, protein precipitation or traditional solid-phase extraction cartridges (such as C 18 , HLB), lack of selectivity, poor specificity, unsatisfactory purification, strong matrix effect in analysis and determination, thus affecting the sensitivity and accurate quantification of the entire detection method

Method used

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  • Azithromycin detection molecular imprinting monolithic micro column and preparation method thereof
  • Azithromycin detection molecular imprinting monolithic micro column and preparation method thereof
  • Azithromycin detection molecular imprinting monolithic micro column and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] (1) Weigh 0.034g (0.04mmoL) spiramycin into a test tube, add 500μL of a mixed porogen of toluene and dodecanol (1:4, v / v), vortex to dissolve, then add 13.6μL ( 0.16mmoL) methacrylic acid functional monomer, ultrasonic for 5min, and stand for 1h to form a prepolymer.

[0047] (2) Add 150μL (0.8mmoL) of ethylene glycol dimethacrylate and 2mg (0.012mmol) of azobisisobutyronitrile to the above-mentioned prepolymer, sonicate for 2min, blow nitrogen gas for 5min, and pipette 40μL into a sealed container at one end. sealed in a small pipette tip, and polymerized in a vacuum oven at 60°C for 24 hours to obtain a small pipette tip for imprinted micro-extraction.

[0048] (3) Seal both ends of the above-mentioned small pipette tip, connect a 2.5mL syringe, load it on a screw syringe pump, and wash it with 6mL of a mixed solution of acetic acid and methanol (the volume ratio of acetic acid and methanol is 1:9, v / v) The template spiramycin was removed, and the flow rate was set t...

Embodiment 2

[0052] (1) Weigh 0.034g (0.04mmoL) tilmicosin into a test tube, add 600μL toluene / dodecanol (1:4, v / v) mixed porogen, vortex to dissolve, then add 13.6μL (0.16mmoL) methacrylic acid functional monomer, sonicated for 5min, and allowed to stand for 1h to form a prepolymer.

[0053] (2) Add 150μL (0.8mmoL) of ethylene glycol dimethacrylate and 2mg (0.012mmol) of azobisisobutyronitrile to the above-mentioned prepolymer, sonicate for 2min, blow nitrogen gas for 5min, and pipette 40μL into a sealed container at one end. sealed in a small pipette tip, and polymerized in a vacuum oven at 60°C for 24 hours to obtain a small pipette tip for imprinted micro-extraction.

[0054] (3) Seal both ends of the above-mentioned small pipette tip, connect a 2.5mL syringe, load it on a screw syringe pump, wash with 6mL of a mixed solution of acetic acid and methanol (the volume ratio of acetic acid and methanol is 1:9) to remove template spiral mold The flow rate was 0.05mL / min, and then washed wi...

Embodiment 3

[0058] (1) Weigh 0.034g (0.04mmoL) spiramycin into a test tube, add 500μL of a mixed porogen of toluene and dodecanol (1:4, v / v), vortex to dissolve, then add 13.6μL ( 0.16mmoL) p-vinylbenzoic acid functional monomer, ultrasonic for 5min, and stand for 1h to form a prepolymer.

[0059] (2) Add 150.4μL (0.8mmoL) of ethylene glycol dimethacrylate and 2mg (0.012mmol) of azobisisobutyronitrile to the above prepolymer, sonicate for 2min, blow nitrogen gas for 5min, pipette 40μL and seal at one end sealed, and polymerized in a vacuum oven at 60°C for 24 hours to obtain imprinted micro-extraction tips.

[0060] (3) Seal both ends of the above-mentioned small pipette tip, connect a 2.5mL syringe, load it on a screw syringe pump, and wash it with 6mL of a mixed solution of acetic acid and methanol (the volume ratio of acetic acid and methanol is 1:9, v / v) The template spiramycin was removed at a flow rate of 0.05 mL / min, and acetic acid was removed by washing with 6 mL of methanol at ...

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Abstract

The invention discloses an azithromycin detection molecular imprinting monolithic micro column and a preparation method thereof, and belongs to the technical field of material chemistry. The preparation method of the azithromycin detection molecular imprinting monolithic micro column comprises the following steps: a template, a mixed pore forming agent, a functional monomer, a crosslinking agent and an initiator are polymerized at 50-80 DEG C for 48h, and the template is removed to obtain the azithromycin detection molecular imprinting monolithic micro column. The azithromycin recovery rate of the prepared molecular imprinting monolithic micro column is more than 90%, the prepared molecular imprinting monolithic micro column shows high cross reactivity, high selectivity and specificity, and has a broad application prospect in use as a purification and pretreatment material for analysis of a sample of azithromycin in animal tissues, feeds and environmental water, and other matrix.

Description

technical field [0001] The invention belongs to the technical field of material chemistry, and in particular relates to a molecularly imprinted integral microcolumn for detecting azithromycin and a preparation method thereof. Background technique [0002] Azithromycin, chemical name: (2R, 3S, 4R, 5R, 8R, 10R, 11R, 12S, 13S, 14R)-13-[(2,6-dideoxy-3-C-methyl-3 -O-methyl-α-L-nucleo-hexapyranosyl)oxy]-2-ethyl-3,4,10-trihydroxy-3,5,6,8,10,12,14-hepta Methyl-11-[[3,4,6-trideoxy-3-(dimethylamino)-β-D-xyl-hexapyranosyl]oxy]-1-oxa-6-azacyclodeca Penta-15-one is a 15-membered ring macrolide antibiotic with a nitrogen heterocycle, which has good curative effect on pneumonia caused by Streptococcus pneumoniae, Haemophilus influenzae and Mycoplasma pneumoniae, Streptococcus pyogenes, etc. . Since the drug has not yet been listed as a veterinary clinical drug, the maximum residue limits (MRLs) and testing standards for azithromycin in animal edible tissues have not yet been formulated ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F220/06C08F226/06C08F220/28C08F220/56C08F222/14C08F212/36C08F212/14C08J9/26G01N30/60
Inventor 贺利民杨海翠方炳虎靳珍张嘉慧曾振灵陈红
Owner SOUTH CHINA AGRI UNIV
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