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Preparation method and application of antibiotic solid-phase extraction material

A technology of solid phase extraction materials and antibiotics, which is applied in separation methods, analysis materials, material separation, etc., can solve problems affecting the effect of adsorption, agglomeration, etc., achieve organic solvent saving, environmental friendliness, and improve separation selectivity and detection sensitivity Effect

Active Publication Date: 2021-08-24
NINGXIA UNIVERSITY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, due to the lamellar structure of LDHs, it appears agglomerated during the synthesis process, which affects its adsorption effect.

Method used

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  • Preparation method and application of antibiotic solid-phase extraction material
  • Preparation method and application of antibiotic solid-phase extraction material
  • Preparation method and application of antibiotic solid-phase extraction material

Examples

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preparation example Construction

[0029] A kind of preparation method of antibiotic solid phase extraction material, following steps:

[0030] (1)Al 2 o 3 Preparation of -C template: Add rapeseed pollen to absolute ethanol and soak for 10-15 hours, then continue ultrasonic soaking for 3-5 hours, and then rinse with deionized water; then add Al(NO 3 ) 3 9H 2 Ultrasonic immersion in O solution for 3-5 hours, followed by centrifugal cleaning with deionized water at 5000-10000r / min for 2-3 times, drying the obtained samples at 50-70°C for 12-24 hours, and placing them in a tube furnace Raise the temperature to 400-600°C at a rate of 5°C / min, and keep it under flowing nitrogen for 60-120min to obtain Al 2 o 3 -C template; rapeseed pollen, absolute ethanol and Al(NO 3 ) 3 9H 2 The addition ratio of O solution is rapeseed pollen: absolute ethanol: Al(NO 3 ) 3 9H 2 O solution = (8-12) g: (300-500) mL: (300-500) mL.

[0031] (2)Al 2 o 3 -Preparation of C@NiAl-LDH: Ni(NO 3 ) 2 ·6H 2 O: Al(NO 3 ) 3 9H ...

Embodiment 1

[0036] The preparation method of the antibiotic solid-phase extraction material of the present embodiment, the following steps:

[0037] (1)Al 2 o 3 -Preparation of template C: soak rapeseed pollen in absolute ethanol for 10 h, then continue ultrasonic soaking for 3 h, and rinse with deionized water; then add Al(NO 3 ) 3 9H 2 Ultrasonic immersion in O solution for 3 h, followed by centrifugal washing with deionized water at 8000 r / min for 3 times, drying the obtained sample at 55 °C for 12 h, and then placing the temperature in a tube furnace to 450 °C at a speed of 5 °C / min. ℃, kept under flowing nitrogen for 60min, to obtain Al 2 o 3 -C template; rapeseed pollen, absolute ethanol and Al(NO 3 ) 3 9H 2 The addition ratio of O solution is rapeseed pollen: absolute ethanol: Al(NO 3 ) 3 9H 2 O solution = 10g: 500mL: 400mL.

[0038] (2)Al 2 o 3 -Preparation of C@NiAl-LDH: Ni(NO 3 ) 2 ·6H 2 O: Al(NO 3 ) 3 9H 2 O: urea = 1:1:20, weigh Ni(NO 3 ) 2 ·6H 2 O, Al(N...

Embodiment 2

[0043] The preparation method of the antibiotic solid-phase extraction material of the present embodiment, the following steps:

[0044] (1)Al 2 o 3 Preparation of -C template: soak rape pollen in absolute ethanol for 14 hours, then continue ultrasonic soaking for 4 hours, and then rinse with deionized water; then add Al(NO 3 ) 3 9H 2 Ultrasonic immersion in O solution for 4 h, followed by centrifugal washing with deionized water at 8000 r / min for 2 times, and drying the obtained sample at 60 °C for 12 h, then placing it in a tube furnace and raising the temperature to 500 °C at a speed of 5 °C / min. ℃, kept under flowing nitrogen for 80min, to obtain Al 2 o 3 -C template; rapeseed pollen, absolute ethanol and Al(NO 3 ) 3 9H 2 The addition ratio of O solution is rapeseed pollen: absolute ethanol: Al(NO 3 ) 3 9H 2 O solution = 12g: 400mL: 450mL.

[0045] (2)Al 2 o 3 -Preparation of C@NiAl-LDH: Ni(NO 3 ) 2 ·6H 2 O: Al(NO 3 ) 3 9H 2 O: urea = 2:1:15, weigh Ni(N...

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Abstract

The invention provides a preparation method and application of an antibiotic solid-phase extraction material, firstly, rape pollen is soaked in an aluminum nitrate solution through an impregnation method, and after drying, an Al2O3-C template with a developed pore structure is prepared through a calcination method; then, an Al2O3-C template is used as a matrix for loading LDH, layered LDH is intercalated to the surface of a biological template, and Al2O3-C coated NiAl-LDH is prepared; and finally, the material is calcined in a muffle furnace, and the composite material Al2O3-C-coated NiAl-LDO with the 3D flower-shaped structure is prepared. The material is stable in property and has good adsorption capacity to the quinolone antibiotics, the maximum adsorption capacity to the quinolone antibiotics is 52.28-64.08 mg / g, the recovery rate can reach 76.4-91.2%, the preparation process is simple, and conditions are mild. The material is used as a solid-phase extraction material to enrich, separate and detect the quinolone antibiotics in a complex matrix, so that the separation selectivity and the detection sensitivity of the quinolone antibiotics are further improved, the efficiency and the reliability of enrichment treatment are improved, the detection process is simple and reliable, the organic solvent is saved, and the material can be repeatedly used and is environment-friendly.

Description

technical field [0001] The invention relates to the technical field of solid phase extraction, in particular to a method for preparing an antibiotic solid phase extraction material. Background technique [0002] Quinolones (QAS) are an important class of synthetic antimicrobials that are widely used in humans, animal husbandry, and aquaculture because of their broad-spectrum antibacterial activity. However, the widespread use and relative stability of QAS have resulted in QAS residues in a variety of environmental and food media. If the QAS residue reaches a certain level and is ingested by consumers for a long time, it may cause allergic reactions, chronic toxicity, disrupt the balance of gastrointestinal flora, and other health effects on the human body. Many countries and organizations have defined the maximum residue limits (MRL) of QAS in foods of animal origin. Due to the relatively low content of QAS in actual samples, belonging to trace levels, and the complexity o...

Claims

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Application Information

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IPC IPC(8): B01J20/20B01J20/28B01J20/30G01N30/02G01N30/06B01D15/20
CPCG01N30/02G01N30/06B01J20/08B01J20/20B01J20/28014B01D15/20G01N2030/062
Inventor 李媛媛杨媛媛马玉龙吉文欣陈阳
Owner NINGXIA UNIVERSITY
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