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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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] However, due to the lamellar structure of LDHs, it appears agglom

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

Experimental program
Comparison scheme
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Example Embodiment

[0029] Preparation method of antibiotic solid phase extraction material, the following steps:

[0030] (1) Al 2 O 3 -C template: The rapeseed pollen is added to anhydrous ethanol soaked for 10 to 15 h, then continue to soak for 3 to 5 hours, then rinse with deionized water; then add concentration of 0.25 mol / L of Al (NO 3 ) 3 · 9h 2 In the O solution, the ultrasonic soaked 3 to 5 h, then centrifugated by deionized water at 5,000 to 10,000 r / min radius, and the resulting sample was dried at 50 to 70 ° C for 12 to 24 hours, placed in the tube furnace. Renained from 5 ° C / min to 400 ~ 600 ° C, keeping 60 to 120 min under flowing nitrogen to obtain Al 2 O 3 -C template; rape pollen, absolute ethanol and Al (no 3 ) 3 · 9h 2 The addition ratio of O solution is rape pollen: anhydrous ethanol: Al (NO 3 ) 3 · 9h 2 O Solution = (8-12) g: (300 ~ 500) mL: (300 ~ 500) ml.

[0031] (2) Al 2 O 3 -C @ nial-LDH Preparation: Mass Mole than Ni (NO 3 ) 2 · 6h 2 O: Al (no 3 ) 3 · 9h 2 O: Urea = ...

Example Embodiment

[0035] Example 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 -C template: The rapeseed pollen is added to anhydrous ethanol soaked for 10 h, then continue to soak for 3 h, then rinse with deionized water; then add Al (NO) of 0.25 mol / L. 3 ) 3 · 9h 2 In the O solution, the ultrasonic soaked 3 h, then washed with deionized water at 8000 r / min split at 8000 r / min to dry 12 h at 55 ° C, and the speed was raised in the tube furnace at a rate of 5 ° C / min to 450. ° C, keep 60 min under flowing nitrogen to obtain Al 2 O 3 -C template; rape pollen, absolute ethanol and Al (no 3 ) 3 · 9h 2 The addition ratio of O solution is rape pollen: anhydrous ethanol: Al (NO 3 ) 3 · 9h 2 O Solution = 10g: 500ml: 400ml.

[0038] (2) Al 2 O 3 -C @ nial-LDH Preparation: Mass Mole than 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 (NO 3 ) 3 ·...

Example Embodiment

[0042] Example 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 -C template: The rapeseed pollen is added to anhydrous ethanol for 14 h, then continuing ultrasonic soaking for 4 h, then rinsing with deionized water; then adding Al (NO) of 0.25 mol / L 3 ) 3 · 9h 2 Ultrasound for 4 h in O solution, then washed with deionized water at 8000 r / min radius and washed 2. After drying at 60 ° C for 12 h, it was placed in a tube furnace at a rate of 5 ° C / min to 500. ° C, keep 80 min under the flow of nitrogen to obtain Al 2 O 3 -C template; rape pollen, absolute ethanol and Al (no 3 ) 3 · 9h 2 The addition ratio of O solution is rape pollen: anhydrous ethanol: Al (NO 3 ) 3 · 9h 2 O Solution = 12g: 400ml: 450ml.

[0045] (2) Al 2 O 3 -C @ nial-LDH Preparation: Mass Mole than Ni (NO 3 ) 2 · 6h 2 O: Al (no 3 ) 3 · 9h 2 O: Urea = 2: 1: 15, weigh Ni (NO 3 ) 2 · 6h 2 O, Al (NO 3 ) 3 · 9...

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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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