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
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[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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