MOFs type molecularly imprinted polymer, preparation method thereof and pesticide residue fluorescence detection method
A technology of molecular imprinting and polymers, applied in fluorescence/phosphorescence, chemical instruments and methods, analytical materials, etc., can solve the problems of long cycle, single type of detection, high false positive and false negative rate of detection, etc.
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Embodiment 1
[0091] This embodiment provides a method for fluorescent detection of pesticide residues, which includes the following steps:
[0092] S1: FeCl 3 ·6H 2 O, FeCl 2 4H 2 O and high-purity water are mixed according to a certain volume ratio and placed in a 250mL three-necked bottle for ultrasonic dispersion for 0.5h; magnetically stirred for 0.5-1h at a temperature of 50-100°C, and a certain volume of NH with a mass fraction of 28% is added 3 ·H 2 O, continue to react for 1 h under the protection of nitrogen; after magnetic separation, use absolute ethanol and pure water to alternately wash several times, and vacuum dry the obtained magnetic nanoparticles Fe 3 o 4 NPs; among them, FeCl 3 ·6H 2 O, FeCl 2 4H 2 The consumption ratio of O, high-purity water and ammoniacal liquor is 0.5g:0.15g:200mL:5mL; The used dehydrated alcohol and high-purity water volume ratio of each washing are 10mL:15-30mL;
[0093] S2: The magnetic nanoparticles Fe 3 o 4 Add NPs and high-purity wa...
Embodiment 2
[0099] It differs from Example 1 in that:
[0100] In step S1, FeCl 3 ·6H 2 O, FeCl 2 4H2 The consumption ratio of O, high-purity water and ammoniacal liquor is 0.6g:0.35g:200mL:10mL; The used dehydrated alcohol and high-purity water volume ratio of each washing are 10mL:25mL.
[0101] In step S2, the magnetic nanoparticles Fe 3 o 4 NPs, high-purity water, FeCl 3 ·6H 2 O, FeCl 3 ·6H 2 O aqueous solution, H 2 The dosage ratio of BDC and DMF is 0.2g:200mL:0.45g:80mL:0.174g:50mL.
[0102] In step S3, the magnetic MOFs composite Fe 3 o 4 - The dosages of MIL-Fe, methanol, acetamiprid molar mass, clothianidin molar mass, APTES, TEOS and acetic acid solution are 0.4g:10mL:0.15mM:0.15mM:0.2mL:2mL, respectively.
Embodiment 3
[0104] It differs from Example 1 in that:
[0105] In step S1, FeCl 3 ·6H 2 O, FeCl 2 4H 2 The consumption ratio of O, high-purity water and ammoniacal liquor is 0.75g:0.45g:200mL:15mL; The used dehydrated alcohol and high-purity water volume ratio of each washing are 10mL:30mL.
[0106] In step S2, the magnetic nanoparticles Fe 3 o 4 NPs, high-purity water, FeCl 3 ·6H 2 O, FeCl 3 ·6H 2 O aqueous solution, H 2 The dosage ratio of BDC and DMF is 0.3g:200mL:0.9g:120mL:0.498g:100mL.
[0107] In step S3, the magnetic MOFs composite Fe 3 o 4 - The dosages of MIL-Fe, methanol, acetamiprid molar mass, clothianidin molar mass, APTES, TEOS and acetic acid solution are 0.5g:10mL:0.2mM:0.2mM:0.4mL:4mL, respectively.
[0108] In conjunction with above-mentioned embodiment and accompanying drawing, refer to figure 1 , MIL-Fe is a blocky three-dimensional highly cross-linked polymer with a non-smooth surface and irregular corners; when Fe 3 o 4 Fe prepared after doping modif...
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