Melamine dual-mode sensor based on Au-Fe3O4 composite nanoparticles and preparation method thereof
A composite nanoparticle, au-fe3o4 technology, applied in the direction of color/spectral characteristic measurement, material magnetic variables, etc., can solve problems such as urine can not be discharged smoothly, renal tubule obstruction, kidney failure, etc., to shorten the detection cost, selectivity High, strong anti-interference ability effect
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Embodiment 1
[0058] (1) Preparation of specific receptor unit.
[0059] (1.1) Take 1.42 mL of ethyl isothiocyanate (12 mmol) and dissolve it in 100 mL of acetone.
[0060] (1.2) Take 1.022g 2-amino-2-thiazoline (10mmol), dissolve in 200mL CH 2 Cl 2 middle.
[0061] (1.3) Slowly add the solution obtained in step (1.2) dropwise to the solution obtained in step (1.1), heat the obtained mixed solution to 50°C and keep it for 0.5h to obtain a precipitate, filter and wash with acetone. get
[0062]
[0063] (1.4) take 2.00g (10.7mmol) was added to 100mL 18% HCl, and heated to reflux for 6.5h under argon atmosphere. During the reaction, lead acetate test paper was used to detect H 2 S, after the reaction is finished, cool, filter, and dry to obtain a white solid specific receptor unit
[0064]
[0065] specific receptor unit 1 H NMR spectrum as figure 1 shown. figure 1 middle,
[0066] 1 H NMR (DMSO-d 6 ): δ=2.66(m,3,CH 2 S+SH), δ=3.77(m,2,CH 2 N), δ=11.45(s,2,2NH)
[0067] ...
Embodiment 2
[0079] (1) The preparation of the specific receptor unit is the same as in Example 1.
[0080] (2) Au-Fe 3 o 4 The preparation of nanoparticles is the same as in Example 1.
[0081] (3) Based on Au-Fe 3 o 4 Preparation of a dual-mode sensor for the detection of melamine by nanoparticles.
[0082] Take 0.1g NOBF 4 Dissolve in 10mL DMF, ultrasonically dissolve. Take ~50mg Au-Fe 3 o 4 Nanoparticles were dispersed into 10mL of n-hexane to make it evenly mixed. put NOBF 4 The DMF solution was added to the Au-Fe 3 o 4 In the n-hexane solution of the nanoparticles, shake and shake, the nanoparticles enter the DMF solution, and centrifuge with n-hexane and toluene (1:1). Disperse into DMF. Then add 20 mg of specific receptor unit, shake the reaction for 48 hours. Obtaining Au-Fe that modifies the acceptor unit through coordination 3 o 4 DMF solution of nanoparticles, dialyzed for 72 hours.
[0083] The shaking time is 3-5 minutes.
Embodiment 3
[0085] (1) The preparation of the specific receptor unit is the same as in Example 1.
[0086] (2) Au-Fe 3 o 4 The preparation of nanoparticles is the same as in Example 1.
[0087] (3) Based on Au-Fe 3 o 4 Fabrication of a dual-mode sensor for the detection of melamine by nanoparticles
[0088] Take 0.1g NOBF 4 Dissolve in 10mL DMF, ultrasonically dissolve. Take ~100mg Au-Fe 3 o 4 Nanoparticles were dispersed into 10mL of n-hexane to make it evenly mixed. put NOBF 4 The DMF solution was added to the Au-Fe 3 o 4 In the n-hexane solution of the nanoparticles, shake and shake, the nanoparticles enter the DMF solution, and centrifuge with n-hexane and toluene (1:1). Disperse into DMF. Then add 20 mg of specific receptor unit, shake the reaction for 24 hours. Obtaining Au-Fe that modifies the acceptor unit through coordination 3 o 4 DMF solution of nanoparticles, dialyzed for 72 hours.
[0089] The shaking time is 3-5 minutes.
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