Preparation method and application of fluorine-19 magnetic resonance imaging probe for sulfydryl detection
A magnetic resonance and sulfhydryl technology, applied in the field of nanoprobes, can solve the problems of background interference, poor imaging effect, affecting the diagnosis results, etc., and achieve the effect of easy analysis and processing and high selectivity.
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Embodiment 1
[0025] Synthesis of embodiment 1 polymer P4
[0026] Add the reversible addition-fragmentation chain transfer polymerization (RAFT) chain transfer agent phenyl-(2-hydroxyethyl) thiocarbonate (12.2 mg, 0.1 mM) and polyethylene glycol monomethyl ether in sequence in the shlenk reaction tube Methyl methacrylate (mPEGMA) (500 mg, 1 mM) and 2-((2,4-dinitro-N-(3,3,3-trifluoropropyl)phenylsulfonamide) ethyl methacrylate Ester (AMA-DNBSF) (455 mg, 1 mM), initiator (AIBN) (1.64 mg, 0.01 mM) and 3 mL solvent dimethylformamide (DMF), after three cycles of vacuum / argon, Seal the reaction tube and react in an oil bath at 68-72°C for 24 h. After the reaction, add DMF to dissolve it, put it into a dialysis bag (molecular weight cut-off 3500 Da), dialyze with deionized water for 72 h, and replace it every 12 h Dialysate. Afterwards, lyophilization obtains PEDF polymkeric substance. Utilize proton nuclear magnetic spectrum and fluorine spectrum to carry out characterization to P4 polymkeric s...
Embodiment 2
[0030] Example 2 Preparation method of nanoprobe N4
[0031] Weigh 20 mg of PEDF polymer and directly disperse it in 10 mL of 0.01 M phosphate buffer solution with pH=7.4 under the action of ultrasound (25 °C, 50 Hz, 5 min) to obtain N4 nanoparticles with a concentration of 2 mg / mL. The particle size and shape of nanoparticles were detected by laser particle size analyzer and transmission electron microscope, and the detection results are shown in the attached figure 2 As shown, the nanoparticles prepared in this example have a particle size of 45 nm, a particle size distribution of 0.12, and an obvious core-shell structure.
[0032] According to the preparation method in Example 2, nanoparticles composed of other polymers can be prepared.
Embodiment 3
[0033] Example 3 Nanoprobe N4 19 F NMR signal changes with reaction time
[0034] Take 5 mL of 2 mg / mL N4 nanoprobe solution, add cysteine (Cys) mother solution under argon protection conditions, so that the final concentration of Cys is 5 mg / mL, at the set time point, take 300 µL, add 100 µL heavy water for field lock, use nuclear magnetic resonance to analyze the 19 F NMR signal was detected. as attached image 3 As shown, the nanoprobe can respond rapidly to sulfhydryl groups, in the presence of cysteine, within 30 min 19 The F NMR signal can be significantly enhanced.
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