Synthesis method of nano material with high magnetic resonance imaging performance and dual-emission wavelength fluorescence imaging performance

Abstract

The invention relates to the field of fluorescence / magnetic resonance quantitative analysis and medical detection, and particularly discloses a synthesis method of a nano material with high magnetic resonance imaging performance and dual-emission wavelength fluorescence imaging performance. The method comprises the following steps: stirring and dissolving sodium hydroxide and diethylene glycol under the protection of nitrogen, and heating to obtain a NaOH / DEG yellow mixed solution; the preparation method comprises the following steps: dissolving ascorbic acid in water and ethanol under magnetic stirring, sequentially adding manganese chloride, polyacrylic acid and diethylene glycol, rapidly heating, adding a NaOH / DEG mixed solution, and transferring into a reaction kettle for reaction to obtain a black viscous solution; the prepared fluorescent nano material is of a sheet structure and has fluorescence and magnetic resonance imaging performance at the same time.

Description

Technical Field

[0001] The present invention discloses a method for synthesizing a nanomaterial having both high magnetic resonance imaging performance and dual-emission wavelength fluorescence imaging performance, which can be applied to fluorescence / magnetic resonance quantitative analysis and detection and the medical field. Background Art

[0002] Magnetic resonance imaging (MRI) is a very important medical imaging technology. It can be used to detect the structure and function of tissues in the human body. It can also be used in the medical field to mark tumor substances in the patient's body to achieve early diagnosis of diseases. However, the existing MRI technology has the disadvantage of slow imaging speed, so other detection methods are needed to supplement MRI technology. Manganese oxide nanomaterials are one of the materials that have attracted much attention in magnetic resonance research due to their better relaxation rate and water solubility. Studies have found that dual-wavelength near-infrared ratiometric fluorescent probes can be combined with MRI technology. By preparing nanomaterials with high MRI performance and dual-emission wavelength fluorescence imaging performance, the dual-mode imaging time is shortened and the technology is better, which can be effectively used for disease analysis in the medical field. Summary of the invention

[0003] The invention uses ascorbic acid, manganese chloride, polyacrylic acid and diethylene glycol as raw materials and prepares nanometer materials with high magnetic resonance imaging performance and dual-emission wavelength fluorescence imaging performance through an inorganic hydrothermal method.

[0004] To achieve the above-mentioned synthesis purpose, the present invention provides a method for synthesizing fluorescent nanomaterials with high magnetic resonance performance, and the specific steps are as follows: (1) Under nitrogen protection, a certain amount of sodium hydroxide and diethylene glycol are stirred until dissolved, heated at 120°C for 1 h, and a NaOH / DEG yellow viscous solution is obtained, which is stored in an oven at 70°C. (2) Under magnetic stirring, 0.5 g of ascorbic acid is completely dissolved in deionized water, ethanol and polyacrylic acid are added, the pH is adjusted to 6 with sodium hydroxide, manganese chloride and diethylene glycol are added, the solution is transparent and viscous, and the temperature is quickly raised to 80°C, the NaOH / DEG solution synthesized in (1) is added, and the pH is adjusted again. The obtained solution is transferred to a reactor, and the reactor is heated at 140°C for 2.5 h, and the product is finally obtained as a black viscous solution.

[0005] Furthermore, the concentration of the NaOH / DEG solution in step (1) is preferably 0.5 mol / L.

[0006] Furthermore, the heating temperature in step (1) is 100°C to 140°C, preferably 120°C.

[0007] Furthermore, the heating time in step (1) is 1 to 2 h, preferably 1 h.

[0008] Furthermore, the pH in step (2) is 6 to 9, preferably pH 6.

[0009] Furthermore, the heating temperature in step (2) is 60-100°C. When the temperature exceeds 100°C, the structure of diethylene glycol changes. The heating temperature is preferably 80°C.

[0010] Furthermore, the calcination time in step (2) is 2 to 4 h, preferably 2.5 h.

[0011] Furthermore, the nanomaterial prepared above is a sheet-like structure.

[0012] The nanomaterial with high magnetic resonance imaging performance and dual-emission wavelength fluorescence imaging performance prepared by the present invention exhibits obvious green fluorescence under 365 nm ultraviolet light irradiation. The fluorescence spectrum shows that it has dual emission wavelengths at 448 nm and 530 nm, a good magnetic resonance signal, and a relaxation rate of 64.95 M -1 ·S -1 . Through transmission electron microscopy, it can be seen that the synthesized material has a flake structure of about 200nm. High-resolution transmission electron microscopy shows that the lattice spacing is 0.22nm, which corresponds to the lattice characteristics of manganese tetraoxide. XPS analysis can prove that the material contains C, O and Mn elements. BRIEF DESCRIPTION OF THE DRAWINGS

[0013] Figure 1 The fluorescence spectrum of the synthesized material.

[0014] Figure 2 This is a magnetic resonance imaging image of the synthesized material.

[0015] Figure 3 Transmission electron microscopy image of the synthesized material.

[0016] Figure 4 XPS graph of the synthesized material. DETAILED DESCRIPTION

[0017] The implementation method of the present invention is explained through specific examples, and researchers involved in the field of this invention can easily understand the advantages and functions of this invention through the contents explained in the specification.

[0018] Example 1: The specific method for preparing nanomaterials with high magnetic resonance imaging performance and dual-emission wavelength fluorescence imaging performance is as follows: (1) Under nitrogen protection, a certain amount of sodium hydroxide and diethylene glycol are stirred until dissolved, heated at 120°C for 1h to obtain a yellow viscous solution of NaOH / DEG, and stored in an oven at 70°C. (2) Under magnetic stirring, 0.5 g of ascorbic acid is completely dissolved in deionized water, ethanol and polyacrylic acid are added, the pH is adjusted to 6 with sodium hydroxide, manganese chloride and diethylene glycol are added, the solution is transparent and viscous, the temperature is quickly raised to 80°C, the NaOH / DEG solution synthesized in step 1 is added, and the pH is adjusted again. The obtained solution is autoclaved at 140°C for 2.5 h, and the final product is a black viscous solution.

[0019] Example 2: TEM, XPS, fluorescence and magnetic resonance imaging were used to characterize the synthesized nanomaterials. Figure 1 As shown, magnetic resonance imaging Figure 2 As shown in the transmission electron microscope Figure 3 As shown, XPS Figure 4 shown.

[0020] Example 3: Evaluation of Fluorescence Imaging Performance and Magnetic Resonance Imaging Performance of Nanomaterials Fluorescence Performance Analysis: Figure 1 As shown in the figure, when the excitation wavelength is 365 nm and the slit width is 5.5 nm, the fluorescence intensity of the synthesized material is 609 at 448 nm and 604 at 530 nm. Figure 2 As shown, the relaxation rate of the synthesized material is 64.95M -1 ·S -1 Through transmission electron microscopy, Figure 3 It can be seen that the synthesized material is a flake structure of about 200 nm. High-resolution transmission electron microscopy shows that the lattice spacing is 0.22 nm, which is the lattice characteristic of manganese tetraoxide. XPS analysis shows Figure 4 , indicating that the material contains C, O and Mn elements.

Claims

1. A method for synthesizing a nanomaterial having both high magnetic resonance imaging performance and dual-emission wavelength fluorescence imaging performance, characterized in that Follow these steps: (1) Under nitrogen protection, take a certain amount of sodium hydroxide and diethylene glycol and stir until dissolved, heat at 120 °C for 1 h to obtain a yellow viscous solution of NaOH / DEG, and store it in an oven at 70 °C; (2) Under magnetic stirring, completely dissolve 0.5 g of ascorbic acid in deionized water, add ethanol and polyacrylic acid, adjust the pH to 6 with sodium hydroxide, add manganese chloride and diethylene glycol, the solution is transparent and viscous, quickly heat it to 80 °C, add the NaOH / DEG solution synthesized in (1), and adjust the pH again. The obtained solution is autoclaved at 140 °C for 2.5 h, and the final product is a black viscous solution.

2. The synthesis method according to claim 1: wherein the concentration of the NaOH / DEG solution in (1) is preferably 0.5 mol / L.

3. The synthesis method according to claim 1: wherein the heating temperature in (1) is 100°C to 140°C, preferably 120°C.

4. The synthesis method according to claim 1: wherein the heating time in (1) is 1 to 2 hours, preferably 1 hour.

5. The synthesis method according to claim 1: wherein the pH in (2) is 6 to 9, preferably pH 6.

6. The synthesis method according to claim 1: (2) the heating temperature is 60 to 100 °C, preferably 80 °C.

7. The synthesis method according to claim 1: wherein the calcination time in (2) is 2 to 4 h, preferably 2.5 h.

8. The synthesis method according to claim 1: the material has a flaky structure.

9. The synthetic method according to claim 1: the relaxation rate of the material is 64.95 M -1 ·S -1 .

10. The synthesis method according to claim 1: the fluorescence emission wavelengths of the material are 448 nm and 530 nm respectively.

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