CN108743978B - Preparation method and application of gold @ gadolinium-based coordination polymer nanocomposite - Google Patents
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Abstract
The invention relates to a method for converting GdCP with up-conversion luminescence property into light by using a one-pot method: yb of3+，Er3+(GdCP) nanoparticles are compounded with gold nanoparticles (AuNPs) to prepare gold @ gadolinium-based coordination polymer core-shell structure multifunctional nanocomposite (Au @ GdCP), and the gold @ gadolinium-based coordination polymer core-shell structure multifunctional nanocomposite is applied to T1Weighted magnetic resonance (T)1-MRI) imaging. In the invention, the gold nanoparticles have strong plasma resonance effect (LRET), so that the magnetic field intensity at the periphery of GdCP can be increased, and the effects of improving contrast relaxation rate and MRI imaging effect are achieved. The hydrothermal synthesis method adopted by the invention has the advantages of simple synthesis path, easy regulation and control, greenness, high efficiency and the like. The Au @ GdCP has good biocompatibility, so that the application of the Au @ GdCP in magnetic contrast imaging can be further considered, and a new way is provided for obtaining a high-efficiency magnetic resonance contrast material.
Description
Technical Field
The invention relates to the field of rare earth up-conversion nano materials, in particular to a gold @ gadolinium-based coordination polymer nano composite material, and a method and application thereof.
Background
Magnetic Resonance Imaging (MRI) is a non-radiative imaging technique, and is an effective clinical diagnosis mode for imaging body tissue structures and observing pathological tissue structures including solid tumors. It functions as contrast imaging by altering the longitudinal and transverse relaxation times of the aqueous environment in vivo. This has the advantage that no ionizing radiation is required and that a three-dimensional image with high spatial resolution and high contrast can be provided.
The rare earth Up-conversion nano material (UCNPs) is excited by continuous visible light, and can display a unique, high-energy and narrow emission spectrum through an anti-Stokes process, multi-photon absorption or energy transfer. Based on this light-emitting characteristic, it is particularly suitable for the field of biomedicine. The reasons are: the luminescence is not influenced by the autofluorescence of the biological material; the exciting light has strong penetrating power to the tissue, can penetrate into the tissue and has small toxicity to the tissue. Compared with the traditional up-conversion nano material, the material has the characteristics of good optical stability and chemical stability, high quantum yield, large anti-Stokes displacement, multiple sharp emission peaks and the like. The application range can be from the technical field of high-resolution biological imaging and detection photoelectronics. Therefore, the magnetic resonance imaging material is good.
At present, many nano-carriers are available for magnetic contrast imaging, such as noble metal nanoparticles, silica, rare earth nanomaterials [ nanoscales, 2016,8:878-]. Among the rare earth UCNPs, rare earth gadolinium ion (Gd)3+) The magnetic contrast agent with seven unpaired electrons and larger magnetic moment is the most widely clinically applied magnetic contrast agent at present, but the low relaxation rate of Gd and certain nephrotoxicity influence the application of the magnetic contrast agent, so that the development of the magnetic contrast agent with low toxicity and strong relaxation performance is very significant. There have been many studies on the improvement of contrast relaxation rate and the reduction of toxicity. Such as surface modification of Gd contrast agent, so as to achieve the purposes of improving relaxation rate and reducing toxicity. Literature [ Biomaterials, 2017,121:109-120]The carbon quantum dots are doped in Gd contrast agents (Gd-doped CDs) by utilizing good optical characteristics and low toxicity of the carbon quantum dots, and have good MRI living body imaging effect and good biocompatibility. Literature [ adv.mater, 2017,29(35)]A multifunctional diagnosis and treatment integrated DOX-loaded gadolinium-based contrast material (CDPGM) is synthesized by taking PDA as a template, and the result shows that the DOX-loaded gadolinium-based contrast material has good biocompatibility, strong near infrared absorption and high relaxation rate. Simultaneously, gold nanoparticles with Surface Enhanced Raman Scattering (SERS) and doped Gd2O3The silicon dioxide nano material is combined and applied to a contrast experiment, and can also obtain a high-efficiency MRI contrast agent material [ Spectrochim Acta A.,2017,181: 218-225-]. Gd (III) is introduced into Carbon Quantum Dots (CQD), so that fluorescence/magnetic resonance dual-mode imaging can be realized, and a magnetic contrast imaging signal (J.Mater.chem.B, 2017,5: 92-101) is enhanced]. The unseen gold nanoparticles are combined with the rare earth coordination polymer up-conversion nanomaterial to be applied to enhancing a magnetic resonance imaging signal.
Gd3+The good biomedical imaging materials of the composites, but they have low relaxivity and potential biotoxicity, which requires modification to achieve Gd reduction3+The relaxation rate can be enhanced, and the imaging effect is improved.
Disclosure of Invention
The invention aims to provide a preparation method and application of a gold @ gadolinium-based coordination polymer nanocomposite. According to the invention, the gold nanoparticles and the gadolinium-based nanocomposite material are effectively combined, and the existence of the gold nanoparticles in the product is expected to improve the contrast relaxation rate and the MRI imaging effect on the magnetic field intensity at the periphery of the gadolinium-based nanocomposite material, so that a new thought and a new method are provided for developing the magnetic contrast material with low toxicity and strong relaxation performance.
According to the invention, GdCP nanoparticles with up-conversion luminescence performance and gold nanoparticles are effectively combined to form a composite material Au @ GdCP, and the composite material Au @ GdCP is applied to T1-in MRI imaging. Compared with GdCP, Au @ GdCP has the capacity of enhancing a magnetic contrast signal and presents good biocompatibility.
Gold @ gadolinium-based coordination polymer nanocompositeA preparation method of a material (Au @ GdCP) is characterized by comprising the following steps: with HAuCl4·3H2Gold nanoparticles (Au NPs) synthesized by taking O as raw material and allantoin (C) as organic ligand4H6N4O3) For binding, Gd is used3+As a central metal ion, and Yb3+、Er3+And (3) synthesizing the gold @ gadolinium-based coordination polymer nanocomposite by using a seed-mediated method for doping ions. The method comprises the following specific steps:
(1) dissolving allantoin in solvent, respectively injecting boiled sodium citrate solution and gold nanoparticle (AuNPs) solution, and mixing;
(2) gd (NO)3)3、Yb(NO3)3、Er(NO3)3The solution is mixed with the solution and transferred into a reaction kettle to react at the temperature of 140-180 ℃;
(3) and after the reaction is completed, cooling, centrifugally separating out solid substances, washing and drying the solid substances to obtain the gold @ gadolinium-based coordination polymer nanocomposite.
In the method, all solvents used are water, and deionized water is preferred.
In the method, the concentration of the boiled sodium citrate solution is 0.035 mol/L.
In the method, the Gd (NO) is3)3、Gd(NO3)3And Gd (NO)3)3In a molar ratio of 6:3: 1.
In the method, the Gd (NO) is3)3Gd (NO) in an aqueous solution of3)3And Gd (NO)3)3The concentration of the aqueous solution (2) was 0.02 mol/L.
In the method, the reaction kettle is a polytetrafluoroethylene lining reaction kettle.
According to the method, the gold @ gadolinium-based coordination polymer nanocomposite with the average particle size of 150nm can be obtained, and the transverse relaxation rate and the longitudinal relaxation rate of Au @ GdCP are r respectively1＝5.72，r227.69. AuNPs are introduced into GdCP nano-particles to formAu @ GdCP has good biocompatibility and can ensure T1MRI imaging signal enhancement. Due to the introduction of AuNPs, Au @ GdCP can be used in-vitro magnetic resonance imaging and can also enhance magnetic resonance imaging signals.
The invention has the beneficial effects that: the average particle size of the synthesized Au @ GdCP particles is 150nm, and the condition of biomedical application is met. AuNPs are introduced into GdCP nanoparticles, and formed Au @ GdCP has good biocompatibility and can enhance T1-MRI imaging signals. Therefore, the material has potential application value in the fields of biomedicine, optical images and the like. The used solvents are deionized water, and the synthesis method is simple, green and efficient.
Drawings
Fig. 1 is SEM and TEM images of GdCP and Au @ GdCP nanocomposites.
FIG. 2 is a graph of the results of in vitro biocompatibility evaluations of GdCP and Au @ GdCP nanocomposites.
FIG. 3 shows relaxation information and enhanced T of GdCP and Au @ GdCP nanocomposites1MRI imaging signal maps.
FIG. 4 is a graph of upconversion luminescence spectra for GdCP and Au @ GdCP.
Detailed Description
Firstly, dissolving 0.1mmol of allantoin in 20mL of water, heating to dissolve, and cooling to room temperature; secondly, respectively injecting boiled sodium citrate solution (1mL, 0.035mol/L) and gold nanoparticle solution (2mL), uniformly mixing, and magnetically stirring for 5 minutes at room temperature; finally, a certain concentration of Gd (NO) is taken3)3、Yb(NO3)3、Er(NO3)3Was mixed with the above solution, magnetically stirred at room temperature for 5 minutes, and placed in a 50mL Teflon-lined reaction vessel at 160 ℃ for 15 hours. After the reaction was complete, it was cooled to room temperature, centrifuged, and the product was washed 3 times with deionized water and ethanol. Drying in a vacuum oven at 60 ℃ for 12 hours gave a purple product, sample designated Au @ GdCP.
Fig. 1 is SEM and TEM images of GdCP and Au @ GdCP. As can be seen from FIGS. 1a-c, GdCP is spherical particles, the particles are uniformly distributed, the monodispersity is good, the particle diameter is about 300nm, and the spherical particles are hollow. FIG. 1d-f are SEM and TEM images of Au @ GdCP after complexing, the particle size of Au @ GdCP is slightly smaller than that of GdCP, about 150nm, and it can be observed that Au @ GdCP is a spherical particle. The periphery of the Au @ GdCP is the GdCP nano composite material, and a plurality of Au nano particles are wrapped inside the Au @ GdCP nano composite material. The magnification TEM (fig. 1f) shows that the Au @ GdCP nanosphere outer thickness is about 50 nm. The Au @ GdCP has a proper particle size, and meets the application requirements of biomedicine.
Good biocompatibility is a prerequisite for the application of nanomaterials in the field of biomedicine. Fig. 2 is a graph showing the results of evaluating cytotoxicity of Au @ GdCP under the MTT method, and at the same time, shows the results of testing GdCP as a control under the same conditions. As can be seen from the figure, the viability of HeLa cells cultured with Au @ GdCP and GdCP gradually decreased with increasing concentration. Compared with the influence of Au @ GdCP and GdCP on cells, the influence of the AuNPs on the cell survival rate is small. When the concentration of Au @ GdCP and GdCP reaches 1.0mg/mL, the cell survival rate still keeps more than 80%, namely 80% and 82.2%, respectively, which shows that Au @ GdCP has low toxicity and good biocompatibility under the conditions of no illumination and dark field and meets the basic requirements of medical and pharmaceutical use.
FIG. 3 shows relaxation information and T for GdCP and Au @ GdCP nanocomposites1-weighting the magnetic resonance imaging signal map (T)1-MRI). In vitro magnetic resonance imaging results show that the longitudinal relaxation time and the transverse relaxation time are in good linear relation with the increase of GdCP and Au @ GdCP concentrations. T is1In the MRI imaging signal map, both exhibit the phenomenon that the magnetic resonance imaging signal becomes gradually brighter and the pseudo-color map becomes gradually redder.
Their relaxivity is: GdCP, r1＝0.66，r2＝3.45；Au@GdCP，r1＝5.72，r227.69. The longitudinal and transverse relaxivity of Au @ GdCP is 8.7 times and 8.0 times of the longitudinal and transverse relaxivity of GdCP respectively. Furthermore, as the concentration increases, T of GdCP increases1The MRI signal appearance is gradually enhanced, but T1Less contrast improvement in weighted magnetic resonance imaging, Au @ GdCP and T1Weighting magnetic resonance imaging contrast with concentrationIncrease, greater variation, T1The weighted imaging signal exhibits a good enhancement effect.
Therefore, the magnetic contrast effect of Au @ GdCP is much better than that of GdCP. The existence of AuNPs greatly enhances the contrast effect and plays a role in enhancing imaging signals, and meanwhile, the transverse relaxation rate of the AuNPs and the longitudinal relaxation rate of the AuNPs are higher than that of the AuNPs, so that the material is expected to realize T1-T2Dual mode magnetic resonance imaging.
FIG. 4 is a graph of upconversion luminescence spectra of samples GdCP and Au @ GdCP under excitation of a 980nm laser. As can be seen in the figure, both exhibit Er3+Are respectively located at 525nm, 545nm and 655nm, which correspond to2H11/2→4H15/2、4S3/2→4I15/2、4F9/2→4H15/2Energy level transition of (2). Wherein, the green light emission process is as follows:4H15/2→2I11/2→4F7/2→2H11/2→4S3/2，4H15/2→4I11/2→4F13/2→4H9/2the red light is emitted in the process of4H15/2→4I11/2→4F13/2→4F9/2. When AuNPs are wrapped, the up-conversion luminescence intensity is obviously enhanced.
Research shows that the Au NPs in the up-conversion material can adjust the luminescence property of the up-conversion material, and the enhancement of the luminescence property by wrapping the gold nanoparticles mainly comes from the surface plasma effect of the Au NPs. The plasma action causes a local crystal field enhancement resulting in an increase in the excitation light flux. Meanwhile, the coupling effect of the plasmon resonance and the up-conversion emission can also improve the efficiency of the emitted light. In the invention, the plasma resonance peak of the gold nanoparticles is 527nm, and the position of the peak is very close to the position of green light emission in an up-conversion spectrum. Thus, more green emission is absorbed.
The theoretical calculation of electromagnetism suggests that the surface plasma resonance of the metal particles can transfer energyEfficiency improvement of 104-105. Moreover, the distance of energy transmission can reach 70-100nm, which is more typical than
The distance is about 10 times longer. Therefore, the Au NPs have the effect of enhancing fluorescence in Au @ GdCP.
Claims (9)
1. The preparation method of the gold @ gadolinium-based coordination polymer nanocomposite is characterized by comprising the step of preparing HAuCl4·3H2Gold nanoparticles (Au NPs) synthesized by taking O as raw material are combined with allantoin serving as organic ligand, and Gd is used3+As a central metal ion, and Yb3+And Er3+And (3) synthesizing the gold @ gadolinium-based coordination polymer nanocomposite by using a seed-mediated method for doping ions.
2. The method according to claim 1, characterized by the following specific steps:
(1) dissolving allantoin in a solvent, respectively injecting a boiled sodium citrate solution and a gold nanoparticle solution, and uniformly mixing;
(2) gd (NO)3)3、Yb (NO3)3、Er (NO3)3The solution is mixed with the solution and transferred into a reaction kettle to react at the temperature of 140-180 ℃;
(3) and after the reaction is completed, cooling, centrifugally separating out solid substances, washing and drying the solid substances to obtain the gold @ gadolinium-based coordination polymer nanocomposite.
3. The process according to claim 2, wherein the solvent used is water.
4. The method of claim 2, wherein the concentration of the boiled sodium citrate solution is 0.035 mol/L.
5. The method of claim 2, wherein the first and second light sources are selected from the group consisting of,characterized in that said Gd (NO)3)3Aqueous solution of Yb (NO)3)3And Er (NO)3)3The concentration of the aqueous solution of (3) was 0.02 mol/L.
6. The method of claim 2, wherein the reaction vessel is a polytetrafluoroethylene-lined reaction vessel.
7. A gold @ gadolinium-based coordination polymer nanocomposite, characterized in that the gold @ gadolinium-based coordination polymer nanocomposite is obtained by the method according to any one of claims 1 to 6.
8. The use of gold @ gadolinium-based coordination polymer nanocomposite as defined in claim 7, wherein said gold @ gadolinium-based coordination polymer nanocomposite is used in the preparation of a contrast agent.
9. The use of claim 8, wherein said gold @ gadolinium-based coordination polymer nanocomposite is used in the preparation of a contrast agent for magnetic resonance imaging.
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| CN106893111A (en) * | 2017-03-30 | 2017-06-27 | 江西师范大学 | Method for preparing gold @ rare earth coordination polymer nanoparticles |
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| CN104258422A (en) * | 2014-09-15 | 2015-01-07 | 东华大学 | Method for preparing CT/MR dual-mode imaging contrast agent based on hyperbranched polyethyleneimine molecules |
| CN106893111A (en) * | 2017-03-30 | 2017-06-27 | 江西师范大学 | Method for preparing gold @ rare earth coordination polymer nanoparticles |
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| Multifunctional Coordination Polymer Nanoparticles Based on Allantoin: Single Peak Upconversion Emission, Drug Delivery and Cytotoxicity Study;Shengliang Zhong et al;《J Inorg Organomet Polym》;20160406;第26卷;第527-535页 * |
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