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Preparation method of bifunctional contrast agent based on up-conversion material and gadolinium chelate

A conversion material and dual-function technology, applied in the field of nano-biomedical materials, can solve the problems of contrast agent signal confusion, magnetic resonance signal reduction, etc., achieve good physical and chemical stability, meet production and application, and simple process effects

Inactive Publication Date: 2014-02-12
SHANGHAI NAT ENG RES CENT FORNANOTECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, superparamagnetic iron oxide is easy to cause the decrease of magnetic resonance signal, and the confusion of contrast agent signal and surrounding tissue signal
While most of the commercially used contrast agents are gadolinium chelates, such as gadopentetate meglumine (Gd-DTPA), few studies have been done on dual-function contrast agents, especially the combination of up-conversion materials and gadolinium chelates. The dual function contrast agent has not been reported

Method used

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  • Preparation method of bifunctional contrast agent based on up-conversion material and gadolinium chelate
  • Preparation method of bifunctional contrast agent based on up-conversion material and gadolinium chelate
  • Preparation method of bifunctional contrast agent based on up-conversion material and gadolinium chelate

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Experimental program
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Effect test

Embodiment 1

[0023] 1. Add 200 mg NaYF 4 :Yb 3+ ,Er 3+ (0.97 mmol) was dispersed in 40 mL ethanol solution, after ultrasonication for 40 minutes, 10 mL, 15% NH 3 ·H 2 O solution. Under stirring conditions, add 0.097 mmol TEOS and 0.97 mmol APTES, and stir for 1 hour to obtain solution a.

[0024] 2. Add 0.97 mmol DTPA to 50 mL DMSO, add 0.97 mmol NHS and EDC after complete dissolution, and stir at room temperature for 24 hours to obtain solution b.

[0025] 3. After mixing and stirring the two solutions for 24 hours, add 0.97 mmol Gd(NO 3 ) 3 ·6H 2 O, after stirring for 24 hours, the product was filtered, washed several times with absolute ethanol, and vacuum-dried to obtain NaYF 4 :Yb 3+ ,Er 3+ / Gd-DTPA as a dual function contrast agent.

[0026] figure 1 For the prepared NaYF 4 :Yb 3+ ,Er 3+ / Gd-DTPA dual-functional contrast agent up-conversion fluorescence spectrum. The fluorescence intensity at 540 nm is 5.5×10 5 . In addition, the signal intensity in MRI was 411.22. ...

Embodiment 2

[0028] 1. Add 130 mg NaGdF 4 :Yb 3+ ,Er 3+ (0.5 mmol) was dispersed in 30 mL ethanol solution, after ultrasonication for 40 minutes, 5 mL, 15% NH 3 ·H 2 O solution. Under stirring conditions, add 0.1 mmol TEOS and 1 mmol APTES, and stir for 2 hours to obtain solution a.

[0029]2. Add 1 mmol DOTA to 50 mL DMSO, add 1 mmol NHS and EDC after complete dissolution, and stir at room temperature for 24 hours to obtain solution b.

[0030] 3. After mixing the two solutions for 24 hours, add 1 mmol GdCl 3 ·6H 2 O, after stirring for 24 hours, the product was filtered, washed several times with absolute ethanol, and vacuum-dried to obtain NaGdF 4 :Yb 3+ ,Er 3+ / Gd-DOTA dual function contrast agent.

[0031] figure 2 For the prepared NaGdF 4 :Yb 3+ ,Er 3+ / Gd-DOTA dual-functional contrast agent upconversion fluorescence spectrum. The fluorescence intensity at 540 nm is 3.5×10 5 . In addition, the signal intensity in MRI was 870.32.

Embodiment 3

[0033] 1. Mix 65 mg NaYF 4 :Gd 3+ ,Yb 3+ ,Er 3+ (0.29 mmol) dispersed in 30 mL ethanol solution, after ultrasonication for 40 minutes, add 1 mL, 15% NH 3 ·H 2 O solution. Under stirring conditions, add 0.087 mmol TEOS and 0.435 mmol APTES, and stir for 2 hours to obtain solution a.

[0034] 2. Add 0.435 mmol DTPA to 50 mL DMSO, add 0.435 mmol NHS and EDC after complete dissolution, and stir at room temperature for 24 hours to obtain solution b.

[0035] 3. After mixing and stirring the two solutions for 24 hours, add 0.435 mmol Gd(OOCCH 3 ) 3 ·xH 2 O, after stirring for 24 hours, the product was filtered, washed several times with absolute ethanol, and vacuum-dried to obtain NaYF 4 :Gd 3+ ,Yb 3+ ,Er 3+ / Gd-DTPA dual function contrast agent.

[0036] image 3 For the prepared NaYF 4 :Gd 3+ ,Yb 3+ ,Er 3+ / Gd-DTPA dual-functional contrast agent up-conversion fluorescence spectrum. The fluorescence intensity at 540 nm is 3.7×10 5 . In addition, the signal inte...

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Abstract

The invention relates to a preparation method of a bifunctional contrast agent based on an up-conversion material and a gadolinium chelate. The preparation method comprises following steps: preparing surface-aminated silica by utilization of the combined action of tetraethoxysilane (TEOS) and (3-aminopropyl)trimethoxysilane (APTES) and by utilization of an up-conversion nano material as a substrate; coupling a chelate to the surface-aminated silica by utilization of 1-ethyl-3-(3-dimethylaminopropyl)-carbodiimide (EDC) and N-hydroxysuccinimide (NHS) as coupling agents; and finally reacting with a gadolinium salt to obtain the gadolinium chelate, and therefore the bifunctional contrast agent combined the up-conversion material and the gadolinium chelate is obtained. The raw materials used in the preparation method have high biosecurity, and some of the raw materials are already commercial products. The preparation method has simple technology and strong operationality, and can satisfy production and applications. The bifunctional contrast agent prepared has good physical and chemical stability, luminescence performance and magnetic resonance imaging performance.

Description

technical field [0001] The invention relates to a contrast agent and a preparation method thereof, in particular to a dual-function contrast agent based on an up-conversion material gadolinium chelate and a preparation method thereof, belonging to the field of nanobiological medical materials. Background technique [0002] In today's clinical diagnosis of cancer, magnetic resonance imaging (MRI) technology has become one of the most powerful detection means. This technology has been widely used in the examination of human tissues or organs, especially for the early diagnosis of tumors, which can greatly improve the success rate of treatment. However, MRI is not very sensitive when used to monitor small tissue lesions, molecular activities, or cellular activities. Therefore, in order to ensure the sensitivity and accuracy of clinical diagnosis, more than 45% of MRI examinations need to use contrast agents to improve image contrast. In recent years, with the development of n...

Claims

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Application Information

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IPC IPC(8): A61K49/00A61K49/06
Inventor 朱君路青周涓何丹农
Owner SHANGHAI NAT ENG RES CENT FORNANOTECH
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