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
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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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