A kind of tumor targeting thermosensitive prodrug and its preparation method and application
A tumor-targeted, anti-tumor drug technology, applied in the field of biomedicine, can solve problems such as intractability and stability, and achieve the effects of reducing toxic side effects, increasing concentration, and overcoming insoluble in water
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Embodiment 1
[0055] (1) Accurately weigh 0.00028g (0.001mmol) 4,4'-azobis(4-cyanovaleric acid), dissolve it in 0.1mL dimethyl sulfoxide, then add 0.00012g (0.001mmol) NHS React with 0.00019g (0.001mmol) EDC and 1μL pyridine at room temperature for 0.5h under nitrogen protection.
[0056] (2) Add 0.00054 g (0.001 mmol) of doxorubicin hydrochloride to the above reaction solution, and react for 0.5 h at room temperature under nitrogen protection (the carboxyl group at one end of 4,4'-azobis(4-cyanovaleric acid) and Amino reaction of doxorubicin hydrochloride).
[0057] (3) The product was purified by silica gel column chromatography and dried in vacuum.
[0058] (4) Dissolve the dried product in step (3) in 0.1 mL dimethyl sulfoxide, then add 0.00012 g (0.001 mmol) NHS, 0.00019 g (0.001 mmol) EDC and 1 μL pyridine, and react at room temperature for 0.5 h under nitrogen protection get a mixed solution.
[0059] (5) Dissolve 0.0067g of human serum albumin in 1mL of PBS, add the above mixed s...
Embodiment 2
[0062] (1) Accurately weigh 2.8g (10mmol) 4,4'-azobis(4-cyanovaleric acid), dissolve it in 100mL dimethyl sulfoxide, then add 1.2g (10mmol) NHS and 1.9g (10 mmol) EDC and 200 μL pyridine, reacted at room temperature for 48 h under nitrogen protection.
[0063] (2) Add 5.4g (10mmol) doxorubicin hydrochloride to the above reaction solution, and react for 48h at room temperature under the protection of nitrogen (4,4'- azobis(4-cyanovaleric acid) at one end of the carboxyl group and doxorubicin hydrochloride aminomycin reaction).
[0064] (3) The product was purified by silica gel column chromatography and dried in vacuum.
[0065] (4) Dissolve the dried product in step (3) in 100 mL of dimethyl sulfoxide, then add 1.2 g (10 mmol) of NHS, 1.9 g (10 mmol) of EDC and 200 μL of pyridine, and react at room temperature for 48 h under nitrogen protection to obtain a mixed solution.
[0066] (5) Dissolve 0.67g of human serum albumin in 1000mL of PBS, add the above mixed solution to it,...
Embodiment 3
[0069] (1) Accurately weigh 0.28g (1mmol) 4,4'-azobis(4-cyanovaleric acid), dissolve it in 100mL dimethyl sulfoxide, then add 0.24g (2mmol) NHS and 0.19g (1 mmol) EDC and 20 μL pyridine were reacted at room temperature for 24 h under nitrogen protection.
[0070] (2) Add 0.54g (1mmol) doxorubicin hydrochloride to the appealing reaction solution, and react for 24 hours at room temperature under the protection of nitrogen (4,4'-azobis(4-cyanovaleric acid) at one end of the carboxyl group and doxorubicin hydrochloride aminomycin reaction).
[0071] (3) The product was purified by silica gel column chromatography and dried in vacuum.
[0072] (4) Dissolve the product in 100 mL dimethyl sulfoxide, add 0.12 g (1 mmol) NHS, 0.19 g (1 mmol) EDC and 20 μL pyridine, and react at room temperature for 24 h under nitrogen protection to obtain a mixed solution.
[0073] (5) 6.7g of human serum albumin was dissolved in 100mL of PBS, and the above mixed solution was added thereto, and the r...
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