A kind of synthesis method of papaverine artificial antigen
A technology of artificial antigen and synthesis method, which is applied in the field of synthesis of papaverine artificial antigen, can solve the problems of long-term use and easy addiction, and achieve the effect of simple synthesis steps
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Embodiment 1
[0034] Example 1 Synthesis of Hapten PAPAM
[0035]
[0036] Weigh papaverine technical drug Ⅰ (1 g, 2.95 mmol) and dissolve it in a solution (10 mL) mixed with acetic acid and water at a volume ratio of 1:1, dilute bromine (0.4 mL) with acetic acid (4 mL) and add dropwise to the above solution , stirred at room temperature for 3.5 h. Add 30 mL of water and extract with dichloromethane (10 mL × 3). The organic layer was saturated with Na 2 S 2 o 3 , 10% NaHCO 3 , washed with water and dried. Compound II (1.1 g, 89.4% yield) was obtained.
[0037] Weigh compound II (600 mg, 1.43 mmol), cuprous iodide (50 mg), copper (100 mg, 1.78 mmol) and suspend in aqueous ammonia (10 mL), and stir overnight at 140°C in a 50 mL sealed tube. The reaction system is an aqueous solution system, which is extracted with ethyl acetate. The organic layer was washed with brine, dried over sodium sulfate and concentrated to give crude product. The crude product was purified by preparative H...
Embodiment 2
[0039] The preparation of embodiment 2 conjugates PAPAM-KLH
[0040] Weigh 4 mg of PAPAM [Mw (PAPAM) is 390.85], dissolve it in 300 μL of anhydrous N,N-dimethylformamide, add 31 μL of 1M HCl (control the molar ratio of PAPAM to hydrochloric acid at 1:3), and incubate at 4 °C Ice bath for 30 minutes, then add 3 μL of 30% sodium nitrite solution (the molar ratio of PAPAM and 30% sodium nitrite solution is controlled at 1:1.3), and react for 1-5 minutes under the condition of pH 2-3 (the color of the activation solution changes from yellow to red as the standard, called A liquid). Take keyhole limpet hemocyanin KLH [Mw (KLH) is 4000000] 1mL (6.8mg / mL), (the molar ratio of PAPAM to KLH is about 6000:1) and add the same volume of KLH sodium carbonate / sodium bicarbonate buffer solution ( (referred to as solution B), under ice bath conditions, add solution A to solution B drop by drop, adjust the pH to 8-9, and react for 4-5 hours under ice bath conditions to obtain the conjugate PA...
Embodiment 3
[0042] The preparation of embodiment 3 conjugates PAPAM-BSA
[0043] Weigh 3 mg of PAPAM, dissolve it with 300 μL of anhydrous N,N-dimethylformamide, add 24 μL of 1M HCL (the molar ratio of PAPAM to hydrochloric acid is controlled at 1:3), keep ice-bathed at 4°C for 30 minutes, and then add 2.5 μL 30% sodium nitrite solution (the molar ratio of PAPAM and 30% sodium nitrite solution is controlled to be 1:1.3), and react for 1-5 minutes under the condition of pH 2-3 (the color of the activation solution changes from yellow to red as the standard, called A solution ). Weigh 10 mg of bovine serum albumin BSA [Mw (BSA) is 67000] (the molar ratio of PAPAM to BSA is about 50:1), dissolve it in 2 mL of sodium carbonate / sodium bicarbonate buffer solution, and dissolve it dropwise under ice bath conditions Add liquid A into liquid B, adjust the pH to 8-9, and react in ice bath for 4-5 hours to obtain the conjugate PAPAM-BSA mixture.
[0044] Pre-treatment of dialysis bag: Take a 10cm ...
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