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Ursodeoxycholic acid molecular imprinting polymer and its preparing method
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A technology of ursodeoxycholic acid and molecular imprinting, applied in the field of molecularly imprinted polymers of ursodeoxycholic acid
Inactive Publication Date: 2008-12-10
EAST CHINA UNIV OF SCI & TECH
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For example, most molecularly imprinted polymers can only be polymerized and applied in the organic phase, while most natural molecular recognition systems are carried out in aqueous solutions. How to perform molecular imprinting and recognition in aqueous solutions or polar solvents is still an issue. big problem
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Embodiment 1
[0050] Synthesis of ursodeoxycholic acid molecularly imprinted polymer
[0051] 1. Synthesis of Core Layer Polymers
[0052] NaHCO 3 (0.27g, 3.23mmol); Sodium dodecyl sulfate (SDS) (0.261g, 0.903mmol), 148mL of distilled water was added into a 250mL Erlenmeyer flask with stopper, stirred slowly, the water bath was heated to 90°C, and then added Body mixture (MMA 10g, 0.1mol; EDMA 1.04g, 5.14mmol), through N 2 Divide O 2 The post-initiator ammonium persulfate 0.144g was placed in a constant temperature water bath shaker, and the reaction was continued at 250 rpm and 85°C for 12h.
[0053] 2. Synthesis of core-shell molecularly imprinted polymers
[0054] Add water 18mL, SDS (0.1g, 0.346mmol) into a 150mL Erlenmeyer flask with stopper, stir to 70°C, then add the monomer mixture (EDMA 2.02g, 10.18mmol; MAA 0.22g, 2.54mmol or AM 0.18g, 2.54mmol; template molecule UDCA 0.1g; core layer polymer emulsion 11g, N 2 Divide O 2 Finally, add 0.036 g of ammonium persulfate as an ini...
Embodiment 2
[0056]Wash the polymer with HCl with a concentration of 0.05-0.1mol until no bubbles are generated, and then the core-shell molecularly imprinted polymer is sequentially mixed with: I dissolve 1mol ammonium acetate in 40mL ethanol, 25mL acetic acid, 35mL water solution; II acetic acid : ethanol=1: 3 (volume ratio) solution; III methanol solution; IV aqueous solution to wash the obtained polymer. That is, the target product is obtained.
Embodiment 3
[0058] Equilibrium binding experiment example, ursodeoxycholic acid is used as the target substance, dissolved in NaOH aqueous solution with pH 10, the initial concentration is 0.4mg / mL, the volume is 20mL, 100mg molecularly imprinted polymer is added, at 30℃ Under shaking for 24 hours, the adsorption amount of ursodeoxycholic acid reached 43.52 mg / g polymer, and the specific adsorption reached 13.93 mg / g polymer.
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Abstract
The invention discloses ursodesoxycholic acid molecular engram polymer and its preparation method. The molecular engram polymer is formed by stratum nuclear polymer, monomer polymer (1), monomer polymer (2) through random copolymerization. The mass ratio of the monomer polymers (1) and (2) is 1:0.09. The stratum nuclear polymer is formed by monomer polymer (3) and (2) whose mass ratio is 10:1 through emulsion polymerization random copolymerization. The produced molecular engram polymer has 143m2 / g specific surface area, and 43.52mg UDCA / g maximum adsorption capacity. Compared with the existing molecular engram polymer, it can separate ursodesoxycholic acid and chenodeoxycholic acid to gain the high purity former in water phase condition.
Description
technical field [0001] The invention relates to a molecularly imprinted polymer of ursodeoxycholic acid, in particular to a molecularly imprinted polymer for separating high-purity ursodeoxycholic acid from ursodeoxycholic acid and its analogues. Background technique [0002] Ursodeoxycholic acid (3α, 7β-dihydroxy-5β-cholic acid, Ursodeoxycholic acid, UDCA) is an active ingredient in traditional Chinese medicine bear bile, which is widely used in the treatment of gallstones, primary biliary cirrhosis (PBC ) and primary sclerosing cholangitis (PSC), which is the only drug approved by the FDA for the treatment of PBC. [0003] However, since bear bile is a very scarce resource, it is difficult to meet the needs of clinical research and use. Wild bears are national key protected animals, and hunting bear bile is illegal. At present, my country mainly adopts the method of breeding bears and extracting UDCA by drainage from living bodies, but this method has a long cycle, low e...
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