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Preparation method for chiral separation benzenesulfonic acid amlodipine molecularly imprinted membrane

A technology of amlodipine besylate and ammonium chloride besylate, which is applied in the field of preparation of chiral separation amlodipine besylate molecularly imprinted membrane, can solve problems such as difficult industrial production, and achieve simple preparation method and good adsorption and separation function, the effect of low equipment requirements

Inactive Publication Date: 2015-06-24
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] There have been related reports on enantiomeric separation methods of amlodipine, such as extraction resolution, crystallization, kinetic resolution, chromatographic resolution, membrane separation, capillary electrophoresis, and chiral column resolution. and molecular imprinting techniques; these methods are mostly small-scale splitting methods in the laboratory, and it is difficult to scale up to realize industrial production

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  • Preparation method for chiral separation benzenesulfonic acid amlodipine molecularly imprinted membrane
  • Preparation method for chiral separation benzenesulfonic acid amlodipine molecularly imprinted membrane
  • Preparation method for chiral separation benzenesulfonic acid amlodipine molecularly imprinted membrane

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Embodiment 1

[0027] The specific steps of the preparation method of the chiral separation amlodipine besylate molecularly imprinted membrane of the present invention are as follows:

[0028] (1) Prepare a NaOH aqueous solution with a concentration of 0.5mol / L, then put the PVDF hollow fiber membrane into it, soak it at 40°C for 3 hours, take out the residual alkali solution and dry it naturally, and soak the membrane in anhydrous methanol for later use;

[0029] (2) The template molecule S-amlodipine besylate is dissolved in chloroform, the molar volume ratio of S-amlodipine besylate and chloroform is 2:10 (mmol:mL), and then ultrasonically The template molecule is completely dissolved, add the functional monomer 4-vinylpyridine, the molar ratio of 4-vinylpyridine to S-amlodipine besylate is 5:2, leave it at room temperature for 2h, then add the cross-linking agent ethylene glycol Dimethacrylate and initiator azobisisobutyronitrile, the molar ratio of ethylene glycol dimethacrylate and azo...

Embodiment 2

[0032] The specific steps of the preparation method of the chiral separation amlodipine besylate molecularly imprinted membrane of the present invention are as follows:

[0033] (1) Prepare a NaOH aqueous solution with a concentration of 2mol / L, then put the PVDF hollow fiber membrane into it, soak it at 60°C for 1 hour, take out the residual alkali solution and dry it naturally, and soak the membrane in anhydrous methanol for use;

[0034] (2) The template molecule S-amlodipine besylate is dissolved in chloroform, the molar volume ratio of S-amlodipine besylate and chloroform is 2:30 (mmol:mL), and then ultrasonically The template molecules are completely dissolved, add the functional monomer 4-vinylpyridine, the molar ratio of 4-vinylpyridine to S-amlodipine besylate is 10:2, leave it at room temperature for 6h, and then add the cross-linking agent ethylene glycol Dimethacrylate and initiator azobisisobutyronitrile, the molar ratio of ethylene glycol dimethacrylate and azobi...

Embodiment 3

[0037] (1) Surface pretreatment of PVDF membrane: configure 1.0mol / L NaOH aqueous solution, put the PVDF hollow fiber membrane into it and soak it at 50°C for 2 hours, take out the residual alkali solution and dry it naturally, and soak the membrane in anhydrous methanol stand-by;

[0038] (2) Dissolve 2 mmol of template molecule S-amlodipine besylate in 20 mL of chloroform, sonicate for 5 minutes to completely dissolve the template molecule, add 8 mmol of functional monomer 4-vinylpyridine, and place at room temperature for 4 hours. After the functional monomers and template molecules are sufficiently pre-polymerized, add 40 mmol of ethylene glycol dimethacrylate as a crosslinking agent and 0.88 mmol of azobisisobutyronitrile as an initiator, and mix them uniformly by ultrasonic vibration for 5 minutes to obtain a pre-polymerization solution.

[0039] (3) The PVDF hollow fiber membrane treated above was immersed in the pre-polymerization solution for 5 minutes, taken out to d...

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Abstract

The invention discloses a preparation method for a chiral separation benzenesulfonic acid amlodipine molecularly imprinted membrane. The method comprises the following steps of mixing S-benzenesulfonic acid amlodipine and 4-vinylpyridine into trichloromethane to obtain a pre-polymer system; adding ethylene glycol dimethacrylate and azodiisobutyronitrile to obtain a polymeric system; soaking a PVDF film into the polymeric system, and then transferring the PVDF film subjected to soaking treatment into a vacuum system to be subjected to polymeric reaction; washing the PVDF film after reaction with acetic acid and methyl alcohol, and preparing the S-benzenesulfonic acid amlodipine molecularly imprinted hollow fiber membrane. The molecularly imprinted membrane takes the PVDF membrane which is good in performance and low in cost in market as a basal membrane, has the advantage of selectivity of molecular imprinting technology and the advantage of simplicity and easiness in amplification of the membrane separation technology, has good adsorption and separation functions, and can be combined with a membrane separation component to perform amplification and technological separation.

Description

technical field [0001] The invention relates to the technical fields of polymer chemistry, analytical chemistry, separation and purification, in particular to a preparation method of a chiral separation amlodipine besylate molecularly imprinted membrane. Background technique [0002] Amlodipine besylate is a cardiovascular drug with a chiral center. It is very effective in treating hypertension and angina pectoris. It is a third-generation dihydropyridine derivative calcium channel blocker with strong vascular selectivity and promotes Coronary blood flow can lower blood pressure at the same time, but also relax coronary blood vessels and systemic blood vessels, so it is the drug of choice for the treatment of hypertension. Levoamlodipine (S-amlodipine besylate) is vasodilator, dexamlodipine (R-amlodipine besylate) is inactive, and it is possible that taking racemic amlodipine Causes of lower extremity edema. Compared with dexamlodipine, levamlodipine is a more effective ca...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J9/26C08J7/16C08L27/16C08F226/06C08F222/14B01J20/29B01J20/30
Inventor 陈小明赖申枝蔡昌群陈春燕谢佳琦汤韶坛
Owner XIANGTAN UNIV
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