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Preparation method of scopolamine imprinted monolithic column

A technology of scopolamine and monolithic column is applied in the field of preparation of scopolamine imprinted polymer monolithic column, which can solve the problems of unreachable, limited monomer or template interaction and the like

Inactive Publication Date: 2021-01-29
XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] CN102617674A reports a method for preparing scopolamine monomer from anisodamine root. The method adopts a series of operations such as silica gel column loading, chloroform extraction, dimethyl sulfoxide extraction, semi-preparative liquid phase preparation, etc. But the purity of the scopolamine prepared and purified by this method is only 95%, which does not meet the requirements of the standard substance (purity greater than or equal to 98%)
The metal ions are assembled as fulcrums, and the monomers are regularly positioned around the template through metal bridge coordination, which greatly limits the interaction of monomers or templates

Method used

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  • Preparation method of scopolamine imprinted monolithic column
  • Preparation method of scopolamine imprinted monolithic column
  • Preparation method of scopolamine imprinted monolithic column

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Preparation of scopoletin imprinted monolithic column by in situ polymerization:

[0018] a. template scopoletin 0.94%, bridging agent nickel acetate 0.16%, functional monomer 4-vinylpyridine 0.56%, introduce macromolecular hydrophilic monomer oligo(ethylene glycol) methyl ether methacrylic acid according to mass percentage Ester 3.35%, initiator azobisisobutyronitrile 0.36%, crosslinking agent ethylene glycol dimethacrylate 11.80%, soluble in porogen as 1-butyl-3-methylimidazolium tetrafluoroborate In a mixed solution of 55.32%, 4.03% N,N-dimethylformamide and 23.48% dimethyl sulfoxide, ultrasonically dissolve for 30 minutes to dissolve, clarify, remove oxygen in the liquid, and then inject the mixed solution into a stainless steel column 100 ×4.6mmI.D., seal both ends of the stainless steel column, and react in a water bath at a temperature of 60°C for 12 hours;

[0019] b. Connect the reacted column to the high-pressure pump of HPLC, first wash it with acetonitrile ...

Embodiment 2

[0022] Preparation of scopoletin imprinted monolithic column by in situ polymerization:

[0023] a. 0.47% template scopoletin, 0.16% bridging agent nickel acetate, 0.56% functional monomer 4-vinylpyridine, and macromolecular hydrophilic monomer oligo(ethylene glycol) methyl ether methacrylic acid are introduced by mass percentage Ester 3.37%, initiator azobisisobutyronitrile 0.36%, crosslinking agent ethylene glycol dimethacrylate 11.86%, soluble in porogen as 1-butyl-3-methylimidazolium tetrafluoroborate 55.58%, N,N-dimethylformamide 4.05%, dimethyl sulfoxide 23.59% mixed solution, ultrasonically dissolved for 30 minutes, dissolved, clarified, removed oxygen in the liquid, and then injected the mixed solution into a stainless steel column 100 ×4.6mm I.D., seal both ends of the stainless steel column, and react in a water bath at a temperature of 60°C for 12 hours;

[0024]b. Connect the reacted column to the high-pressure pump of HPLC, first wash it with acetonitrile to remo...

Embodiment 3

[0027] Preparation of scopoletin imprinted monolithic column by in situ polymerization:

[0028] a. 0.31% by mass percentage of template scopoletin, 0.16% of bridging agent nickel acetate, 0.56% of functional monomer 4-vinylpyridine, and introducing macromolecular hydrophilic monomer oligo(ethylene glycol) methyl ether methacrylate 3.37%, initiator azobisisobutyronitrile 0.36%, crosslinking agent ethylene glycol dimethacrylate 11.88%, soluble in porogen 1-butyl-3-methylimidazolium tetrafluoroborate 55.67 %, N,N-dimethylformamide 4.06%, dimethyl sulfoxide 23.63% mixed porogen solution, ultrasonically dissolved for 30 minutes, dissolved, clarified, and oxygen in the liquid was removed, and then the mixed solution was injected into the stainless steel Column 100×4.6mm

[0029] In I.D., seal both ends of the stainless steel column and react in a water bath at a temperature of 60°C for 12 hours;

[0030] b. Connect the reacted column to the high-pressure pump of HPLC, first wash ...

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Abstract

The invention relates to a preparation method of a scopolamine imprinted monolithic column, which comprises the following steps: using scopolamine as a template molecule, 4-vinylpyridine as a functional monomer, oligomeric (ethylene glycol) methyl ether methacrylate as a macromolecular hydrophilic monomer, ionic liquid 1-butyl -3-methylimidazolium tetrafluoroborate as a pore-foaming agent, and metal ions as fulcrums for assembly. The monomers are regularly positioned around a template under the coordination action of metal bridges, so that the interaction of the monomers or the template is greatly limited. The scopolamine crude extract is subjected to separation and purification research by using a molecular imprinting solid-phase extraction technology. Macromolecular hydrophilic monomersare introduced, metal ion nickel acetate serves as a bridging agent, the scopolamine serves as template molecules to synthesize molecularly imprinted polymers, due to the existence of the metal ions and the macromolecular hydrophilic monomers, the combination of the template molecules and imprinted holes has high specificity, and the imprinting effect of MIPs is improved. The imprinting factor ofthe polymer to the scopolamine is 2.53.

Description

technical field [0001] The invention relates to a preparation method of a scopolamine imprinted polymer monolithic column. The imprinted monolithic column shows good selectivity and specificity to scopolamine, and can be used for the separation and purification of scopolamine. Background technique [0002] Scopolamine, commonly known as belladonna, is the dry whole plant of the nightshade plant Atropa belladonna L., which mainly contains alkaloids. As a potential drug, it has anti-rheumatic, swelling and pain-relieving effects, and can be used to treat rheumatic pain . Pharmacological studies in recent years have shown that it has good antioxidant activity on nerve cells. Kong Yushan et al. Development, 2014.] The research results show that scopoletin can not only protect the cell membrane from damage to a certain extent, but also restore the activity of antioxidant enzymes or antioxidants in nerve cells. However, since scopolamine can be separated and extracted by convent...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/26B01J20/285C08F222/14C08F220/28C08F226/06C08J9/26
CPCB01J20/268B01J20/285C08F222/102C08J9/26C08F220/286C08F226/06
Inventor 黄艳萍张雪杨建刘照胜阿吉艾克拜尔·艾萨
Owner XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI