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Preparation methods and applications of menthofuran molecular imprinted polymer and monolithic column

A mint furan and molecular imprinting technology, which is applied in chemical instruments and methods, other chemical processes, organic chemistry, etc., can solve the problems that the maximum usage amount and the allowable residue amount are not clearly stipulated, and achieve good and fast molecular recognition performance. The mass transfer rate and the effect of simple and easy preparation process

Inactive Publication Date: 2018-04-20
XINJIANG UYGUR AUTONOMOUS REGION PROD QUALITY SUPERVISION & INSPECTION RES INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to the national standard GB 2760, mint furan is an approved spice in food, but there is no clear regulation on the maximum usage amount and allowable residue amount

Method used

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  • Preparation methods and applications of menthofuran molecular imprinted polymer and monolithic column
  • Preparation methods and applications of menthofuran molecular imprinted polymer and monolithic column
  • Preparation methods and applications of menthofuran molecular imprinted polymer and monolithic column

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] First, dissolve 0.34mmol of the template molecule menthafuran in the porogen toluene / dodecanol (1.89:1.74), add 1.36mmol of the functional monomer methacrylic acid, and 5.1mmol of the crosslinking agent ethylene glycol dimethacrylate , the initiator azobisisobutyronitrile 11 mg was mixed and ultrasonically treated for 15 minutes, and then nitrogen gas was passed for 15 minutes. The solution was injected into a stainless steel chromatographic column (150 mm × 4.6 mmi. The reaction was carried out in a 55°C oven for 24 hours, and thermally initiated to obtain a molecularly imprinted monolithic column. Connect the column to the LC pump with methanol / KH 2 PO 4 (Volume ratio 50 / 50, pH=8) and methanol / water (95 / 5, v / v) cleaning solution to remove the template molecules to obtain the monolithic column (MIP1) of mint furan molecularly imprinted.

Embodiment 2

[0057] Dissolve 0.34 mmol of the template molecule menthol furan in the porogen toluene / dodecanol (2.27:10.36), sonicate in an ice-water bath for 15 minutes, blow nitrogen for 10 minutes, and put it in an oven at 55°C for 24 hours. Others are the same as in Example 1. , and the monolithic column (MIP2) of mentha furan molecularly imprinted can be obtained.

Embodiment 3

[0059] Dissolve 0.34 mmol of the template molecule menthol furan in the porogen toluene / dodecanol (3.415:19.355), 3.4 mmol of the cross-linking agent ethylene glycol dimethacrylate, sonicate for 20 minutes in an ice-water bath, and blow nitrogen for 10 minutes. Put it in an oven at 55° C. for 24 hours, and the others are the same as in Example 1 to obtain a monolithic column (MIP3) of menthafuran molecularly imprinted.

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Abstract

The invention discloses preparation methods and applications of a menthofuran molecular imprinted polymer and a monolithic column. The preparation method of the monolithic column comprises the following steps: dissolving template molecule menthofuran into a pore forming agent, separately adding a functional monomer, a cross-linking agent and an initiator for mixing, performing ultrasonic treatmentin an ice-water bath, introducing a nitrogen gas, injecting the reactants into a stainless steel chromatographic column and a container, performing sealing, putting the sealed objects into a drying oven with the temperature of 50-60 DEG C, performing a reaction for 12-24h to obtain a molecular imprinted polymer monolithic column through thermal initiation, connecting the monolithic column to a liquid chromatography pump to wash away the template molecule, so as to finally obtain the monolithic column with good separation effects. According to the methods, a frontier chromatography method is utilized to analyze the number of effective binding sites and dissociation constant of the prepared molecular imprinted polymer monolithic column and the menthofuran, the molecular recognition performance of the method is good, the molecular imprinted polymer provided by the invention is used as a liquid chromatography column filler and can realize the separation, enrichment and purification of thementhofuran in essential oil with more complex components.

Description

technical field [0001] The invention relates to the technical field of analysis of volatile components of natural products, in particular to a preparation method and application of a menthol furan molecularly imprinted polymer and a monolithic column. Background technique [0002] Molecular imprinting technique (MIT), also called molecular template technology, refers to the use of a specific target molecule as a template and the use of covalent or non-covalent bonds to prepare polymers with specific selectivity for the molecule. process. It is a new high-efficiency separation and molecular recognition technology with superior recognition and selectivity. This technique has been widely used in chiral separation, solid phase extraction, imprinted membrane, sensor and so on. Combining molecular imprinting technology with monolithic column technology is a current frontier topic. The molecularly imprinted monolithic column prepared directly in the chromatographic column by in-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F222/14C08F220/06C08J9/28B01J20/26B01J20/285C07D307/79
CPCB01J20/268B01J20/285B01J2220/84C07D307/79C08F220/06C08F222/1006C08F222/102C08J9/28C08J2335/02
Inventor 鹿毅杨涛孙蕾封顺赵建勇刘莉丁春瑞殷超李静任水英袁辉田蕾
Owner XINJIANG UYGUR AUTONOMOUS REGION PROD QUALITY SUPERVISION & INSPECTION RES INST
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