Preparation method and application of a camphor molecularly imprinted polymer and its monolithic column and packed chromatographic column

A packed chromatographic column and molecular imprinting technology is applied in the field of preparation of camphor molecularly imprinted polymer and its monolithic column and packed chromatographic column, and achieves the effects of good molecular recognition performance, simple and easy preparation process, and overcoming serious impurity interference.

Inactive Publication Date: 2016-03-09
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

With the continuous development and growth of the essential oil industry, quality problems are also emerging. The main reason is that there is no complete technical method to identify the quality of essential oils, true and false in China.

Method used

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  • Preparation method and application of a camphor molecularly imprinted polymer and its monolithic column and packed chromatographic column
  • Preparation method and application of a camphor molecularly imprinted polymer and its monolithic column and packed chromatographic column
  • Preparation method and application of a camphor molecularly imprinted polymer and its monolithic column and packed chromatographic column

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Firstly, 0.9 mmol of template molecule camphor was dissolved in 8 mL of porogen methanol, and 1.8 mmol of functional monomer methacrylic acid, 8 mmol of crosslinking agent ethylene glycol dimethacrylate, and 30 mg of initiator azobisisobutyronitrile were added and mixed. ; Ultrasonic treatment in an ice-water bath for 15 minutes, then pass nitrogen gas for 15 minutes, inject this solution into a stainless steel chromatographic column (150 mm × 4.6 mmi.d) that has sealed the lower nozzle, seal the upper nozzle, and put it into an oven at 50 ° C for reaction After 24 hours, thermal initiation resulted in a molecularly imprinted monolithic column. Connect the column to the liquid chromatography pump and use methanol:water (95:5, v / v) to remove the template molecules to obtain a camphor molecularly imprinted monolithic column (MIP1).

Embodiment 2

[0041]Firstly, 0.9 mmol of template molecule camphor was dissolved in 8 mL of porogen methanol, and 3.6 mmol of functional monomer methacrylic acid, 8 mmol of cross-linking agent ethylene glycol dimethacrylate, and 30 mg of initiator azobisisobutyronitrile were added and mixed. ; Ultrasonic treatment in an ice-water bath for 15 minutes, and then pass nitrogen gas for 10 minutes, inject this solution into a stainless steel chromatographic column (150 mm × 4.6 mmi.d) that has sealed the lower nozzle, seal the upper nozzle, and put it into a 55 ° C oven for reaction After 24 hours, thermal initiation resulted in a molecularly imprinted monolithic column. Connect the column to the liquid chromatographic pump and use methanol:water (95:5, v / v) to remove the template molecules to obtain a camphor molecularly imprinted monolithic column (MIP2).

Embodiment 3

[0043] Firstly, 0.9 mmol of template molecule camphor was dissolved in 8 mL of porogen methanol, and 5.4 mmol of functional monomer methacrylic acid, 8 mmol of cross-linking agent ethylene glycol dimethacrylate, and 30 mg of initiator azobisisobutyronitrile were added and mixed. ; Ultrasonic treatment in an ice-water bath for 20 minutes, then pass nitrogen gas for 10 minutes, inject this solution into a stainless steel chromatographic column (150 mm × 4.6 mmi.d) that has sealed the lower nozzle, seal the upper nozzle, and put it into a 55 ° C oven for reaction For 12 hours, thermal initiation resulted in a molecularly imprinted monolithic column. Connect the column to the liquid chromatography pump and use methanol: water (95:5, v / v) to remove the template molecules to obtain a camphor molecularly imprinted monolithic column (MIP3).

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Abstract

The present invention discloses a camphor molecular imprinted polymer, and a preparation method and application of a monolithic column and a packed column thereof. The preparation method includes dissolving a template molecule camphor in a pore-foaming agent, adding a functional monomer, a crosslinker and an initiator, mixing, treating by ultrasound in an ice-water bath, feeding nitrogen, injecting the reactant into a stainless steel chromatographic column and a container, sealing, placing in an oven of 50-60 DEG C to react for 12-24h, and initiating by heat to obtain a molecular imprinted polymer monolith column and the polymer. The polymer is ground, sieved and filled in a chromatographic column to get a molecular imprinted polymer packed column. The packed column and the monolithic column are connected with a liquid chromatography pump to remove the template molecules. Finally the chromatographic and the monolithic column with good separation effects are obtained. The method is good in molecular recognition. The molecular imprinted polymer provided by the invention as a liquid chromatographic column filler can realize separation, enrichment and purification for camphor in essential oil.

Description

technical field [0001] The invention relates to the technical field of volatile component analysis of natural products, in particular to a camphor molecularly imprinted polymer (Molecular Imprinted Polymer, MIP) and a preparation method and application of a monolithic column and a packed chromatographic column. Background technique [0002] Molecular imprinting technology is a new high-efficiency separation and molecular recognition technology with superior recognition and selectivity. Molecularly imprinted polymers are high molecular polymers that match a specific compound (template molecule) at the binding site and chemical space structure. Due to the excellent molecular recognition performance and good physical and chemical stability, molecularly imprinted polymers have shown good application prospects in chromatographic analysis, solid phase extraction, membrane separation, catalysts, etc. The chromatographic column synthesized by the bulk polymerization method is the m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F222/14C08F220/06C08J9/26C08J9/28B01J20/285B01J20/30C07C49/437C07C45/79G01N30/60
Inventor 鹿毅杨涛孙蕾任水英于红封顺
Owner XINJIANG UYGUR AUTONOMOUS REGION PROD QUALITY SUPERVISION & INSPECTION RES INST
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