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Preparation method of chiral molecularly imprinted adsorption-extraction stirring rod

A technology for imprinting adsorption and chiral molecules, which is applied in the field of analytical chemistry and sample pretreatment to achieve the effect of avoiding competitive adsorption

Active Publication Date: 2019-06-28
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Molecularly imprinted polymers have the ability of specific adsorption in molecular recognition, and there is no report on the preparation of chiral molecularly imprinted adsorption and extraction stirring rods by click reaction.

Method used

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  • Preparation method of chiral molecularly imprinted adsorption-extraction stirring rod
  • Preparation method of chiral molecularly imprinted adsorption-extraction stirring rod
  • Preparation method of chiral molecularly imprinted adsorption-extraction stirring rod

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Example 1: The preparation method of the chiral molecularly imprinted stirring rod described in this example, the specific steps are as follows:

[0031] (1) Clean and dry the iron core and put it into the glass capillary I, then melt and seal the two ends of the glass capillary I to obtain a stirring bar, and prepare the glass capillary II sintered at one end as a jacket;

[0032] (2) Dissolve 1 mmol of the chiral template molecule S-naproxen in 15 mL of methanol-dimethyl sulfoxide (1:1, v / v), and then add the chiral functional monomer L-cysteine Hydrochloride 4 mmol, mixed uniformly, pre-assembled for 10 hours to obtain a pre-assembled solution, then added 30 mmol ethylene glycol dimethacrylate and 20 mg azobisisobutyronitrile to the pre-assembled solution, mixed uniformly, The mixed solution was obtained, and then the mixed solution was ultrasonically deoxygenated and degassed, and then the mixed solution was injected into the glass capillary II using a syringe, and ...

Embodiment 2

[0038] Example 2: The preparation method of the chiral molecularly imprinted stirring rod described in this example, the specific steps are as follows:

[0039] (1) Clean and dry the iron core and put it into the glass capillary I, then melt and seal the two ends of the glass capillary I to obtain a stirring bar, and prepare the glass capillary II sintered at one end as a jacket;

[0040] (2) Dissolve 1 mmol of the chiral template molecule S-naproxen in 15 mL of methanol-dimethyl sulfoxide (1:1, v / v), and then add the chiral functional monomer D-cysteine Hydrochloride 4 mmol, mixed well, pre-assembled for 10 h to obtain a pre-assembled solution, then added 20 mmol ethylene glycol dimethacrylate and 20 mg azobisisobutyronitrile to the pre-assembled solution, mixed well , to obtain a mixed solution, and then ultrasonically deoxygenate and degas the mixed solution, and then use a syringe to inject the mixed solution into the glass capillary II, insert a stirrer, and heat in a wat...

Embodiment 3

[0045] Example 3: The preparation method of the chiral molecularly imprinted stirring rod described in this example, the specific steps are as follows:

[0046] (1) Clean and dry the iron core and put it into the glass capillary I, then melt and seal the two ends of the glass capillary I to obtain a stirring bar, and prepare the glass capillary II sintered at one end as a jacket;

[0047] (2) Dissolve 1 mmol of the chiral template molecule S-naproxen in 15 mL of methanol-dimethylsulfoxide (1:1, v / v), and then add the chiral functional monomer N-acetyl-L - Cysteine ​​4 mmol, mixed well, pre-assembled for 10 h to obtain a pre-assembled solution, then added 25 mmol ethylene glycol dimethacrylate and 20 mg azobisisobutyronitrile to the pre-assembled solution, mixed homogeneously to obtain a mixed solution, and then ultrasonically deoxygenate and degas the mixed solution, and then use a syringe to inject the mixed solution into the glass capillary II, insert a stirring bar, and hea...

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Abstract

The invention discloses a preparation method of a chiral molecularly imprinted adsorption-extraction stirring rod and belongs to the technical field of analytical chemistry and sample pretreatment. The preparation method comprises the following steps: first, inserting an iron core into a capillary tube sintered at one end, intercepting a proper length, and then blocking the capillary tube to obtain a stirrer, activating the prepared stirrer, dissolving chiral template modules and a chiral functional monomer in a polymerization solvent, ultrasonically and uniformly mixing the mixture and leaving the mixture to stand, and adding a crosslinking agent and an initiator to obtain an assembling solution and removing oxygen; and injecting the assembling solution without oxygen into the glass capillary tube sintered at one end, inserting the stirrer, carrying out water bath heating and initializing polymerization through a click reaction, removing a jacket of the glass capillary tube after thereaction, and cutting the coating to a proper length by a blade to prepare the chiral molecularly imprinted adsorption-extraction stirring rod. The stirring rod prepared by the preparation method canbe applied to adsorbing a naproxen raceme in a sample.

Description

technical field [0001] The invention relates to a preparation method of a chiral molecular imprinted adsorption extraction stirring rod, which belongs to the technical field of analytical chemistry and sample pretreatment. Background technique [0002] Naproxen is a common NSAID. Naproxen and paracetamol, aspirin and ibuprofen are known as one of the "four pillars" of antipyretic and analgesic drugs [1] . Naproxen has a chiral center and a pair of optical isomers, namely R-naproxen and S-naproxen [2-3] . Due to the difference in the optical enantiomers of chiral drugs, it often leads to different pharmacological activities, so the pharmacological activity of S-naproxen is about 28 times that of R-naproxen. The structure of chiral naproxen is shown in the figure below: [0003] [0004] Chiral functional monomers based on three cysteine ​​derivatives, which contain sulfhydryl functional groups in the structure, and can undergo sulfhydryl click chemistry reactions [4]...

Claims

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Application Information

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IPC IPC(8): B01J20/26B01J20/28B01J20/30B01D15/08
Inventor 许志刚刘育坚刘智敏
Owner KUNMING UNIV OF SCI & TECH
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