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

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Problems solved by technology

[0006] Molecularly imprinted polymers have the ability of specific adsorption in molecular recognition, and there is n

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

Example Embodiment

[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) After cleaning and drying the iron core, put it into the glass capillary Ⅰ, then melt and seal the two ends of the glass capillary Ⅰ to obtain a stir bar, and prepare a glass capillary Ⅱ with one end sintered as the outer jacket;

[0032] (2) Dissolve 1 mmol of chiral template molecule S-naproxen in 15 mL methanol-dimethyl sulfoxide (1:1, v / v), and then add the chiral functional monomer L-cysteamine 4 mmol hydrochloride, mix well, pre-assemble for 10 hours to obtain a pre-assembled solution, then add 30 mmol ethylene glycol dimethacrylate and 20 mg azobisisobutyronitrile to the pre-assembled solution, mix well, Obtain the mixed solution, and then perform ultrasonic deoxidation and degassing of the mixed solution. Then, use a syringe to inject the mixed solution into the glass capillary II, insert a stir bar, and heat in...

Example Embodiment

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

[0039] (1) After cleaning and drying the iron core, put it into the glass capillary Ⅰ, then melt and seal the two ends of the glass capillary Ⅰ to obtain a stir bar, and prepare a glass capillary Ⅱ with one end sintered as the outer jacket;

[0040] (2) Dissolve 1 mmol of the chiral template molecule S-naproxen in 15 mL methanol-dimethyl sulfoxide (1:1, v / v), and then add the chiral functional monomer D-cysteamine 4 mmol of hydrochloride, mix well, pre-assemble for 10 hours to obtain a pre-assembled solution, then add 20 mmol of ethylene glycol dimethacrylate and 20 mg of azobisisobutyronitrile to the pre-assembled solution, and mix well , The mixed solution is obtained, and then the mixed solution is ultrasonically deaerated and degassed, and then the mixed solution is injected into the glass capillary II with a syringe, an...

Example Embodiment

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

[0046] (1) After cleaning and drying the iron core, put it into the glass capillary Ⅰ, then melt and seal the two ends of the glass capillary Ⅰ to obtain a stir bar, and prepare a glass capillary Ⅱ with one end sintered as the outer jacket;

[0047] (2) Dissolve 1 mmol of the chiral template molecule S-naproxen in 15 mL methanol-dimethyl sulfoxide (1:1, v / v), and then add the chiral functional monomer N-acetyl-L -4 mmol of cysteine, mix well, pre-assemble for 10 hours to obtain a pre-assembled solution, then add 25 mmol of ethylene glycol dimethacrylate and 20 mg of azobisisobutyronitrile to the pre-assembled solution, and mix After uniformity, the mixed solution is obtained, and then the mixed solution is ultrasonically deaerated and degassed, and then the mixed solution is injected into the glass capillary II with a syring...

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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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