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Chiral capillary electrochromatography open tube column based on gold nano-modification, preparation method and application

A technology of capillary electrochromatography and capillary column, which is applied in the direction of instruments, measuring devices, scientific instruments, etc., to achieve the effect of improving separation and selectivity

Active Publication Date: 2020-09-25
济宁市第一人民医院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] At present, there are no related reports on the introduction of gold nanoparticles, glycidyl methacrylate and glutathione into chiral capillary electrochromatographic open-tube columns

Method used

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  • Chiral capillary electrochromatography open tube column based on gold nano-modification, preparation method and application
  • Chiral capillary electrochromatography open tube column based on gold nano-modification, preparation method and application
  • Chiral capillary electrochromatography open tube column based on gold nano-modification, preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0062] Preparation of gold nanoparticles

[0063] Take a clean round bottom flask and prepare 100ml of HAuCl with a mass concentration of 0.01% 4 The aqueous solution is heated until the solution boils, and 0.7ml of a mass concentration of 1% trisodium citrate aqueous solution is added under the condition of magnetic stirring, and the heating and boiling reaction is continued for 15 minutes. It can be observed that the color of the solution changes from light yellow to gray, and finally to black. Finally stabilized to red. Stop the reaction, cool to room temperature, add distilled water to restore the original volume. Put it in the refrigerator at 4°C for later use.

[0064] The size and shape of the synthesized gold nanoparticles were characterized, and its particle size was measured by a Malvern laser particle size analyzer. It can be seen from the report that the average particle size of the synthesized gold nanoparticles is about 40nm, and the particle size distribution ...

Embodiment 2

[0066] Preparation of Gold Nanocoated Columns

[0067] Capillary column activation: first rinse the capillary column with 1mol / L NaOH for 1h, rinse with water until neutral, then rinse the capillary with 1mol / L HCl for 30min, rinse with water until neutral, rinse with methanol for 15min, blow dry with nitrogen, and activate at 100°C for 1h , placed in a 4°C refrigerator for later use.

[0068] The first step: silanization of the inner surface of the capillary. Prepare 50% (V / V) γ-MAPS methanol solution, pour it into the activated capillary column, cap it, and place it in a water bath at 55°C for 10-14 hours. Take it out, flush it with methanol to remove unreacted γ-MAPS, and flush it dry with nitrogen gas for later use.

[0069] Step 2: Synthesize the GMA polymer layer. Prepare 10% (w / w) GMA dissolved in toluene, add about 0.75mg / ml AIBN as a thermal initiator, flush it into a silanized capillary column, cap it, and react in a water bath at 80°C for 10-14 hours. Wash the c...

Embodiment 3

[0075] Preparation of sample solution and running buffer

[0076] Sample solution: Take an appropriate amount of the above drugs, dissolve them in water or methanol, and prepare a sample solution with a concentration of 1 mg / ml. The injection concentration is 1 mg / ml, and thiourea is used as a neutral marker.

[0077] Preparation of running buffer solution: Weigh an appropriate amount of chiral selector CM-β-CD according to the required conditions, dissolve it in 40mmol / L Tris solution, add dropwise 30% phosphoric acid to adjust to the required pH value, all sample solutions And the running buffer is used after being sonicated through a 0.45 μm microporous membrane.

[0078] Calculation formula:

[0079] The formula for calculating electroosmotic flow is:

[0080] mu eof= ( L × l ) / ( V × t 0 )

[0081] where μ eof is the electroosmotic flow, L, l is the total length and effective length of the capillary; V is the operating voltage; t 0 is the peak time of the neutral...

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Abstract

The invention relates to a chiral capillary electrochromatography open tube column based on gold nano modification, a preparation method and an application. The method comprises the steps: bonding a glycidyl methacrylate (GMA) tentacle type polymer coating on the inner wall of a capillary tube; carrying out alkaline ring opening on an epoxy group of GMA under an alkaline condition by utilizing amino of reduced glutathione (GSH), and successfully synthesizing GSH on the capillary tube column; combining gold nanoparticles on the capillary tube column by utilizing the property that sulfydryl of glutathione can generate Au-S bonds with the gold nanoparticles, successfully introducing gold nanoparticles into a capillary stationary phase, and constructing a chiral resolution system based on carboxymethyl-beta-cyclodextrin. Experiments prove that compared with a hollow tubular column which is not modified with gold nanoparticles, the prepared capillary open tube column has the advantages thatthe separation degree and selectivity of three lol drugs (atenolol, sotalol and bisoprolol) are greatly improved, and the purpose of baseline separation is achieved.

Description

technical field [0001] The invention belongs to the technical field of capillary column preparation, and relates to a chiral capillary electrochromatographic open column based on gold nanometer modification, a preparation method and an application. Background technique [0002] More than half of the more than 1,850 commonly used clinical drugs are chiral drugs, and most of them are put on the market in racemic form. Studies have found that drug enantiomers usually have different pharmacological effects, pharmacokinetic behaviors and toxic effects. For example, thalidomide, which has a sedative effect, its R type is used to treat pregnancy reactions in pregnant women, while its S type causes fetal malformations. Due to technical difficulties in separation and analysis, most drug enantiomers are sold in the market in the form of racemates, which is extremely dangerous. [0003] Chromatography is currently the most effective method for chiral separation detection methods. Am...

Claims

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Application Information

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IPC IPC(8): G01N30/60
CPCG01N30/6078Y02P20/55
Inventor 江沛赵世媛崔昌萌徐鹏飞王长水
Owner 济宁市第一人民医院
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