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Application of graphene quantum dot in hydrophilic chromatographic analysis

A graphene quantum dot and hydrophilic interaction technology, applied in the field of hydrophilic interaction chromatography, can solve problems such as complex bonding schemes, and achieve the effect of enhancing hydrophilic performance and high stability

Inactive Publication Date: 2018-06-29
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there is no universal hydrophilic interaction chromatographic column that can be widely used in the separation of hydrophilic compounds. They only show certain retention and separation capabilities for specific compounds.
If you want to modify different types of strong polar groups on the silica matrix to broaden its application range, the bonding scheme may be very complicated, so it is necessary to find a substance or material containing a variety of strong polar groups to serve the hydrophilic water interaction chromatography

Method used

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  • Application of graphene quantum dot in hydrophilic chromatographic analysis
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  • Application of graphene quantum dot in hydrophilic chromatographic analysis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Embodiment 1: Preparation of graphene quantum dots containing different functional groups

[0028] Graphene oxide powder (provided by Beijing Deke Daojin Technology Co., Ltd.) was ultrasonically processed to form a 5 mg / mL solution. Take 50 mL of the above solution, add 1 mL ammonia water and 6 mL hydrogen peroxide (30%), and transfer to a 400 mL high-pressure React in the kettle at 200 °C for 3 h, cool to room temperature, filter with a 0.22 µm nylon membrane, dialyze the filtrate with a 500-1000 KDa dialysis bag for 2 days, and freeze-dry to obtain yellow powder graphene quantum dots. Gained graphene quantum dots are separated by silica gel column chromatography to obtain graphene quantum dots containing hydroxyl and alkoxy groups ( figure 1 ) and graphene quantum dots containing hydroxyl, carboxyl and alkoxy groups ( figure 2 ).

Embodiment 2

[0029] Example 2: Separation of alkaloids by graphene quantum dots containing hydroxyl and alkoxy groups in the mode of hydrophilic interaction chromatography

[0030] In a 500 mL round bottom flask, add 200 mg of graphene quantum dots containing hydroxyl and alkoxy groups, 200 mL of N,N-dimethylformamide, sonicate for 15 min to disperse the graphene quantum dots, and then add 100 mg of isocyanate propionate Triethoxysilane reagent, stirred at 80 °C for 6 h to react the hydroxyl groups of graphene quantum dots; 2 g of silica gel was added to the above solution, and the reaction was continued for 6 h. After the reaction, the product was centrifuged and washed three times with water, methanol, and ethanol, respectively, and dried in a vacuum oven at 60°C. Elemental analysis results: C 1.67%, N 0.37%, H 0.67%. Pack the obtained stationary phase packing into a 4.6 mm * 150 mm I.D. stainless steel chromatographic column.

[0031] The prepared chromatographic column was used to te...

Embodiment 3

[0032] Example 3: Separation of alkaloids by graphene quantum dots containing hydroxyl, carboxyl and alkoxy groups in the mode of hydrophilic interaction chromatography

[0033] In a 500 mL round bottom flask, add 200 mg of graphene quantum dots containing hydroxyl, carboxyl and alkoxy groups, 200 mL of N,N-dimethylformamide, sonicate for 15 min to disperse the graphene quantum dots, and then add 100 mg of EDC (1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride) / NHS (N-hydroxysuccinimide) coupling agent, stirred at room temperature for 30 min to activate graphene quantum point carboxyl group; add 20 µL of aminopropyltriethoxysilane and stir at room temperature for 12 h. 2 g of silica gel was added to the above solution, the temperature was raised to 80 °C, and the reaction was continued for 6 h. After the reaction, the product was centrifuged and washed three times with water, methanol, and ethanol, respectively, and dried in a vacuum oven at 60°C. Elemental analysi...

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Abstract

The invention relates to an application of graphene quantum dot in a hydrophilic chromatographic analysis. The method comprises the following steps: 1) bonding the graphene quantum dot on silica gel;2) filling a chromatographic column with the graphene quantum dot-modified silica gel; and 3) performing separating analysis on an analyte. The graphene quantum dot can be taken as a hydrophilic chromatogram fixed-phase component, hydrophilic performance of the fixed-phase is enhanced, and the fixed phase contains a plurality of strong-polar functional groups, so that a plurality of strong-polar substances can be kept and separated. The graphene quantum dot can be used as the effective components of the hydrophilic chromatogram fixed-phase, the preparation is simple, and stability is high.

Description

technical field [0001] The invention belongs to the technical field of hydrophilic interaction chromatography and relates to the application of graphene quantum dots in hydrophilic interaction chromatography analysis. Background technique [0002] Hydrophilic interaction chromatography is a chromatographic technique used to improve the retention of highly polar substances that are poorly retained in reversed-phase chromatography. It achieves the retention and separation of highly polar substances by using a strong polar stationary phase combined with a mobile phase composed of a high proportion of organic phase / low proportion of water phase, and such a mobile phase is especially beneficial to improve the efficiency of electrospray ionization mass spectrometry Sensitivity has attracted the attention of researchers in the field of chromatography in recent years. [0003] Strong polar chromatography stationary phase is the core part of hydrophilic interaction chromatography, a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06G01N30/74
CPCG01N30/06G01N30/74
Inventor 赵亮武琪董树清李辉罗国英
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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