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Preparation and application of tetraethylenepentamine carbon quantum dot/monomer co-bonded silica gel hydrophilic chromatography stationary phase

A tetraethylenepentamine carbon quantum and tetraethylenepentamine technology is applied in the field of separation of base nucleosides, amino acids and ginsenosides, achieving excellent separation effects, simple and reliable methods, and cheap and easy-to-obtain raw materials

Active Publication Date: 2019-11-01
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

So far, there are no reports and products based on tetraethylenepentamine carbon quantum dots doped tetraethylenepentamine monomer co-bonded silica gel hydrophilic chromatography stationary phase

Method used

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  • Preparation and application of tetraethylenepentamine carbon quantum dot/monomer co-bonded silica gel hydrophilic chromatography stationary phase
  • Preparation and application of tetraethylenepentamine carbon quantum dot/monomer co-bonded silica gel hydrophilic chromatography stationary phase
  • Preparation and application of tetraethylenepentamine carbon quantum dot/monomer co-bonded silica gel hydrophilic chromatography stationary phase

Examples

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Effect test

Embodiment 1

[0046] 5.0 g of tetraethylenepentamine was placed in a 100 mL three-necked flask, and then deoxygenated with nitrogen for 10 min. It was then heated to 240° C. and 1.0 g of anhydrous citric acid was added with vigorous stirring. After the reaction lasted for 1 min, the resulting reddish-brown solution was cooled to 190 °C, and then the reaction solution was blown with nitrogen to remove excess TEPA under continuous stirring until the total mass of the reaction solution became 2.0 g, and a mixture of TEPACDs and TEPA was obtained. Take 2.0g TEPACDs and TEPA, dissolve in 20 mL of anhydrous acetonitrile; take another 2.0 g gamma - Isocyanatopropyltriethoxysilane (ICPTES) was added to 10 mL of anhydrous acetonitrile, and the ICPTES solution was added dropwise to the mixed solution of TEPACDs and TEPA within 3 h under stirring (in the first Within hours, the reaction solution needs to be placed in ice water to keep the reaction at low temperature), after the ICPTES solution is add...

Embodiment 2

[0049] Take 5.0 g of tetraethylenepentamine in a 100 mL three-necked flask, and then deoxygenate it with nitrogen for 10 min; then heat it to 250 °C, add 2.0 g of anhydrous citric acid under vigorous stirring, and continue the reaction for 3 min. The reddish-brown solution was cooled to 160°C, and the reaction solution was blown with nitrogen to remove excess TEPA under continuous stirring until the total mass of the reaction solution became 3.0g to obtain a mixture of TEPACDs and TEPA; then 2.0g of TEPACDs and TEPA mixture was dissolved in 20 mL of anhydrous acetonitrile, then take 2.0 g gamma - Isocyanatopropyltriethoxysilane (ICPTES) was added to 10 mL of anhydrous acetonitrile, and the ICPTES solution was added dropwise to the mixed solution of TEPACDs and TEPA within 3 h under stirring (in the first Within hours, the reaction solution needs to be placed in ice water to keep the reaction at low temperature). After the addition of the ICPTES solution was completed, the rea...

Embodiment 3

[0051] Take 5.0 g of tetraethylenepentamine in a 100 mL three-necked flask, then heat it to 200 °C, add 2.0 g of anhydrous citric acid under vigorous stirring, continue the reaction for 5 min, and then cool the obtained red-brown solution to 150 °C. Then, the reaction solution was blown with nitrogen to remove excess TEPA under continuous stirring until the total mass of the reaction solution became 3.5 g, and a mixture of TEPACDs and TEPA was obtained. Dissolve 2.0 g of the above mixture in 20 mL of anhydrous acetonitrile, then add 4.0 g of γ-isocyanatopropyltriethoxysilane (ICPTES) into 10 mL of anhydrous acetonitrile, and dissolve the ICPTES solution within 3 h under stirring Add dropwise to the mixed solution of TEPACDs and TEPA (in the first hour of the reaction, the reaction solution needs to be placed in ice water to keep the reaction at low temperature). After the ICPTES solution was added dropwise, the reaction was continued for 11 h at room temperature. Finally, 2.0...

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Abstract

The invention discloses a preparation method of a tetraethylenepentamine carbon quantum dot / monomer co-bonded silica gel chromatographic packing. The preparation method comprises the following steps:reacting tetraethylenepentamine (TEPA) serving as a precursor substance and a medium with citric acid to prepare a mixture of functionalized carbon quantum dots (TEPACDs) and a TEPA monomer; and carrying out silanization treatment on the functionalized carbon quantum dots TEPACDs, and bonding the silanized functionalized carbon quantum dots TEPACDs to the surface of silica gel to prepare the silica gel chromatographic stationary phase Sil-TEPA / CDs formed by co-bonding of the TEPACDs and the TEPA monomer. Material characterization experiments show that the bonding amount of surface functional groups of the Sil-TEPA / CDs is large, and rich interaction sites can be provided for chromatographic separation of samples. Chromatographic separation experiments show that the hydrophilic chromatographic stationary phase Sil-TEPA / CDs prepared by the invention has good hydrophilic chromatographic selectivity, and has an excellent separation effect on basic nucleoside, amino acids and ginsenoside.

Description

technical field [0001] The invention relates to the preparation of a tetraethylenepentamine carbon quantum dot doped tetraethylenepentamine monomer co-bonded silica gel hydrophilic chromatographic filler, which is mainly used for the separation of basic nucleosides, amino acids and ginsenosides, and belongs to the chromatographic stationary phase technology field. Background technique [0002] Hydrophilic interaction liquid chromatography (HILIC) is an important branch of liquid chromatography, which is suitable for the separation of strongly polar and hydrophilic substances. The development of new hydrophilic chromatographic stationary phases is an important part of the research and application of hydrophilic interaction chromatography. [0003] Carbon quantum dots have the advantages of various types, easy functionalization, rich surface groups, etc., and have extremely small particle size and moderate adsorption capacity. When used as a silica gel packing bonded phase, i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/30B01D15/30
CPCB01D15/305B01J20/286
Inventor 邱洪灯蔡天培陈佳
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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