Carbon quantum dot doped liquid chromatography filler as well as preparation method and application thereof

A technology of carbon quantum dots and doped liquid phase, which is applied in the field of chromatographic packing, can solve the problems of poor peak shape symmetry and short retention time, and achieve the effect of high specific surface area and abundant action sites

Pending Publication Date: 2022-04-08
YANTAI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, some small molecules such as nucleoside antibiotics and sulfonamide antibiotics with strong polarity have problems such as short retention time and poor peak shape symmetry (Microchemical Journal 2018, 195-201; Molecules 2019, 24, 2580), so it is urgent to develop Novel Chromatographic Separation Materials to Compensate for Inadequacies of Existing Materials

Method used

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  • Carbon quantum dot doped liquid chromatography filler as well as preparation method and application thereof
  • Carbon quantum dot doped liquid chromatography filler as well as preparation method and application thereof
  • Carbon quantum dot doped liquid chromatography filler as well as preparation method and application thereof

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preparation example Construction

[0026] refer to figure 1 , the preparation method of the carbon quantum dot-doped liquid chromatographic filler provided by the present invention comprises: silica gel acidification and double bond modification steps, carbon dot doping and polymerization steps.

[0027] 1. Silica gel acidification and double bond modification

[0028] Silica gel: select commercial bare silica gel, with a particle size of 1-50 μm and a pore size of 15-50 nm.

[0029] Silylating reagents: γ-methacryloxypropyltrimethoxysilane (γ-MPS), vinyltriisopropoxysilane, vinyltriethoxysilane, vinyltriacetoxysilane, ethylene One or more of yltrimethoxysilane and vinyltris(2-methoxyethoxy)silane.

[0030] Catalyst: pyridine or triethylamine.

[0031] Reaction solvent: toluene.

[0032] (1) Acidification of silica gel

[0033] Prepare an aqueous solution of nitric acid, hydrochloric acid or a mixture of the two. The concentration of hydrogen ions in the aqueous solution is 2-10mol / L. Add silica gel to the...

Embodiment 1

[0049] Prepare a nitric acid aqueous solution with a concentration of 3.35 mol / L, take commercial bare silica gel with a particle size of 5 μm and a pore size of 20 nm, add bare silica gel to the nitric acid aqueous solution at a ratio of 10 mL:1 g, stir at 25 °C for 1.5 h, and wash with water until Wash with neutral and absolute ethanol three times to obtain acidified silica gel, and dry it in vacuum at 50°C for later use.

[0050] Mix γ-methacryloxypropyltrimethoxysilane (silylating agent), triethylamine (catalyst), toluene (reaction solvent) and acidified silica gel according to the ratio of 2.5mL: 0μL: 50mL: 1g Then heat and stir to reflux, wash the material several times with toluene and absolute ethanol respectively, and dry it in vacuum at 50° C. to obtain a double-bond-modified silica gel.

[0051] Methacrylic acid (functional monomer), methanol (porogen) and zidovudine (template molecule) were mixed according to the ratio of 40μL: 100mL: 200mg, and prepolymerized at 4°C...

Embodiment 2

[0064] Prepare a hydrochloric acid aqueous solution with a concentration of 2mol / L, take commercial bare silica gel with a particle size of 20μm and a pore size of 30nm, add bare silica gel to the aqueous hydrochloric acid solution at a ratio of 10mL:1g, stir at 30°C for 2h, and wash with water until neutral , washed 3 times with absolute ethanol to obtain acidified silica gel, dried in vacuum at 55°C for later use.

[0065] Mix vinyltriisopropoxysilane (silylating agent), pyridine (catalyst), toluene (reaction solvent) and acidified silica gel according to the ratio of 1mL: 0.5mL: 100mL: 1g, heat and stir to reflux, and use toluene respectively Wash the material several times with absolute ethanol, and dry it under vacuum at 55°C to obtain a double-bond-modified silica gel.

[0066] Methyl methacrylate (functional monomer), ethanol (porogen) and sulfonamide (template molecule) were mixed according to the ratio of 500μL: 1000mL: 1mg, and prepolymerized at -10°C for 5h to obtai...

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Abstract

The invention discloses a carbon quantum dot doped liquid chromatography filler and a preparation method and application thereof.The preparation method comprises the steps that silica gel is acidified, a silanization reagent, a catalyst, a reaction solvent and the acidified silica gel are mixed, heated, stirred and refluxed, and double-bond modified silica gel is obtained; the preparation method comprises the following steps: mixing and pre-polymerizing a functional monomer, a pore-foaming agent and template molecules to obtain a pre-polymerization system, adding a cross-linking agent, double-bond modified silica gel, an initiator and carbon quantum dots into the pre-polymerization system, carrying out programmed heating, stirring for a period of time, washing and drying to obtain the carbon quantum dot doped liquid chromatography filler. According to the chromatographic packing prepared by the invention, the properties of small size effect, high specific surface area, abundant acting sites and the like of the carbon quantum dot material are combined with the unique selectivity of the molecularly imprinted polymer and various excellent properties that the porous silica gel is suitable for being used as a chromatographic separation material carrier; therefore, the method is suitable for separation and analysis of various small-molecule polar drugs.

Description

technical field [0001] The invention relates to a liquid chromatography filler and its preparation method and application, in particular to a carbon quantum dot-doped liquid chromatography filler and its preparation method and application in the separation of polar medicines, belonging to the technical field of chromatography fillers. Background technique [0002] At present, in the separation and analysis of liquid chromatography, the reversed-phase chromatography separation mode occupies the vast majority. However, some small molecules such as nucleoside antibiotics and sulfa antibiotics with strong polarity have problems such as short retention time and poor peak shape symmetry (Microchemical Journal 2018, 195-201; Molecules 2019, 24, 2580), so it is urgent to develop New chromatographic separation materials to make up for the deficiencies of existing materials. [0003] Carbon quantum dots have excellent properties such as small size effect, high surface area, π bond in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/26B01J20/20B01D15/08C07B63/00C07C51/47C07C63/06C07C65/03C07D213/80C07H19/067C07D473/34C07H19/073C07H1/06
Inventor 宋志花柴佩君朱瑞瑞王玉朦林文刘金秋张京秀薛俊萍吴文璞张异梦
Owner YANTAI UNIV
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