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Fluorine-containing liquid chromatography filler for polar drug separation and preparation method of fluorine-containing liquid chromatography filler

A liquid chromatography and drug technology, which is applied in the field of chromatographic packing, can solve the problems of unsatisfactory separation effect of polar drugs and insufficient coverage of packing surface, and achieve good separation of polar drugs, high coverage and simple process.

Pending Publication Date: 2022-07-29
YANTAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, most of the commonly used fluorine-containing functional group-bonded silica gel fillers use a single fluorine-containing silanization reagent to modify the porous silica gel, and the surface coverage of the filler is not high enough, resulting in an unsatisfactory separation effect of polar drugs.

Method used

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  • Fluorine-containing liquid chromatography filler for polar drug separation and preparation method of fluorine-containing liquid chromatography filler
  • Fluorine-containing liquid chromatography filler for polar drug separation and preparation method of fluorine-containing liquid chromatography filler
  • Fluorine-containing liquid chromatography filler for polar drug separation and preparation method of fluorine-containing liquid chromatography filler

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Silica gel microspheres: particle size 5μm, pore size 10nm.

[0032] Fluorine-substituted silylation reagent containing benzene ring: pentafluorophenylpropyltrimethoxysilane.

[0033] Fluorine-substituted silylation reagent containing aliphatic chain: trimethoxy (1H, 1H, 2H, 2H-heptadecafluorodecyl) silane.

[0034] Basic catalyst: triethylamine.

[0035] Silanation capping reagent: trichloro(3,3,3-trifluoropropyl)silane.

[0036] Step1: Add pentafluorophenylpropyltrimethoxysilane and triethylamine to anhydrous toluene, then add silica gel microspheres, pentafluorophenylpropyltrimethoxysilane, anhydrous toluene, triethylamine and silica gel The ratio of the microspheres is: 110 μL: 25 mL: 445 μL: 1 g, and the reaction is stirred for 12 h. After the reaction is completed, it is washed with anhydrous toluene and anhydrous ethanol in turn, and finally dried to prepare fluorine-containing silica microspheres bonded once.

[0037] Step2: Replace the fluorine-substituted s...

Embodiment 2

[0044] Silica gel microspheres: particle size 3μm, pore size 15nm.

[0045] Fluorine-substituted silylation reagent containing benzene ring: (2,4-difluorophenyl)trimethylsilane.

[0046] Fluorine-substituted silylation reagents containing aliphatic chain: (heptafluoroisopropoxy)propylmethyldichlorosilane, 1H, 1H, 2H, 2H-perfluorodecyltrichlorosilane.

[0047] Basic catalyst: pyridine.

[0048] Silanation capping reagent: Trimethylchlorosilane.

[0049] Step1: Add (2,4-difluorophenyl)trimethylsilane and pyridine into anhydrous toluene, then add silica gel microspheres, (2,4-difluorophenyl)trimethylsilane, and anhydrous toluene The ratio of , pyridine and silica gel microspheres is: 10 μL: 10 mL: 1 μL: 1 g, stirring and reacting for 5 h, washing with anhydrous toluene and anhydrous ethanol in turn after the reaction, and finally drying. Silica microspheres.

[0050] Step2: Replace the fluorine-substituted silylation reagent, add (heptafluoroisopropoxy)propylmethyldichlorosil...

Embodiment 3

[0054] Silica gel microspheres: particle size 6 μm, pore size 30 nm.

[0055] Fluorine-substituted silylation reagents containing benzene ring: (3,5-difluorophenylethynyl)trimethylsilane, (2-fluorophenyl)trimethylsilane.

[0056] Fluorine-substituted silylation reagents containing aliphatic chain: 1H, 1H, 2H, 2H-perfluorodecyldimethylchlorosilane, 1H,1H, 2H,2H-perfluorooctyltrichlorosilane.

[0057] Basic catalyst: triethylamine.

[0058] Silanation capping reagent: dimethyldichlorosilane.

[0059] Step1: Add (3,5-difluorophenylethynyl)trimethylsilane and triethylamine to anhydrous toluene, then add silica gel microspheres, (3,5-difluorophenylethynyl)trimethylsilane The ratio of base silane, anhydrous toluene, triethylamine and silica gel microspheres is: 5mL: 50mL: 5mL: 1g, and the reaction is stirred for 24h. Fluorine-containing silica microspheres bonded once.

[0060] Step2: Replace the fluorine-substituted silylation reagent, add (2-fluorophenyl)trimethylsilane and tr...

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Abstract

The invention discloses a fluorine-containing liquid chromatogram filler for polar drug separation and a preparation method thereof, the fluorine-containing liquid chromatogram filler takes silica gel microspheres as a matrix, the surface of the matrix is bonded with two types of fluorine-containing functional groups, i.e., 2-5 fluorine-containing functional groups, one class of the fluorine-containing functional groups is fluorine substituent groups containing benzene rings, and the other class of the fluorine-containing functional groups is fluorine substituent groups containing lipid chains. The fluorine-containing liquid chromatography packing has the beneficial effects that the fluorine-containing liquid chromatography packing contains rich fluorine-containing functional groups, has relatively strong chemical stability, and can be used for relatively well separating polar drugs such as uridine, thymine, beta-thymidine, adenosine, dihydroxyinosine, sulfanilamide, sulfathiazole, sulfapyridine, sulfamethoxypyridazine and the like.

Description

technical field [0001] The invention relates to a chromatographic filler and a preparation method thereof, in particular to a fluorine-containing liquid chromatography filler for polar drug separation and a preparation method thereof, belonging to the technical field of chromatography fillers. Background technique [0002] In recent years, with the continuous development of the biomedical and health industry, drug separation and analysis is very important to ensure the safety and effectiveness of drugs. At present, the C18 column-based reversed-phase chromatography separation mode is widely used in the separation of weak and moderately polar compounds, and is known as the gold standard for drug separation and analysis. However, when the C18 column is used for the separation and analysis of more polar compounds, it often faces problems such as low resolution. [0003] In order to solve the separation problem of strongly polar compounds, researchers have developed a fluorine-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/28B01J20/30B01D15/08
CPCB01J20/286B01J20/103B01J20/28021B01D15/08B01J2220/52B01J2220/54
Inventor 宋志花朱瑞瑞王玉朦刘金秋王英豪林文宫琬晴王志霞
Owner YANTAI UNIV
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