Condensed ring aromatic hydrocarbon based amide embedded type liquid chromatography stationary phase synthesis method

An aromatic hydrocarbon amide and liquid chromatography technology, which is applied in the field of a new approach for the synthesis of a condensed ring aromatic hydrocarbon amide embedded type liquid chromatography stationary phase, can solve the problems of complicated process, cumbersome process, many synthesis steps, etc., and achieves reduction of synthesis time and raw materials. cost effect

Active Publication Date: 2019-05-03
JIANGSU HANBON SCI & TECH CO
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] In summary, it can be seen that C. H. Lochmuller et al. have too many synthesis steps, and the process is complex and cumbersome; Feng Yuqi et al. used two methods that are three-step synthesis of pyrenyl-modified chromatographic stationary phases, and the synthesis steps are also relatively cumbersome.

Method used

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  • Condensed ring aromatic hydrocarbon based amide embedded type liquid chromatography stationary phase synthesis method
  • Condensed ring aromatic hydrocarbon based amide embedded type liquid chromatography stationary phase synthesis method
  • Condensed ring aromatic hydrocarbon based amide embedded type liquid chromatography stationary phase synthesis method

Examples

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Embodiment 1

[0029] (1) Homogeneous synthesis of amide-embedded silanes

[0030] At room temperature, add pyrenylbutyric acid (8 mmol) and 3-isocyanatopropyltriethoxysilane (10 mmol) into a flask containing 60 mL of tetrahydrofuran, and then add the catalyst 4-dimethylaminopyridine in one go , continue to stir for 5 hours and then heat to reflux for 30 minutes. The solvent was removed by rotary evaporation, and then recrystallized from a benzene / n-hexane mixed solvent to obtain a tan solid, which was the synthesized pyrenylamide-embedded silane.

[0031] (2) Surface bonding modification

[0032] Disperse 5 g of vacuum-dried spherical silica at 140°C in toluene as a solvent, then add 8 mmol of pyrenylamide intercalation silane reagent synthesized, mechanically stir and reflux for 24 hours, cool and filter, and then wash the obtained solid with toluene, Wash with tetrahydrofuran, chloroform, ethanol, ethanol / water and methanol, and finally dry under vacuum at 120°C.

Embodiment 2

[0033] Embodiment 2: Change the 3-isocyanate group propyl triethoxysilane in embodiment 1 into 3-isocyanate group butyl triethoxysilane or other carbon chain length isocyanate silane, can prepare corresponding under the same conditions Pyrenylamide embedded stationary phase for liquid chromatography.

Embodiment 3

[0034] Example 3: The pyrenyl butyric acid in Example 1 was changed to anthracenyl butyric acid, the stationary phase matrix spherical silica was changed to spherical titanium oxide, and the rest of the conditions were the same to prepare an anthracenyl amide embedded liquid chromatography stationary phase .

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Abstract

The invention relates to a novel condensed ring aromatic hydrocarbon based amide embedded type liquid chromatography stationary phase synthesis method. According to the condensed ring aromatic hydrocarbon based amide embedded type liquid chromatography stationary phase synthesis method, condensed ring aromatic hydrocarbon based carboxylic acids and isocyanate silane reagents are taken as raw materials, amide type silane reagents are synthesized, simple purification is adopted, modification onto stationary phase matrix surfaces is realized so as to synthesize a condensed ring aromatic hydrocarbon based amide embedded type liquid chromatography stationary phase. The properties such as bonding density, aromatic and hydrophobic compound separation effect, charge transfer capacity, and isomer selectivity are tested, it is shown that better aromatic compound selectivity and shape selectivity are achieved.

Description

technical field [0001] The method of the invention relates to a new way to synthesize a condensed ring aromatic hydrocarbon base amide embedded liquid chromatography stationary phase. Background technique [0002] The stationary phase of high performance liquid chromatography is generally prepared by condensing different chlorosilanes or alkoxysilanes with silanols on the surface of silica gel to form siloxanes, and the bonding units are connected to silica gel with covalent chemical bonds. The properties of organic bonded phases, such as bonded body size, bonded phase density, thickness, configuration, mobility, and arrangement, have a major impact on the interaction between analyte and stationary phase. Among the various chemically bonded stationary phases, the alkyl bonded stationary phase, especially the C18 bonded silica gel, is the most successful reversed-phase stationary phase so far, and is well-known in the chromatographic field. [0003] Despite the excellent chr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C233/65C07C231/12C07F7/18B01J20/286
Inventor 韩海峰张明亮范大双张大兵张加栋
Owner JIANGSU HANBON SCI & TECH CO
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