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Olig-(polyethylene glycol) bonding silica-gel stationary phase and method for preparing the same

A technology of oligoethylene glycol and bonded silica gel, applied in the field of chromatographic stationary phase, can solve problems such as the influence of separation performance, and achieve the effects of good separation selectivity, simple and reliable preparation process, and novel structure

Active Publication Date: 2008-10-01
浙江华谱新创科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although hydrophobicity is the main factor determining the separation selectivity, the flexibility of the chain, the length of the chain may have an important impact on the separation performance
Design and preparation of new reversed-phase chromatography stationary phase from the perspective of molecular structure similarity has not been reported in the literature

Method used

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  • Olig-(polyethylene glycol) bonding silica-gel stationary phase and method for preparing the same
  • Olig-(polyethylene glycol) bonding silica-gel stationary phase and method for preparing the same
  • Olig-(polyethylene glycol) bonding silica-gel stationary phase and method for preparing the same

Examples

Experimental program
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Effect test

Embodiment 1

[0038]In a 1000ml three-necked flask, add 500ml of anhydrous DMF, 45mmol (about 10ml) of 3-chloropropyltriethoxysilane, 60mmol (about 4.0g) of sodium azide, and then add 3.0mmol of sodium iodide (about 0.5g) As a catalyst, react at 80°C for 24h, then add 20g of spherical silica gel particles with a particle size of 5μm, react at 80°C for another 24h, and then wash with dichloromethane, ethanol, water, and acetone twice, each time 200ml, 60 °C and vacuum-dried for 12 hours to obtain (3-propyl)azido silica gel.

[0039] Add 100ml of dry THF and 10g of tetrapolyethylene glycol into a 250ml three-necked flask, cool to -5°C, add 1.5g of sodium hydride under stirring conditions, react for 15 minutes at -5~0°C, and then add 5.6ml with a volume concentration of 80% propargyl bromide in toluene solution, react at -5~0°C for 2 hours, rise to room temperature and continue to react for 2 hours. The reaction system was subjected to simple post-treatments such as filtration and concentrati...

Embodiment 2

[0043] The difference from Example 1 is that tripolyethylene glycol is used instead of tetrapolyethylene glycol, and another kind of oligoethylene glycol stationary phase (OEG-3) can be obtained according to the synthesis steps of Example 1, the structure of which is The structure is:

[0044]

Embodiment 3

[0046] The difference from Example 1 is that polyethylene glycol with an average molecular weight of 400 is used instead of tetrapolyethylene glycol, and another kind of oligoethylene glycol stationary phase (OEG400) can be obtained according to the synthesis steps of Example 1, and the structure is Its structure is:

[0047]

[0048] Wherein n=8~9.

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Abstract

The invention relates to a liquid chromatography stationary phase, with the bonded phases of oligomeric polyethyleneglycol molecules (polymerization degree of 2-10); in the structure of the invention, X is -OCH3 or -OCH2CH3; wherein n is equal to 2-10. The invention also provides a preparation method of the liquid chromatography stationary phase. The preparation method is characterized in that an azide group is firstly led in the surface of silica gel; 1, 3-ring addition reaction of the azid group and the alkyne group which is also the click chemistry is then carried out for 24-72 hours under the temperature of 20-80 DEG C; the cyclodextrin where the alkyne group or azid group is decorated is bonded onto the surface of the silica gel. The stationary phase prepared by the invention has novel structure and high column efficiency and has extremely good complementarity with routine reverse phase stationary phase (such as ODS, etc.).

Description

technical field [0001] The invention relates to a chromatographic stationary phase, specifically an oligoethylene glycol stationary phase and a preparation method thereof; it is an oligoethylene glycol bonded stationary phase using click chemistry as a bonding reaction method. technical background [0002] High performance liquid chromatography is a separation analysis and separation preparation method widely used in modern scientific research, and stationary phase is one of its core technologies. C18 is currently the most widely used HPLC stationary phase, which can separate most weakly polar and medium polar organic compounds in the reversed phase chromatography mode. However, the separation of C18 stationary phase mainly relies on a single hydrophobic force, and the separation selectivity is limited, for example, the separation selectivity for difficult-to-separate substance pairs such as positional isomers is very limited. In addition, the development of modern life sci...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286
Inventor 梁鑫淼郭志谋张永平丰加涛徐青雷爱文
Owner 浙江华谱新创科技有限公司
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