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Liquid chromatogram silica gel stationary phase and preparation method and application thereof

A liquid chromatography and stationary phase technology, applied in the field of liquid chromatography silica gel stationary phase and its preparation and use, can solve the problems of complex stationary phase preparation method, and achieve the effects of simple preparation method, good reproducibility and wide application

Inactive Publication Date: 2013-05-22
WELTECH TECH WUHAN CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation method of this stationary phase is relatively complicated, so it is necessary to develop a low-cost, simple and highly selective mixed-mode reversed-phase-weak anion-exchange silica gel stationary phase for the simultaneous separation and analysis of multivitamin mixtures

Method used

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  • Liquid chromatogram silica gel stationary phase and preparation method and application thereof
  • Liquid chromatogram silica gel stationary phase and preparation method and application thereof
  • Liquid chromatogram silica gel stationary phase and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Example 1 Preparation of hydrophobic-weak anion exchange mixed mode silica gel stationary phase.

[0023] Add 2.5 g of activated silica gel to 60 ml of treated anhydrous toluene, then add 0.99 g of n-octyltriethoxysilane and 0.80 g of 3-aminopropyltriethoxysilane (total moles of silane coupling agent 0.0072, molar ratio 1:1), stirring mechanically, drop 3 drops of triethylamine. N 2 After heating under reflux for 20 h under protection, it was cooled, filtered, washed several times with toluene, methanol and acetone in turn, and dried in vacuum at 60°C for 5 h before use.

Embodiment 2

[0024] Example 2 Preparation of hydrophobic-weak anion exchange mixed mode silica gel stationary phase.

[0025] Add 2.5 g of activated silica gel to 60 ml of treated anhydrous toluene, then add 1.59 g of n-octyltriethoxysilane and 0.32 g of 3-aminopropyltriethoxysilane (total moles of silane coupling agent 0.0072, molar ratio 4:1), stirring mechanically, drop 3 drops of triethylamine. N 2 After heating under reflux for 20 h under protection, it was cooled, filtered, washed several times with toluene, methanol and acetone in turn, and dried in vacuum at 60°C for 5 h before use.

Embodiment 3

[0026] Example 3 Preparation of hydrophobic-weak anion exchange mixed mode silica gel stationary phase.

[0027] Add 2.5 g of activated silica gel to 60 ml of treated anhydrous toluene, then add 1.77 g of n-octyltriethoxysilane and 0.18 g of 3-aminopropyltriethoxysilane (total moles of silane coupling agent 0.0072, molar ratio 8:1), stirring mechanically, drop 3 drops of triethylamine. N 2 After heating under reflux for 20 h under protection, it was cooled, filtered, washed several times with toluene, methanol and acetone in turn, and dried in vacuum at 60°C for 5 h before use.

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Abstract

The invention relates to a liquid chromatogram silica gel stationary phase and a preparation method and application thereof. The silica gel stationary phase is connected with an amino silane coupling agent and an n-octyl silane coupling agent on silica gel. The preparation method uses anhydrous toluene as a solvent, activated silica gel flows back with the amino silane coupling agent and the n-octyl silane coupling agent in the present of triethylamine or reacts at the room temperature for 1 hour to 25 hours to obtain the liquid chromatogram silica gel stationary phase. N-octyl and amino are bonded on the surface of the silica gel to enable the stationary phase to have the function of water repellent and weak anion exchange. The stationary phase can be used for separation of water-solubility and fat-soluble vitamin compound, can provide multiple reservation mechanisms for analyzed articles and is good in separation effect. In addition, the mixed type stationary phase is low in price of raw material, simple in preparation method and good in application prospect.

Description

technical field [0001] The invention relates to a reverse-phase-weak anion-exchange silica gel stationary phase, its preparation method and its application in the separation of water-soluble and fat-soluble vitamins. Background technique [0002] High-performance liquid chromatography is the most important component of contemporary chromatographic technology. It is the fastest-growing and most widely used separation and analysis technology in modern analytical chemistry. It plays an important role in many fields such as chemistry, medicine, food, environmental protection, biochemistry and industrial preparation. increasingly important role. In high performance liquid chromatography systems, chromatographic stationary phases have always been the core of chromatographic analysis, and the development of highly selective chromatographic stationary phases is the most active frontier research field in modern high performance liquid chromatography. Although a variety of chromatogr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/286
Inventor 冯钰锜彭西甜
Owner WELTECH TECH WUHAN CO LTD
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