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Silica gel fixed phase of mixed model as well as preparation method and application thereof

A mixed mode, stationary phase technology, applied in chemical instruments and methods, other chemical processes, ion exchange, etc., can solve the problems of difficult wide application, difficult development of chromatographic stationary phase, and few available types, and achieve simple and heavy-duty preparation methods. good effect

Inactive Publication Date: 2010-09-15
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005]However, the current mixed-mode chromatographic stationary phase is difficult to develop, and there are few available types, so it is difficult to be widely used

Method used

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  • Silica gel fixed phase of mixed model as well as preparation method and application thereof
  • Silica gel fixed phase of mixed model as well as preparation method and application thereof
  • Silica gel fixed phase of mixed model as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Example 1 Preparation of Mixed Mode Silica Gel Stationary Phase

[0037] In this example, 3-mercaptopropyltriethoxysilane and octyltriethoxysilane were used as silane coupling agents to prepare a mixed-mode silica gel stationary phase. The preparation process is as follows figure 1 shown.

[0038] Preparation steps:

[0039] 1. Preparation of octyl-mercapto bonded silica gel: Take 3.00g of vacuum-dried silica gel in a 250ml three-necked flask, add 120ml of treated anhydrous toluene, 1.28g of 3-mercaptopropyltriethoxysilane and 0.75g of octyltriethoxysilane, stirring mechanically, was added dropwise with 3 drops of triethylamine. N 2 After heating under reflux for 24 hours under protection, it was cooled, filtered, and washed twice with toluene, methanol and acetone. Vacuum dried at 70°C for 5 h before use.

[0040] 2. Preparation of octyl-sulfonate bonded silica gel: Take 3.00 g of octyl-mercapto bonded silica gel in a 100 mL three-necked flask, add 50 ml of 30% hy...

Embodiment 2

[0041] Example 2 Preparation of Mixed Mode Silica Gel Stationary Phase

[0042]1. Preparation of octyl-mercapto bonded silica gel: Take 3.00g of vacuum-dried silica gel in a 250ml three-necked flask, add 120ml of treated anhydrous toluene, 1.28g of 3-mercaptopropyltriethoxysilane and 1.50g of octyltriethoxysilane, stirring mechanically, was added dropwise with 3 drops of triethylamine. N 2 After heated under reflux for 30 hours under protection, it was cooled, filtered, and washed with toluene, methanol and acetone in turn. Vacuum dried at 70°C for 5 h before use.

[0043] 2. Preparation of octyl-sulfonate bonded silica gel: Take 3.00 g of octyl-mercapto bonded silica gel in a 100 mL three-necked flask, add 50 ml of 25% hydrogen peroxide solution and 12 mL of methanol, stir mechanically, add two drops of concentrated sulfuric acid, After reacting at 28°C for 20 h, it was filtered and washed with distilled water and methanol successively. Vacuum dried at 70°C for 5 h before...

Embodiment 3

[0044] Example 3 Preparation of Mixed Mode Silica Gel Stationary Phase

[0045] 1. Preparation of octyl-mercapto bonded silica gel: Take 3.00g of vacuum-dried silica gel in a 250ml three-necked flask, add 120ml of treated anhydrous toluene, 0.64g of 3-mercaptopropyltriethoxysilane and 1.50g of octyltriethoxysilane, stirring mechanically, was added dropwise with 3 drops of triethylamine. N 2 After heated under reflux for 30 hours under protection, it was cooled, filtered, and washed with toluene, methanol and acetone in turn. Vacuum dried at 70°C for 5 h before use.

[0046] 2. Preparation of octyl-sulfonate bonded silica gel: Take 3.00 g of octyl-mercapto bonded silica gel in a 100 mL three-necked flask, add 50 ml of 35% hydrogen peroxide solution and 20 mL of methanol, stir mechanically, add two drops of concentrated sulfuric acid, After reacting at 30° C. for 10 h, filter and wash with distilled water and methanol successively. Vacuum dried at 70°C for 5 h before use.

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Abstract

The invention discloses a silica gel fixed phase of a mixed model, which is the silica gel fixed phase in the mixed model of hydrophobic / strong cation exchange. The silica gel fixed phase is connected with the compounds having structures shown as formulae (I) and (II) on a silica gel surface. The silica gel fixed phase is obtained through bonding a silane coupling agent containing octyl and hydrosulphonyl to an activated silica gel with a hydroxyl and oxidizing hydrosulphonyl carried on the surface, and oxidizing the sulfydryl into sulfonic acid group by using oxydol. When the silica gel as fillers is prepared into a chromatographic column, the silica gel can effectively separate multiple substances. The silica gel fixed phase has simple preparation, favorable reproducibility and excellent application prospect.

Description

technical field [0001] The invention relates to a chromatographic solid phase material, specifically a mixed-mode silica gel stationary phase, and also relates to a preparation method and application of the silica gel stationary phase. 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, the development of high-selectivity chromatographic stationary phases has always been the core of chromatographic analysis, and it is also the most active frontier research field of modern high-performance liquid chromatography. Although a variety of chromatographic fi...

Claims

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Application Information

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IPC IPC(8): B01J20/289B01J20/30B01D15/08
Inventor 冯钰琦彭西甜
Owner WUHAN UNIV
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