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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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005]However, the current mixed-mode chromatographic stationary phase is difficult

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

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Example Embodiment

[0036] Example 1 Preparation of mixed mode silica gel stationary phase

[0037] In this example, 3-mercaptopropyltriethoxysilane and octyltriethoxysilane are used as silane coupling agents to prepare 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, mechanically stirred, drop 3 drops of triethylamine. N 2 After heating and refluxing for 24 hours under protection, it was cooled, filtered, and washed with toluene, methanol and acetone successively twice. Vacuum dry at 70°C for 5 hours and then set aside.

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

Example Embodiment

[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, mechanically stirring, drop 3 drops of triethylamine. N 2 After heating and refluxing for 30 hours under protection, cooling, filtering, and washing with toluene, methanol and acetone in sequence. Vacuum dry at 70°C for 5 hours and then set aside.

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

Example Embodiment

[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, mechanically stirring, drop 3 drops of triethylamine. N 2 After heating and refluxing for 30 hours under protection, cooling, filtering, and washing with toluene, methanol and acetone in sequence. Vacuum dry at 70°C for 5 hours and then set aside.

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

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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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