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Preparing method for amide-embedded alkyl bonding liquid chromatogram filler

A liquid chromatography and alkyl bond technology, applied in the field of liquid chromatography, can solve the problems of increased cost, complicated operation and the like, and achieve the effects of easy operation, good repeatability and simple steps

Inactive Publication Date: 2016-05-25
JIANGSU HANBON SCI & TECH CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Amide-embedded alkyl stationary phases are usually obtained by condensation between acid chlorides and amino groups, such as octadecanoyl chloride and aminopropyltriethoxysilane, which are dehydrochlorinated to form amides in the presence of acid-binding agents, but this method has many disadvantages, If acid chloride must be used, additional acid-binding agent is required, which increases the cost and is cumbersome to operate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1: Preparation of amide-embedded behenyl-bonded silica gel

[0018] (1) Synthesis of N-(triethoxysilylpropyl)behenylamide

[0019] In an inert gas, preheat 7.17g of 3-isocyanate propyltriethoxysilane to 120°C, divide it into 3 times, and put 9.67g of behenic acid into it at an interval of 15 minutes, and heat it to 160°C after the throwing, and keep After 2h, the reaction product was cooled to 20°C, dissolved in 300mL of n-hexane, dried in vacuo at 40°C for 2h, cooled and crystallized for 2h to obtain 13.2g of N-(triethoxysilylpropyl)behenylamide, producing The rate is about 85%.

[0020] (2) Preparation of amide-embedded docosyl-bonded silica gel

[0021] The activated silica gel was dried under vacuum at 140°C for 6 hours to remove the moisture absorbed by the silica gel. Take 10.0g of silica gel and add it to 120mL of toluene, stir it evenly, and add 7g of N-(triethoxysilylpropyl)behenylamide , heated to reflux, kept for 24h, suction filtered while hot, fo...

Embodiment 2

[0022] Example 2: Preparation of amide-embedded octadecyl-bonded silica gel

[0023] (1) Synthesis of N-(triethoxysilylpropyl)octadecamide

[0024] In an inert gas, preheat 14.34g of 3-isocyanate propyltriethoxysilane to 120°C, divide it into 4 times, put 16.50g of octadecanoic acid into it at intervals of 10min, heat it to 160°C after throwing, and keep it for 3h , after the reaction product was cooled to 25°C, the reaction product was dissolved in 450mL of n-hexane, dried in vacuum at 40°C for 3h, cooled and crystallized for 2h to obtain 25g of N-(triethoxysilylpropyl) octadecanoic acid, with a yield of about 90 %.

[0025] (2) Preparation of amide-embedded octadecyl-bonded silica gel

[0026] The activated silica gel was dried under vacuum at 140°C for 6 hours to remove the moisture absorbed by the silica gel. Take 15.0 g of silica gel and add it to 120 mL of toluene, stir it evenly, add 8 g of N-(triethoxysilylpropyl) octadecylamide, Heat to reflux, keep for 24h, suctio...

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Abstract

The invention provides a preparing method for amide-embedded alkyl bonding liquid chromatogram filler. By means of a grafting technology, 3-isocyanate propyl alkoxy silane and normal saturated fatty acid (C12-C22) are condensed to prepare novel N-(trialkoxy silica propyl) alkyl amide, and then N-(trialkoxy silica propyl) alkyl amide is bonded to silica gel to prepare the novel amide-embedded alkyl bonding liquid chromatogram filler. No solvent, or catalyst or acid-binding agent is used in the whole reaction process, when the synthesized filler serves as the stationary phase, pure water can be used as the mobile phase, no organic solvent is used, and the effect of environmental protection is achieved.

Description

technical field [0001] The invention relates to a preparation method of an amide-embedded alkyl-bonded liquid chromatography filler, which belongs to the field of liquid chromatography. Background technique [0002] Alkyl bonded silica gel has excellent chemical inertness and stability, and its preparation process is convenient and mature. It is the most widely used filler in reversed-phase chromatography. As an extension of conventional alkyl-bonded silica gel, the polar group-embedded alkyl-bonded stationary phase further expands the types and application ranges of reversed-phase chromatography stationary phases, greatly improving the performance of polar analytes, especially basic analytes. separation. [0003] The introduction of polar groups, especially amide groups, was originally intended to mask the adverse effects of residual silanols on basic analytes. Subsequently, researchers found that this type of immobilization is unique in the separation of polar analytes, a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/30
CPCB01J20/286B01J2220/52
Inventor 张明亮韩海峰范大双文卡特尤慧艳张大兵
Owner JIANGSU HANBON SCI & TECH CO
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