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Liquid phase chromatogram filler and method for synthesizing same

A liquid chromatography, normal phase technology, applied in the field of preparation of high performance liquid chromatography filling materials, can solve the problems of complex separation mechanism, poor stability and reproducibility, etc., and achieve superior chromatographic performance, strong adsorption and separation capacity, column Efficient effect

Active Publication Date: 2011-10-05
上海迪柯马科技发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the two types of chromatographic columns currently used have disadvantages such as poor stability and reproducibility, and complicated separation mechanisms.

Method used

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  • Liquid phase chromatogram filler and method for synthesizing same
  • Liquid phase chromatogram filler and method for synthesizing same
  • Liquid phase chromatogram filler and method for synthesizing same

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preparation example Construction

[0037] The synthesis method of the high-performance liquid chromatography packing of the present invention uses silica gel particles as a substrate, uses a polar fluorophenyl silylating reagent, and adopts a liquid phase reaction method to carry out surface treatment on the silica gel particles to obtain a bonded silica gel packing. After the material is further inertized, a new type of high performance liquid chromatography filler is prepared. The specific operation steps are as follows:

[0038] Synthesis of trimethoxysilylpropyl-2,3,4,5,6-pentafluorobenzamide: Weigh a certain amount of aminopropyltrimethoxysilane, put it into a three-necked flask, add dry toluene, Add appropriate acid chloride dropwise to triethylamine, pass through dry inert gas, and stir mechanically for 16 hours. The crude material was purified by distillation.

[0039] Synthesis of polar fluorophenyl silica gel: Add activated silica gel into the reactor, pass through dry inert gas, add xylene and pyri...

Embodiment 1

[0044] (1) Weigh 18 grams of aminopropyltrimethoxysilane, put it into a three-necked flask, install a condenser tube and a dropping funnel, feed dry argon, add 50 milliliters of dry toluene, 13 grams of triethylamine, drop 2 , 23 grams of 3,4,5,6-pentafluorobenzoyl chloride, mechanically stirred for 16 hours, and the crude material was purified by distillation.

[0045] (2) Weigh 10.0 grams of spherical silica gel (5 μm, 120 300m 2 / g, the metal impurity content is less than 30ppm), vacuum dried at 120°C for 24 hours, put it into the reactor after cooling, feed dry argon, install a condenser tube and a drying tube, add 50 milliliters of xylene, 4 milliliters of pyridine, and mechanically stir Evenly, then add 7 grams of silane synthesized in step (1), heat to reflux and react at a constant temperature for 24 hours, stop the reaction, vacuum filter, and use successively toluene, methylene chloride, acetone, methanol-water (1: 1, v / v), methanol wash.

[0046] (3) Take 10.0 ...

Embodiment 2

[0049] (1) Weigh 10.0 grams of spherical silica gel (5 μm, 120 300m 2 / g, the metal impurity content is less than 30ppm), vacuum dried at 120°C for 24 hours, put it into the reactor after cooling, feed dry argon, install a condenser tube and a drying tube, add 50 milliliters of xylene, 4 milliliters of pyridine, and mechanically stir Evenly, then add 3 grams of aminopropyltrimethoxysilane, heat to reflux and react at a constant temperature for 24 hours, stop the reaction, vacuum filter, and use toluene, dichloromethane, acetone, methanol-water (1:1, v / v), washing with methanol, and drying at 80° C. for 24 hours.

[0050] (2) Take by weighing 10.0 grams of dry aminopropyl bonded silica gel, put it into a reactor, feed dry argon, install a condenser tube and a drying tube, add 50 milliliters of toluene, 4 grams of triethylamine, drop 2, 8 grams of 3,4,5,6-pentafluorobenzoyl chloride, mechanically stirred for 16 hours. Stop the reaction, vacuum filter, wash with toluene, dic...

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Abstract

The present invention discloses a one-class polarity fluobenzene based high-efficiency liquid phase chromatogram filler and a method for synthesizing the same. The silica gel surface of the chromatogram filler is bonded with polarity fluobenzene based functional groups, and the chemical structure of the filler is shown as the general formula(I):R<1>=C6F5-, C6F5CONH-, C6F5CONHC6H4-, or C6F5CONHC6H4O-; alpha is between 0 to 30, and beta is 0, 1 or 2; R<2> is a C1 to C20 alkyl group, cycloalkyl group, heterocyclic ring alkyl group or phenol group; and X is a halogen, alkoxy group, acyloxy group or amino group. The chromatogram filler has two liquid phase separation modes-positive phase and negative phase, and can be used in 0 to 100 percent of water or 0 to 100 percent of organic mobile phase and also be effectively used for separation analysis of acid, neutral and alkali compounds.

Description

technical field [0001] The invention belongs to the technical field of preparation of high-performance liquid chromatography packing materials, and in particular relates to a high-performance liquid chromatography packing with two separation modes of normal phase and reverse phase and a preparation method thereof. The chromatographic packing can be used in various organic synthesis and pharmaceutical industries Separation and purification of component organic compounds. Background technique [0002] Liquid chromatography is a widely used analytical chromatography technique. The basic principle is to separate the components in the mixture through the separation effect of the mobile phase and the stationary phase, more specifically, to separate the ions or molecules dissolved in the solvent. The column is used to fill the stationary phase, and the mobile phase carries the mixture through the stationary phase. Components in the sample that have a stronger affinity to the stat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/30B01J20/286
Inventor 李广庆马国辉
Owner 上海迪柯马科技发展有限公司
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