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Preparation method of C18 reverse phase silica gel bonded stationary phase

A technology of stationary phase and reverse silica gel, applied in the field of preparation of high performance liquid chromatography packing

Inactive Publication Date: 2015-10-14
HUAIAN CHEM NEW MATERIAL RES CENT DALIAN INST OF CHEM PHYSICS CHINESE ACADEMYOF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Generally speaking, there is still a large gap between the performance of domestic fillers and foreign developed countries.

Method used

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  • Preparation method of C18 reverse phase silica gel bonded stationary phase
  • Preparation method of C18 reverse phase silica gel bonded stationary phase
  • Preparation method of C18 reverse phase silica gel bonded stationary phase

Examples

Experimental program
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Embodiment 1

[0015] (1) Add 50 g of unactivated silica gel and 300 mL of concentrated hydrochloric acid into a 500 mL beaker, stir occasionally, let stand for 24 h, filter, then wash repeatedly with deionized water until the filtrate is neutral, vacuum at 120°C (-0.9 MPa) and dried overnight; (2) Weigh (1) 5 g of pretreated spherical porous silica gel (SPS, particle size 10 μ, pore size 10 nm) into a three-neck flask, add 50 mL of dry toluene, and stir magnetically to make the silica gel Suspended in the solution, then added 2.5 mL of octadecyltrichlorosilane and 1 mL of dried triethylamine, passed through dry nitrogen, and refluxed at 105°C for 24 h. Stop the reaction, filter the product, and wash it thoroughly with dry toluene, toluene, methanol, absolute ethanol and acetone in turn, and dry it under vacuum (-0.9 MPa) at 80°C overnight; (3) Take the product obtained in (2) in a three-necked flask, Add 50 mL of dry toluene, stir magnetically to suspend the silica gel in the solution, then...

Embodiment 2

[0017] (1) Add 50 g of unactivated silica gel and 300 mL of concentrated hydrochloric acid into a 500 mL beaker, stir occasionally, let stand for 24 h, filter, then wash repeatedly with deionized water until the filtrate is neutral, vacuum at 120°C (-0.9 MPa) and dried overnight; (2) Weigh (1) 10 g of pretreated spherical porous silica gel (SPS, particle size 10 μ, pore size 10 nm) into a three-necked flask, add 100 mL of dry toluene, and stir magnetically to make the silica gel Suspended in the solution, then added 5 mL of octadecyltrichlorosilane and 2 mL of dried triethylamine, passed through dry nitrogen, and refluxed at 105°C for 24 h. Stop the reaction, filter the product, wash thoroughly with dry toluene, toluene, methanol, absolute ethanol and acetone in turn, and dry under vacuum (-0.9 MPa) at 80°C overnight. (2) Take the product obtained in (1) in a three-necked flask, add 100 mL of dry toluene, stir magnetically to suspend the silica gel in the solution, then add 3....

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Abstract

The invention discloses a preparation method of an HPLC (high performance liquid chromatography) filler, and particularly relates to a method for bonding octadecyl on the surface of high-purify silica gel. Obtained particles can be used as the filling material of a liquid chromatography column so as to be used for separation and purification of a multi-component organic compound. The preparation method comprises the following specific steps: (1) carrying out acidification treatment on silica gel; (2) carrying out alkylation reaction on Si-OH on the surface of the silica gel by adopting a liquid phase reaction method by utilizing octadecyl trichlorosilane; and (3) carrying out end sealing treatment by using trimethysilyl chloride. Tested by packing a column, the obtained reverse filler is excellent in performance and high in stability compared with a commercial filler.

Description

technical field [0001] The invention relates to the field of preparation methods of high-performance liquid chromatography fillers, in particular to a preparation method of a C18 reversed-phase silica gel bonded stationary phase. Background technique [0002] With the continuous development and improvement of analytical techniques and equipment, liquid chromatography has become one of the indispensable tools for biologists, chemists and medical scientists in scientific research. As the most commonly used bonded phase of liquid chromatography, silica gel has always been one of the hot topics in the field of chromatography packing research. At present, there are many foreign companies researching and developing silica-based liquid chromatography packing materials, and the production technologies of some well-known manufacturers are quite mature. Generally speaking, there is still a big gap between the performance of domestic fillers and foreign developed countries. [0003] ...

Claims

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Application Information

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IPC IPC(8): B01J20/287B01J20/30
Inventor 朱建生汪青王涛
Owner HUAIAN CHEM NEW MATERIAL RES CENT DALIAN INST OF CHEM PHYSICS CHINESE ACADEMYOF SCI
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