Silica matrix chromatogram packing

A chromatographic packing and silica gel matrix technology, which is applied in the field of preparation of silica gel packing for high performance liquid chromatography, can solve the problems of insignificant improvement of tail-capping effect, high device cost, unsatisfactory and the like, and achieves simple post-processing work and time-consuming reaction. Short, high-volume effects

Inactive Publication Date: 2008-08-06
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The equipment used in this method is expensive and inconvenient to operate. Compared with the traditional liquid phase method, the sealing effect is not significantly improved, and it cannot meet the needs of pharmaceutical and other industries for highly inert reversed-phase bonded silica gel chromatography packing.

Method used

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  • Silica matrix chromatogram packing
  • Silica matrix chromatogram packing

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Weigh 20.0g spherical silica gel (BaseLine  Sil, particle size 5μm, specific surface area 250m 2 / g, aperture 100 Ȧ), put it into a three-necked flask, install a condenser, add 200ml of 10% hydrochloric acid aqueous solution, mechanically stir and reflux at 105°C for 12h, repeatedly wash with deionized water until the filtrate is neutral, and vacuum dry at 90°C for 12h .

[0020] Weigh 10.0 g of pretreated dry spherical silica gel, put it into a three-necked flask, install a condenser tube and a drying tube, add 100 ml of dehydrated toluene (treated with activated molecular sieves for more than 12 hours), 1 ml of triethylamine, and octadecyltrimethoxysilane 5ml, under the condition of mechanical stirring, pass through dry nitrogen and heat to toluene reflux, 110 ℃ constant temperature reaction for 6h, stop the reaction, wash with toluene, methanol, methanol-water (1:1, v / v), methanol, acetone successively, Vacuum-dried at 60°C for 12 hours to obtain octadecyl bonded ...

Embodiment 2

[0023] Use the non-inertized octadecyl reversed-phase chromatography silica gel filler prepared in Example 1, and fill it in a 150×4.6mm I.D. stainless steel column tube by homogenization method. The resulting column is used to separate mixture samples. Fig. 1 is the chromatogram of its separation analysis evaluation octadecyl reversed-phase chromatographic stationary phase commonly used mixture, i.e. 1 uracil, 2 pyridine, 3 phenol, and chromatographic condition is as follows: mobile phase, methyl alcohol: water=45: 55 (v / v); flow rate, 1ml / min; column temperature, 25°C; detection wavelength, UV254nm.

Embodiment 3

[0025] Use the highly inert octadecyl reversed-phase silica gel chromatography filler prepared in Example 1, and fill it in a 150×4.6mm I.D. stainless steel column by homogenization method. The resulting column is used to separate mixture samples. Its separation and analysis of Fig. 2 is the chromatogram of evaluation octadecyl reversed-phase chromatographic stationary phase commonly used mixture, i.e. 1 uracil, 2 pyridine, 3 phenol, and chromatographic condition is as follows: mobile phase, methyl alcohol: water=45: 55 (v / v); flow rate, 1ml / min; column temperature, 25°C; detection wavelength, UV254nm.

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Abstract

The invention relates to a preparation method of inert alkyl reversed phase silica gel chromatographic filler, which belongs to the technical field of high performance liquid phase chromatography. The invention comprises the following steps: step 1 of getting silica gel particles with hydroxyl on the surface through acidification pretreatment of silica gel matrix particles; step 2 of hydroxylation of the silica gel matrix particles, and getting the alkyl reversed phase silica gel filler by making use of corresponding alkyl silicane reagents and by adopting a method of liquid phase reaction to make surface alkyl treatment to the acidification pretreated silica gel particles with the hydroxy; step 3 of inert treatment of the alkyl silica gel matrix filler, and putting the prepared dry alkyl reversed phase silica gel filler into an autoclave with a certain volume, adding a certain amount of silicane terminated reagents and sealing the autoclave to make seal terminated reaction in the inert gas atmosphere to obtain the highly inert alkyl reversed phase silica gel chromatographic filler. In appropriate chromatographic conditions, the filler prepared in the invention can be effectively used in the separation analysis of acidic, neutral and basic compounds.

Description

technical field [0001] The invention relates to a preparation method of silica gel filler for high performance liquid chromatography. Specifically, the gas-solid phase chemical bonding reaction is used to inert the reversed-phase bonded phase silica gel filler, thereby eliminating or reducing the tailing phenomenon of basic compounds on the silica gel matrix stationary phase, and improving the column efficiency and efficiency of chromatographic separation. Separation. Background technique [0002] High-performance liquid chromatography (HPLC) is a technique for separating multi-component samples by using the difference in the partition coefficient of compounds between the mobile phase and the stationary phase. Since its inception in the 1970s, HPLC methods have been widely used in the fields of chemistry, pharmacy, clinical, biology, environment, quality inspection, etc. due to their fast, efficient, easy-to-automate operation and high-throughput sample processing. It is t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/283B01J20/286
Inventor 万谦宏郭志强陈磊
Owner TIANJIN UNIV
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