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A kind of preparation method of glycosyl functionalized imidazole type ionic liquid stationary phase

An ionic liquid and imidazole-based technology, which is applied in the field of preparation of glycosyl-functionalized imidazole-based ionic liquid stationary phase, can solve the problems of single target analyte and limited stability, and achieve high separation efficiency, resistance to organic solvents, Apply a wide range of effects

Active Publication Date: 2017-12-29
ZHENGZHOU UNIV
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In summary, in order to overcome the deficiencies of the prior art problems, the invention provides a preparation method of a sugar-based functionalized imidazole-type ionic liquid stationary phase, which solves the problem that the functionalized imidazole-based ionic liquid high-performance liquid chromatography stationary phase is in a solvent The problem of limited stability and single target analyte under conditions such as buffer solution and buffer solution can achieve high-efficiency separation and analysis of similar biomolecular compounds

Method used

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  • A kind of preparation method of glycosyl functionalized imidazole type ionic liquid stationary phase
  • A kind of preparation method of glycosyl functionalized imidazole type ionic liquid stationary phase
  • A kind of preparation method of glycosyl functionalized imidazole type ionic liquid stationary phase

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Embodiment 1

[0033] Such as figure 1 Shown, a kind of preparation method of glycosyl functionalized imidazole type ionic liquid stationary phase, operate according to the following steps:

[0034] Step 1: Heat 3 g of silica gel with concentrated hydrochloric acid to reflux for 4 hours, wash with water until neutral, and dry in vacuum at 120°C for 6 hours to obtain surface-activated silica gel;

[0035] Step 2: Weigh 50mM D-gluconolactone and N-(3-aminopropyl)imidazole in equivalent moles, dissolve the two in 250ml ethanol at the same time, heat to 80°C, reflux for 24h, and place in the refrigerator Set aside for one day to obtain N-imidazolyl propyl glucamide;

[0036] Step 3: Mix and dissolve 6mM N-imidazolyl propyl glucamide and equimolar 3-isocyanatopropyl trimethoxysilane in 50ml ethanol, reflux for 2 days, carry out methylation reaction, and generate N-trimethyl Silylpropyl-N'-glucamidopropylimidazolium + ion;

[0037] Step 4: Add magnets to the solution obtained in Step 3 for mech...

Embodiment 2

[0040] A preparation method of a glycosyl functionalized imidazole-type ionic liquid stationary phase is carried out according to the following steps:

[0041] Step 1: Heat 3 g of silica gel with concentrated hydrochloric acid to reflux for 4 hours, wash with water until neutral, and dry in vacuum at 120°C for 6 hours to obtain surface-activated silica gel;

[0042] Step 2: Weigh 50mM D-gluconolactone and N-(3-aminopropyl)imidazole in equivalent moles, dissolve the two in 250ml ethanol at the same time, heat to 80°C, reflux for 24h, and place in the refrigerator Set aside for one day to obtain N-imidazolyl propyl glucamide;

[0043]Step 3: Weigh 6mM N-imidazolyl propyl glucamide and equimolar 3-isocyanate propyltrimethoxysilane, mix and dissolve in 50ml ethanol, and reflux for 3 days to generate N-trimethylsilyl propyl -N'-glucamidopropyl imidazolium + ion;

[0044] Step 4: Add magnets to the solution obtained in Step 3 for mechanical stirring, and add 20ml of methanol homog...

Embodiment 3

[0047] Such as figure 1 Shown, a kind of preparation method of glycosyl functionalized imidazole type ionic liquid stationary phase, operate according to the following steps:

[0048] Step 1: Heat 2.5 g of silica gel with concentrated hydrochloric acid to reflux for 5 hours, wash with water until neutral, and dry in vacuum at 120°C for 6 hours to obtain surface-activated silica gel;

[0049] Step 2: Weigh 40mM D-gluconolactone and N-(3-aminopropyl)imidazole in equivalent moles, dissolve the two in 200ml ethanol at the same time, heat to 75°C, reflux for 24h, and place in the refrigerator Set aside for one day to obtain N-imidazolyl propyl glucamide;

[0050] Step 3: Weigh 8mM N-imidazolyl propyl glucamide and equimolar 3-isocyanate propyl trimethoxysilane, mix and dissolve in 60ml ethanol, and reflux for 2 days to generate N-trimethylsilyl propyl -N'-glucamidopropyl imidazolium + ion;

[0051] Step 4: Add magnets to the solution obtained in Step 3 for mechanical stirring, a...

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Abstract

The invention provides a preparation method of a glycosyl-functionalized imidazole ionic liquid stationary phase. The method comprises the steps of: firstly preparing activated silica methanol homogenate for standby use; dissolving D-glucolactone and N-(3-amino propyl) imidazole in ethyl alcohol to obtain N-imidazole propyl glucosamide; mixing the N-imidazole propyl glucosamide with 3-isocyanate propyl trimethoxy silane, and dissolving the mixture in ethyl alcohol to obtain N-trimethylsilyl propyl-N'-glucosamide propylimidazole+ iodide ion solution; and then adding the silica homogenate in the solution and heating to obtain an N, N'-trimethoxy propyl glucosamide imidazole ionic liquid bonded silica gel chromatographic stationary phase. The glycosyl-functionalized imidazole ionic liquid stationary phase chromatographic packing material has excellent physical structure of the silica matrix and special chromatographic performance of the functionalized glycosyl, has relatively strong separation performance for biological molecular compounds, and has a stable separation effect; and the chromatographic packing material has the characteristics of organic solvent resistance, acid resistance, high temperature resistance and high separation efficiency.

Description

technical field [0001] The invention relates to the technical field of high-performance liquid chromatography stationary phase, in particular to a preparation method of a sugar-based functionalized imidazole-type ionic liquid stationary phase. Background technique [0002] At present, most of the ionic liquid-functionalized HPLC stationary phases are based on imidazoles or pyridinium cations. The present invention is inspired by the synthesis of glucose-based ionic liquids. Through a simple glycosylation bonding reaction, sugar groups and imidazole-type Ionic liquids are organically combined to produce a new imidazole ionic liquid silica gel stationary phase based on glycosyl, and the obtained glycosyl imidazole functionalized stationary phase is used for the evaluation of analytes in HILIC mode. Similar stationary phases of glucose-based ionic liquids have been reported in the literature, such as: glucosyl quaternary ammonium surface-immobilized ionic liquid silica gel stat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/286B01J20/30B01D15/36C07H23/00C07H1/00
CPCB01D15/36B01D15/361B01D15/368B01J20/286C07H1/00C07H23/00Y02P20/54
Inventor 蒋琼王旭生邱红灯杜慧芳袁雪生吴宁鹏张书胜
Owner ZHENGZHOU UNIV
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