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Novel glucosyl group ionic liquid stationary phase and application thereof

An ionic liquid, glucose-based technology, applied in the liquid separation of solid adsorbents, sugar derivatives, sugar derivatives, etc., can solve the problems of limited stability and single target analyte, and achieve the effect of excellent separation and analysis performance.

Inactive Publication Date: 2016-08-31
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] In order to solve the problem that the imidazole-based ionic liquid functionalized high-performance liquid chromatography stationary phase prepared by the prior art has limited stability and a single target analyte under conditions such as solvents and buffers, the present invention provides a new glucose-based ion Liquid stationary phase to achieve high-efficiency separation and analysis of similar biomolecular compounds

Method used

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  • Novel glucosyl group ionic liquid stationary phase and application thereof
  • Novel glucosyl group ionic liquid stationary phase and application thereof
  • Novel glucosyl group ionic liquid stationary phase and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Preparation of Sil-GLU Glucose-based Ionic Liquid Stationary Phase

[0032] Steps:

[0033] The three steps of the preparative synthesis were carried out in the same vessel.

[0034] ①Weigh 8 mM meglumine and GPTMS of the same mole, dissolve both in 80 mL of methanol at the same time, heat to 70 °C, and reflux for 12 h.

[0035] ② After the reflux for 12 h in step ① is completed, continue to add 10 mM methyl iodide in the same reaction vessel, then continue to heat to 70 ° C, and further reflux for 12 h.

[0036] ③ Add magnets for mechanical stirring, and add methanol homogenate (20 mL) of silica gel (3 g), stir evenly, suspend for 24 h, heat to 70 °C, and reflux for 12 h.

[0037] ④ Filter the milky white suspension obtained in step ③, wash it with methanol / water solution (volume ratio 1 / 1) after filtering, and finally the filtered product is the new glucose-based ionic liquid stationary phase Sil-GLU. Sil-GLU was placed in a vacuum oven, dried for 8 h at 80 °C, and...

Embodiment 2

[0039] Preparation of Sil-GLU Glucose-based Ionic Liquid Stationary Phase

[0040] Steps:

[0041] The three steps of the preparative synthesis were carried out in the same vessel.

[0042] ① Weigh 7.5 mM meglumine and GPTMS of the same mole, dissolve both in 75 mL of methanol at the same time, heat to 70 °C, and reflux for 13 h.

[0043] ②After the reflux for 12 h in step ①, continue to add 9 mM methyl iodide in the same reaction vessel, then continue heating to 70°C, and further reflux for 13 h.

[0044] ③ Add magnets for mechanical stirring, and add methanol homogenate (20 mL) of silica gel (3.2 g), stir evenly, suspend for 24 h, heat to 70 °C, and reflux for 13 h.

[0045] ④ Filter the milky white suspension obtained in step ③, wash it with methanol / water solution (volume ratio 1 / 1) after filtering, and finally the filtered product is the new glucose-based ionic liquid stationary phase Sil-GLU. Sil-GLU was placed in a vacuum oven, dried for 10 h at 80 °C, and stored in ...

Embodiment 3

[0047] Preparation of Sil-GLU Glucose-based Ionic Liquid Stationary Phase

[0048] Steps:

[0049] The three steps of the preparative synthesis were carried out in the same vessel.

[0050] ①Weigh 8 mM meglumine and GPTMS of the same mole, dissolve both in 80 mL of methanol at the same time, heat to 75 °C, and reflux for 12 h.

[0051] ②After the 12 h reflux in step ①, continue to add 10 mM methyl iodide in the same reaction vessel, then continue to heat to 75°C, and further reflux for 12 h.

[0052] ③ Add magnets for mechanical stirring, and add methanol homogenate (20 mL) of silica gel (3 g), stir evenly, suspend for 24 h, heat to 75 °C, and reflux for 12 h.

[0053] ④ Filter the milky white suspension obtained in step ③, wash it with methanol / water solution (volume ratio 1 / 1) after filtering, and finally the filtered product is the new glucose-based ionic liquid stationary phase Sil-GLU. Sil-GLU was placed in a vacuum oven, dried for 8 h at 80 °C, and stored in amber via...

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Abstract

The invention discloses a novel glucosyl group ionic liquid stationary phase. The stationary phase is prepared through the method comprising the steps that firstly, acid treatment is performed on the surface of porous spherical silica gel for chromatography, washing is performed till to neutral, silica gel surface excitation is achieved, then, then, an epoxy loop opening reaction is utilized for enabling meglumine to react with gamma-(2,3-epoxy propyl) propyl trimethoxy silane, methyl iodide is added, the synthesized glucosyl group ionic liquid is modified on the surface of a silica gel carrier, and high efficiency and high selectivity of the stationary phase are achieved. The invention further discloses application of the novel glucosyl group ionic liquid stationary phase on the aspect of nucleoside separation.

Description

technical field [0001] The invention relates to a novel glucose-based ionic liquid stationary phase and an application thereof, belonging to the field of high-performance liquid chromatography stationary phases. Background technique [0002] Currently, most ionic liquid-functionalized HPLC stationary phases are synthesized based on imidazole or pyridine cations. Glucose-based ionic liquids, a new class of ionic liquids, have been reported to have remarkable extraction properties for halogenated hydrocarbons and deoxyribonucleic acid (DNA). The glucose segment of the glucose-based ionic liquid is highly hydrophilic and can be used in hydrophilic interaction chromatography (HILIC). Contents of the invention [0003] In order to solve the problem that the imidazole-based ionic liquid functionalized high-performance liquid chromatography stationary phase prepared by the prior art has limited stability and a single target analyte under conditions such as solvents and buffers, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/286B01J20/30B01D15/30C07H19/073C07H19/067C07H19/167
CPCB01J20/286B01D15/305C07H1/06C07H19/073
Inventor 王旭生蒋琼梁晓静王磊郭勇
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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