Preparation method for ionic liquid silica gel capillary monolithic column stationary phase

A technology of capillary monolithic column and ionic liquid, which is applied in the field of chromatographic stationary phase, can solve the problems that the ionic liquid silica gel capillary monolithic column has not been reported in literature, etc., and achieve the effect of simple preparation method, mild reaction conditions and good reproducibility

Inactive Publication Date: 2012-06-20
GUANGXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the properties of self-assembly and exchange on the surface of gold nanoparticles are widely used in the modification of various carriers, but there is no literature report on the preparation of ionic liquid silica gel capillary monolithic columns.

Method used

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  • Preparation method for ionic liquid silica gel capillary monolithic column stationary phase
  • Preparation method for ionic liquid silica gel capillary monolithic column stationary phase
  • Preparation method for ionic liquid silica gel capillary monolithic column stationary phase

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] (1) Synthesis of gold nanoparticles

[0036] Measure 100mL of deionized water into a 250mL round-bottomed flask, heat to reflux with stirring until boiling, add 1mL of 1% (w / w) chloroauric acid, then continue heating until the solution boils violently, quickly add 2.5mL of 1% (w / w) sodium citrate, keep the solution boiling for 15min. During this period the color of the solution changed from gray to wine red. Cool naturally to room temperature after removing the heat source, and store at 4°C for later use. The gold nanoparticles are spherical in shape, and the particle size is about 15nm. Refer to figure 1 : TEM image;

[0037] (2) Synthesis of ionic liquids

[0038] Weigh 5g of methimazole into a three-necked round-bottomed flask equipped with a condenser tube, add 30mL of absolute ethanol, and then pass nitrogen gas, remove the air in the bottle, heat to 60°C with an oil bath, stir and reflux, and then slowly 7mL of 1-bromobutane was added dropwise, and a reddish-...

Embodiment 2

[0048] Using 7 mL of 1-bromododecane instead of 1-bromobutane, the procedure in Example 1 was followed to prepare a dodecyl imidazolyl silica gel capillary monolithic column.

Embodiment 3

[0050] The ionic liquid silica gel capillary monolithic column prepared in Example 1 has a total cut length of 39 cm and an effective length of 29.6 cm. The buffer solution of v / v) is the mobile phase, under the conditions of applied voltage 22kV and detection wavelength 254nm, the aniline compounds are separated, and the corresponding peaks are respectively t 0 . Thiourea 1. o-phenylenediamine, 2. o-nitroaniline, 3. aniline, 4. p-toluidine, 5. menaphthylamine. Its spectrum is as image 3 shown.

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Abstract

The invention provides a preparation method for a novel ionic liquid silica gel capillary monolithic column stationary phase. The novel ionic liquid silica gel capillary monolithic column stationary phase is prepared by a sol-gel and gold nanoparticle surface functionalization technology. According to the characteristic that the gold nanoparticles have strong affinity on a ligand containing sulfydryl, amino and cyan and the excellent properties of the gold nanoparticles, the ionic liquid and the silica gel monolithic column, the prepared ionic liquid silica gel capillary monolithic column hasthe advantages of high selectivity, high column efficiency, simplicity in preparation, wide application rang and the like. An electropositive imidazole ring and an analyte have various kinds of interactions comprising a hydrophobic interaction, an ion exchange interaction, a pi-pi interaction, a dipolar interaction and a weak hydrophilic interaction and also have multiple action mechanisms such as a hydrogen bond action and the like. Therefore, the preparation method can be applied to separation analysis on hydrophobic neutral compounds, alkaline organic compounds, polar compounds and inorganic anions. The ionic liquid silica gel capillary monolithic column stationary phase can serve as a capillary electrochromatography or capillary liquid chromatography fixed phase and has good application potential in the field of separation science.

Description

technical field [0001] The invention relates to a chromatographic stationary phase, in particular to a preparation method of a novel ionic liquid silica gel capillary monolithic column stationary phase. Background technique [0002] As a new chemical material, ionic liquid has the advantages of good thermal stability, low flammability, non-volatile and low toxicity, etc. It has been widely used in various fields and has attracted increasing attention of many researchers. In recent years, the application of ionic liquids in separation analysis has been reported in relevant literature, such as Li et al. (Jing Li, Haifeng Han, Qing Wang, Xia Liu, Shengxiang Jiang, J. Sep. Sci. 2011 , 34, 1555-1560) prepared capillary electrophoresis columns coated with poly-1-vinyl-3-butylimidazolium bromide salt. Qiu et al. (Hongdeng Qiu, Shengxiang Jiang, Xia Liu, Liang Zhao, J. Chromatogr. , 2006, 1116 , 46-50) prepared imidazolyl-based anion-exchange stationary phases for HPLC analysi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J20/283B01J20/30
Inventor 叶芳贵陆俊宇张爱珠赵书林
Owner GUANGXI NORMAL UNIV
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