Ionic liquid-bonded silica gel for enrichment and purification of phenols and preparation method thereof

A technology of ionic liquid and bonded silica gel, which is applied in the direction of chemical instruments and methods, ion exchange, ion exchange regeneration, etc., can solve the problems of numerous extraction and purification steps, time-consuming and labor-intensive, few separation and purification components, etc., and achieve good enrichment Purification effect, improvement of detection sensitivity, effect of eliminating matrix interference

Active Publication Date: 2018-11-02
YELLOW SEA FISHERIES RES INST CHINESE ACAD OF FISHERIES SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the commonly used commercial solid-phase extraction columns currently have the following problems: the interaction mode with the extraction object is single, and the separation and purification components are few. Various, time-consuming and labor-intensive, and the use of a large amount of organic reagents at the same time causes serious environmental pollution; in addition, conventional solid-phase extraction columns cannot be used repeatedly, and the cost is high
Due to the complex environment and biological sample matrix, many interference substances, and the content of phenols is only trace and ultra-trace (10 -9 ) level, which brings great difficulties to rapid pretreatment and quantitative analysis
Most of the commonly used commercial solid-phase extraction columns (MAX) are in anion exchange mode. It is difficult to achieve good results at the same time when enriching and purifying various phenolic hormones. Multiple different types of small columns are required to extract separately, which is time-consuming, laborious and expensive.

Method used

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  • Ionic liquid-bonded silica gel for enrichment and purification of phenols and preparation method thereof
  • Ionic liquid-bonded silica gel for enrichment and purification of phenols and preparation method thereof
  • Ionic liquid-bonded silica gel for enrichment and purification of phenols and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A method for preparing ionic liquid-bonded silica gel used for the enrichment and purification of phenolic substances in seawater and shellfish, the specific steps are as follows:

[0026] (1) At room temperature, add alkenylimidazole at a concentration of 0.50 g mL -1 The toluene solution of γ-chloropropylmethyldiethoxysilane is stirred evenly; the molar ratio of γ-chloropropylmethyldiethoxysilane to alkenylimidazole is 1:1, and the reaction system is Reflux under nitrogen atmosphere and stop after 48h; After three extractions with dichloromethane, dry over anhydrous sodium sulfate, remove the solvent by rotary evaporation at room temperature, and finally dry in vacuum to obtain a light yellow viscous liquid (silyl alkenyl imidazole ionic liquid); the yield is about 85%.

[0027] The synthetic route is as follows:

[0028]

[0029] 1 H-NMR (DMSO, without TMS; 600MHz; δppm): 9.68(s, 1H, NCHN), 7.52-7.79(m, 5H, PhH), 7.47(t, 2H, NCHCN), 4.11(t, 2H, NCH 2 C),1.78(...

Embodiment 2

[0035] The ionic liquid-bonded silica gel prepared in Example 1 was used to make a solid-phase extraction column for enriching and purifying phenolic substances in shellfish.

[0036] details as follows:

[0037] Solid Phase Extraction Cartridge Filling

[0038] The column tube volume of the solid phase extraction column is 1mL, the column tube material is polypropylene, the inlet and outlet sieve plate is made of high-purity polyethylene material (diameter 6.4mm, pore size 20um, thickness 1.5mm), and the internal solid phase extraction filler is selected from this The ionic liquid bonded silica gel synthesized in Invention Example 1 (60 mg filler, particle size 40-60 um). First put the outlet sieve plate at the bottom of the empty column tube, then load the ionic liquid bonded silica gel layer, press the inlet sieve plate on it, and finally wash and fill it with methanol reagent, and ensure that after all the small columns are filled, the packing height remains ( 5±0.05) mm...

Embodiment 3

[0048] The ionic liquid bonded silica gel prepared in Example 1 was used to make a solid phase extraction column for enriching and purifying phenolic substances in seawater.

[0049] Solid Phase Extraction Cartridge Filling

[0050] As in Example 2.

[0051] Instrument configuration

[0052] Agilent1100 High Performance Liquid Chromatography (Agilent, USA), equipped with UV detector; Phenomenex Kinetex Biphenyl chromatographic column (5μm, 4.6mm×250mm); fully automatic sample loading device AUQA LOADER 698 (Shimadzu); XW-80A type vortex mixing Instrument (Shanghai Medical University Instrument Factory); Milli-Q ultrapure water instrument (Millipore, USA); Thermo Sorvall Biofuge Primo centrifuge (Thermo Fisher Scientific, USA).

[0053] Instrument conditions

[0054] Column temperature: 35°C; Flow rate: 1.1mL / min; Injection volume: 10μL; Mobile phase: Acetonitrile-water (1:1); UV absorption wavelength: 230nm.

[0055] Enrichment and purification of phenols in seawater

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Abstract

The invention relates to ionic liquid bonded silica gel used for enriching and purifying phenol substances in seawater and shells. The ionic liquid bonded silica gel is obtained by carrying out reaction on a toluene solution of polyvinylsilylimidazole chloride salt and activated silica gel powder in reflux under a nitrogen atmosphere. The ionic liquid bonded silica gel provided by the invention has the technical advantages that (1) a polyvinylsilylimidazole chloride salt bonded silica gel material is prepared for the first time, and is reacted with a target object through hydrophobic and ion exchange modes; compared with a common ionic liquid loaded silica gel material and a conventional ionic liquid bonded silica gel material, the target of multi-component enriching and purification in a sample can be realized, and the defect that a separation target is single is changed; and (2) a solid-phase extraction small column filled by the ionic liquid bonded silica gel has relatively good repeatability, is simple to operate and relatively low in cost, and can be easily industrialized.

Description

technical field [0001] The invention relates to the technical field of ionic liquid for solid phase extraction and its preparation, in particular to an ionic liquid-bonded silica gel used for enrichment and purification of phenols in seawater and shellfish and a preparation method thereof. Background technique [0002] Solid Phase Extraction (Solid Phase Extraction, SPE) is widely used in the sample pretreatment process due to its simple operation, good repeatability, and high enrichment rate. Commercial solid phase extraction columns can be divided into normal phase extraction, reverse phase extraction, ion exchange extraction and adsorption extraction according to the different properties of the adsorbent. The separation, purification and enrichment of sample components can be achieved by using force and hydrogen bonding, etc. The main purpose is to reduce the interference of impurities and improve the detection ability of trace components. However, the commonly used comm...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/286B01J20/30B01J20/22B01D15/08G01N30/06G01N30/08
CPCB01D15/08B01J20/103B01J20/22B01J20/286B01J2220/46B01J2220/4806B01J2220/4812G01N30/06G01N30/08G01N2030/062
Inventor 孙晓杰谭杰李兆新邢丽红付树林王联珠翟毓秀
Owner YELLOW SEA FISHERIES RES INST CHINESE ACAD OF FISHERIES SCI
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