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An ionic liquid-bonded silica gel for the enrichment and purification of shellfish toxins and its preparation method

A shellfish toxin and ionic liquid technology, applied in chemical instruments and methods, ion exchange, ion exchange regeneration, etc., can solve the problems of time-consuming and laborious, numerous extraction and purification steps, solid-phase extraction columns cannot be used repeatedly, etc., to achieve improved The effects of detection sensitivity, good enrichment and purification effect, and good design flexibility

Active Publication Date: 2018-05-11
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
Because shellfish toxins contain many functional groups, complex structures, and various components with different properties such as acidic, alkaline, and amphoteric, the commonly used commercial solid-phase extraction columns (MCX or MAX) are mostly anion-exchange or cation-exchange modes. When enriching and purifying multiple shellfish toxins, it is difficult to achieve good results at the same time, and multiple different types of small columns are required for separate extraction, which is time-consuming, laborious and costly, and has become the main bottleneck restricting its accurate quantification.

Method used

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  • An ionic liquid-bonded silica gel for the enrichment and purification of shellfish toxins and its preparation method
  • An ionic liquid-bonded silica gel for the enrichment and purification of shellfish toxins and its preparation method
  • An ionic liquid-bonded silica gel for the enrichment and purification of shellfish toxins and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A method for preparing ionic liquid-bonded silica gel for enrichment and purification of shellfish toxins, the specific steps are as follows:

[0027] (1) At room temperature, add formic acid to a concentration of 0.0368g mL -1 In the concentrated hydrochloric acid suspension of 2-amino-diphenylamine, under nitrogen atmosphere, reflux and stir for 90min, wherein: the molar ratio of 2-amino-diphenylamine to formic acid is: 1:1; then use ammonia water (28%) to adjust the pH to 8; after three extractions with ethyl acetate, drying over anhydrous sodium sulfate, rotary evaporation at room temperature to remove the solvent, and finally vacuum drying to obtain light yellow N-phenylbenzimidazole liquid with a yield of about 85%;

[0028] (2) Soak 40-60 μm silica gel powder in 3mol / L hydrochloric acid for 24 hours, wash it with pure water until neutral, and dry it in vacuum at 120°C for 5 hours;

[0029] (3) The N-phenylbenzimidazole prepared in step (1) will be added to a con...

Embodiment 2

[0031] The ionic liquid bonded silica gel prepared in Example 1 was used to make a solid phase extraction column for enriching and purifying shellfish toxins in shellfish.

[0032] details as follows:

[0033]Solid Phase Extraction Cartridge Filling

[0034] The column tube volume of the solid phase extraction column is 1mL, the column tube is made of polypropylene material, the inlet and outlet sieve plate is made of high-purity polyethylene material (diameter 6.4mm, pore size 20um, thickness 1.5mm), and the inside is filled with solid phase extraction filler The alkenylimidazole polymerized ionic liquid bonded silica gel (filler: 50mg, particle size: 40-60um) synthesized by the present invention is selected. 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, th...

Embodiment 3

[0047] The ionic liquid bonded silica gel prepared in Example 1 was used to make a solid phase extraction column for enriching and purifying shellfish toxins in seawater.

[0048] SPE Cartridge Packing, Instrument Conditions and Instrument Configuration

[0049] Same as Example 2, in addition, an automatic sample loading device AUQA LOADER 698 (Shimadzu Corporation) was added to the instrument configuration.

[0050] Enrichment and purification of shellfish toxins in seawater

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Abstract

The invention relates to ionic liquid bonded silica gel used for enriching and purifying shellfish toxins. N-phenylbenzimidazole is added into a toluene solution of gamma-chloropropylmethyldiethoxysilane, and is evenly stirred; then, reflux reaction is performed under nitrogen atmosphere for 48 hours; activated silica gel is added after cooling, and the reflux reaction is continued for 24 hours. The N-phenylbenzimidazole ionic liquid bonded silica gel material is prepared by the invention for the first time; compared with a common ionic liquid supported silica gel material and a conventional ionic liquid bonded silica gel material, the N-phenylbenzimidazole ionic liquid bonded silica gel material is capable of achieving a goal of enriching and purifying various shellfish toxins in a sample by reacting with a target object through two modes of hydrophobic interaction and ion exchange, so that the defect that isolated objects are single is changed.

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 the enrichment and purification of shellfish toxins 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 commercial solid-...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/286B01J20/30B01J20/22B01D15/08G01N30/88G01N30/08
CPCB01D15/08B01J20/103B01J20/22B01J20/286B01J2220/46B01J2220/4806B01J2220/4812G01N30/08G01N30/88
Inventor 孙晓杰谭杰李兆新丁海燕付树林谭志军翟毓秀
Owner YELLOW SEA FISHERIES RES INST CHINESE ACAD OF FISHERIES SCI
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