Ionic liquid bonded silica gel used for enriching and purifying shellfish toxins and preparation method for ionic liquid bonded silica gel
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
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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 0.0368gmL -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) adding the N-phenylbenzimidazole prepared in step (1) to a concentrati...
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, the...
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 AUQALOADER698 (Shimadzu Corporation) was added to the instrument configuration.
[0050] Enrichment and purification of shellfish toxins in seawater
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