Solid-phase extraction column for enriching and purifying deoxidized nivalenol
A technology of deoxynivalenol and solid phase extraction column, which is applied in the preparation of test samples, chemical instruments and methods, solid adsorbent liquid separation, etc., can solve complex operations, a large amount of waste, and time-consuming Power and other issues
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Embodiment 1
[0019] Take corn randomly collected in the market, crush it and sieve it, take three 20mL centrifuge tubes, accurately weigh 2±0.01g, add DON standard solution, so that the DON content in the sample is 100μg / kg, 200μg / kg, 1000μg / kg respectively , adding 10 mL of acetonitrile-water solution (84:16, V / V) for ultrasonic extraction for 1 hour, centrifuging, and collecting the extract.
[0020] Preparation of solid-phase extraction column: Accurately weigh 1 g of silica gel (200-300 mesh, purchased from China Pharmaceutical Shanghai Chemical Reagent Company), 0.5 g of neutral alumina, (100-200 mesh, purchased from China Pharmaceutical Shanghai Chemical Reagent Company), Florisil 0.5g, (100-200 mesh, purchased from China Pharmaceutical Shanghai Chemical Reagent Co., Ltd.), was successively loaded into a 5mL polypropylene solid-phase extraction container with a sieve plate in the lower layer to make the surface of each layer flat, and finally in Florisil. Add a sieve plate (diameter:...
Embodiment 2
[0031] Take corn randomly collected in the market, crush it and sieve it, take three 20mL centrifuge tubes, accurately weigh 2±0.01g, add DON standard solution to one of them, make the concentration of DON in the extract 100μg / kg, add 10mL acetonitrile -Aqueous solution (84:16, V / V) was ultrasonically extracted for 1 hour, centrifuged, and the extract was collected.
[0032] The solid phase extraction column was as described in Example 1.
[0033] Positive control solution preparation: activate the self-made purification column with 5mL methanol, pass 5mL of the spiked corn sample extract through the solid-phase extraction column, elute with 10mL methanol, collect the eluate, dry it with nitrogen at 45°C, and dry it with 1mL methanol-water solution (20:80 , V / V) redissolved, passed through a 0.22 μm filter membrane, and detected and analyzed.
[0034] Preparation of sample solution: take another 5mL corn sample extract and pass it through the solid phase extraction column, dr...
Embodiment 3
[0043] The liquid chromatography-mass spectrometry (LC-MS / MS) method in Example 2 was used to detect and calculate the recovery rate and method sensitivity after passing through the solid-phase extraction purification column at three addition levels in Example 1.
[0044] Experimental results:
[0045] By testing, the recovery rates of the three groups of post-column solutions in Example 1 are 90.5 ± 1.8%, 98.4 ± 2.1% and 106.9 ± 4.4%, respectively, and the sensitivity of the post-column solution in Example 1 is 10 μg / kg, very The sensitivity of the method is greatly improved (the sensitivity of DON in the unpassed solution is lower than 100 μg / kg), which meets the requirements of relevant domestic and foreign standards.
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