Detection method of thyroid inhibitor based on hydrophilic solid-phase extraction
A detection method and solid-phase extraction column technology, which is applied in the field of sample pretreatment and drug detection, can solve the problem of small sample volume, etc., and achieve the effects of simplifying sample pretreatment steps, reducing errors, and improving accuracy
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Embodiment 1
[0027] Example 1: A solid-phase extraction column based on polyethyleneimine-modified hybrid silica gel material was fabricated according to the following steps.
[0028] (1) Preparation of polyethyleneimine-modified hybrid silica gel material
[0029] In a 50 mL plastic centrifuge tube, weigh 160 mg cetyltrimethylammonium bromide, add 2.24 mL tetraethoxysilane, 2.36 mL aminopropyltriethoxysilane, 4.35 mL absolute ethanol, mix After uniform dissolution, 0.64 mL of water was added, and after mixing, it was immediately placed in a 40 °C water bath for 24 h. After the reaction was completed, rinse with 15 mL of methanol and 15 mL of 100 mmol / L phosphate (pH 8.0) for 2 to 3 times, and then add 2 mL of 10% (v / v) dissolved in 100 mmol / L phosphate (pH 8.0 ) glutaraldehyde solution, react at 90 °C for 0.5 h, the color can be observed to turn brown, and then rinse with 15 mL 100 mmol / L phosphate (pH8.0), add 0.625 mL dissolved in 100 mmol / L phosphoric acid Salt (pH 8.0) in 0.05 g / mL ...
Embodiment 2
[0032] Example 2: Using three standard thyroid inhibitors as samples, the concentration of acetonitrile in the sample was optimized.
[0033]The solid-phase extraction column based on polyethyleneimine-modified hybrid silica gel material prepared in Example 1 was used to rinse with 5 mL of acetonitrile and 5 mL of deionized water, and then washed with 5 mL of 98% (v / v) acetonitrile Equilibrium solid-phase extraction column with aqueous solution, dissolve the standards of three thyroid inhibitors in 60%, 70%, 80%, 85%, 90%, 95% and 98% (v / v) acetonitrile aqueous solution, the concentration is 2.0 μg / mL, load 1 mL of the sample, collect the effluent sample, pass through a 0.45 μm filter membrane, and analyze it by hydrophilic interaction chromatography. Chromatographic analysis conditions: the analytical column is Shimadzu Inertsil-NH 2 (4.6×150 mm, 3 μm), the mobile phase was 95% (v / v) acetonitrile aqueous solution, the flow rate was 0.8 mL / min, the injection volume was 20 μL,...
Embodiment 3
[0034] Example 3: Using three standard thyroid inhibitors as samples, the concentration of acetonitrile for elution was optimized.
[0035] The solid-phase extraction column based on polyethyleneimine-modified hybrid silica gel material prepared in Example 1 was used to rinse with 5 mL of acetonitrile and 5 mL of deionized water, and then washed with 5 mL of 98% (v / v) acetonitrile Equilibrate the solid-phase extraction column with aqueous solution, dissolve the standard substances of the three thyroid inhibitors in 98% (v / v) acetonitrile aqueous solution, the concentration is 2.0 μg / mL, load 1 mL of the sample, rinse with 2 mL of pure acetonitrile, and wash with 1 mL of 50%, 60%, 70%, 80% and 90% (v / v) acetonitrile aqueous solution was used for elution, the eluate was collected, passed through a 0.45 μm filter membrane, and detected by hydrophilic interaction chromatography. Chromatographic analysis conditions: the analytical column is Shimadzu Inertsil-NH 2 (4.6×150 mm, 3 μm...
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