Solid-phase extraction bag and preparation method and application thereof
A solid phase extraction agent and extraction technology, which is applied in the field of chemical detection, can solve problems that have not been reported, and achieve the effects of low cost, low detection limit and good accuracy
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Embodiment 1
[0074] The synthesis of embodiment 1 solid-phase extractant
[0075] (1) Synthesis of carbon microspheres by one-step high-temperature hydrolysis-hydrothermal synthesis
[0076] 16g of glucose was dissolved in 80mL of water, placed in a 100mL reactor with temperature control at 170°C for 8 hours, and cooled to 80°C for 3 hours. The black liquid is centrifuged-washed, circulated for more than 3 times, the centrifugal speed is 3500rpm, and the centrifugation time is 10min, and the water and ethanol are used as detergents for repeated washing to obtain carbon microspheres with a particle size of 400nm.
[0077] (2) Immerse carbon microspheres in acrylic acid solution to increase active sites
[0078] Put 13g of carbon microspheres obtained in step (1) into 100mL of 5% acrylic acid, disperse ultrasonically for 10min, bathe in water at 60°C for 2 hours, and dry at room temperature for 5h to obtain modified carbon microspheres.
[0079] (3) Polyaniline-coated carbon microspheres b...
Embodiment 2
[0083] The preparation of embodiment 2 solid-phase extraction bag
[0084] The solid-phase extraction package consists of an extraction, salting-out package and an adsorption purification package:
[0085] (1) Mix sodium chloride, anhydrous sodium sulfate, and ammonium sulfate uniformly in a mass ratio of 1:2:4 to obtain extraction and salting-out package 1.
[0086] (2) Mix sodium chloride, anhydrous sodium sulfate, and ammonium sulfate uniformly in a mass ratio of 1:4:2 to obtain extraction and salting-out package 2.
[0087] (3) Take the polyaniline@carbon microspheres bag prepared in Example 1 to obtain the adsorption purification bag.
[0088] The extraction and salting-out package and the adsorption purification package are packaged independently.
Embodiment 3
[0089] The adsorption residual analysis (content) detection of mycotoxin in the Chinese medicinal material of embodiment 3
[0090] (1) Sample pretreatment
[0091] Five kinds of Chinese herbal medicines: Shengjianqu, Bitter Almond, Safflower, Eucommia, and Baiben’er were selected as samples, and the collected samples were vacuum-dried at 80°C for 6 hours. After drying, they were pulverized by a high-speed pulverizer, and the powder was sieved (0.3mm sieve hole) , the quartering method is used to obtain a homogeneous sample;
[0092] Weigh 10.0g homogeneous sample, add 40mL of 1% citric acid-acetonitrile extraction solvent, vortex mix for 2min, soak at room temperature for 20min, oscillate for 30min, ultrasonically extract at 50°C for 30min; accurately weigh 35.8g hydrogen phosphate dodecahydrate Add disodium to 1000mL deionized water, ultrasonically stir and dissolve, then adjust the pH of the solution with phosphoric acid to obtain a sulfate buffer; add an appropriate amoun...
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