A kind of preparation method of outer surface hydrophilic hybrid composite solid phase extraction adsorbent
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A hybrid composite, hydrophilic technology, applied in chemical instruments and methods, other chemical processes, etc., can solve the problems of high impurity content in the separated sample liquid, easy adsorption of biological macromolecules, low separation and adsorption efficiency, etc., and shorten the reaction time. Time, not easy to shrink and deform, easy to separate and remove
Inactive Publication Date: 2015-12-30
HEBEI UNIVERSITY
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[0004] The purpose of the present invention is to provide a method for preparing a hydrophilic hybrid composite solid-phase extraction adsorbent on the outer surface, so as to solve the problem that the outer surface of the solid-phase extraction material prepared by the existing method is easy to adsorb biological macromolecules, has poor rigidity, and is easy to shrink. Deformation, poor thermal stability, high swelling degree, low separation and adsorption efficiency, high impurity content in the separated sample liquid, and poor detection accuracy
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Embodiment 1
[0027] (1) Measure 2.25mL of acetonitrile, 0.6mL of styrene, 0.2mL of divinylbenzene and 1.176mL of vinyltriethoxysilane into a three-necked flask, add 0.10g of azobisisobutyronitrile, and dissolve it by ultrasonic , continuously filled with nitrogen for 30 minutes, refluxed at 65°C, a large number of white particles appeared after about 1 hour; continued to stir for 2 hours, and obtained the organic part solution A;
[0028] (2) Add 2.95mL tetraethyl orthosilicate, 4.525mL ethanol and 0.1mL concentrated hydrochloric acid into the Erlenmeyer flask at the same time, in a constant temperature shaker at 60°C (at any other temperature between 40-60°C) Shake for 1 hour to obtain a clear solution, and obtain the inorganic part solution B;
[0029] (3) After adding solution B to solution A dropwise, continue to stir and reflux at 65°C for 3h. That is to obtain a milky white turbid liquid, put the generated milky white turbid liquid evenly into a centrifuge tube and centrifuge at 140...
Embodiment 2
[0033] In step (2) of Example 1, 1.63 mL of tetraethyl orthosilicate, 3.02 mL of ethanol, and 0.07 mL of concentrated hydrochloric acid were added, and the others were the same as in Example 1 to obtain RAM-HCM2.
Embodiment 3
[0035] In step (2) of Example 1, 4.90 mL of tetraethyl orthosilicate, 9.05 mL of ethanol, and 0.20 mL of concentrated hydrochloric acid were added, and the others were the same as in Example 1 to obtain RAM-HCM3.
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Abstract
The invention relates to a preparation method of a hybrid composite solid-phase extraction adsorbent with a hydrophilic outer surface. The preparation method comprises the following steps: a, adding styrene, divinyl benzene and vinyltriethoxysilane to acetonitrile, then adding azobisisobutyronitrile, carrying out ultrasonication, and refluxing to obtain a solution A; b, mixing ethyl orthosilicate, ethanol and concentrated hydrochloric acid, and oscillating to obtain a solution B; c, dropping the solution B into the solution A, and centrifugalizing to obtain a polymer C; d, mixing methylbenzene solutions of the polymer C and gamma-glycidoxy propyl trimethoxy silane, refluxing, centrifugalizing, washing, and drying; and f, adding perchloric acid, and filtering, washing and drying after the reaction is completed. The hybrid composite solid-phase extraction adsorbent prepared through the method can be used for efficiently absorbing the target object and excluding the biological macromolecule from being absorbed on the surface of the target object, has the advantages of suitability for swelling degree, good heat stability, high adsorption capacity, difficulty in contraction distortion, long service life and the like and is suitable for separating and extracting the tetracyclines antibiotics during drug residue detection.
Description
technical field [0001] The invention relates to a preparation method of an extraction and separation material, in particular to a preparation method of an outer surface hydrophilic hybrid composite solid-phase extraction adsorbent. Background technique [0002] The abuse of veterinary drugs can easily cause the residue of harmful substances in animal source food, which not only causes direct harm to human health, but also has a serious impact on the development of animal husbandry and the export trade of agricultural products in our country. At present, the United States, Japan, the European Union and my country have all stipulated the limits of various drug residues in food of animal origin. Methods for the analysis and determination of drug residues include gas chromatography-mass spectrometry, liquid chromatography-mass spectrometry, high performance liquid chromatography, and capillary electrophoresis. The key step to determine the accuracy and precision of the analysis...
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