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Synthesis And Application Of High Efficiency Boric Acid Grafting Material

Posted on:2020-09-13Degree:MasterType:Thesis
Country:ChinaCandidate:L L YingFull Text:PDF
GTID:2381330590998222Subject:Drug Analysis
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Objectives: The cis-dihydroxy-containing substances are mostly biologically active molecules such as glycoproteins,nucleic acids,polysaccharides,catechols and so on.However,its concentration in the living body is generally low,and there are high concentrations of interfering components coexisting therewith.Existing studies have shown that boron affinity materials can achieve extraction and enrichment of cis-dihydroxyl species.1.For the first time,this study applied boron affinity material to capillary solid phase microextraction technology to apply it to the extraction of trace cis-diol molecules in beverages.2.In order to improve the specificity and binding constant of boron affinity,the "teamed boronate affinity" molecular group is introduced to realize the formation of boron-nitrogen coordination in the molecule,so as to achieve a large sample size of cis-diols under physiological pH conditions.High specific recognition of small cis-diols and protein macromolecules.Method: 1.This paper firstly coated a porous silica gel coating on the inner wall of the capillary column,then grafted epoxy on the porous silica coating,and under alkaline conditions,using epoxy and polyethyleneimine(PEI).The ring opening reaction of the amino group,grafting a layer of PEI on the epoxy group,and finally using the reaction of PEI with p-formylbenzeneboronic acid to fix the boric acid on the surface of the PEI to obtain a modified porous silica gel coating grafted boric acid open capillary extraction column.The optimal conditions modified capillary column prepared for the extraction and enrichment of cis-diol molecules in beverages.2.This paper firstly prepares the amino magnetic sphere by hydrothermal method,and then grafts the boric acid group on the surface of the obtained amino magnetic sphere.The optimal ratio of each input substance is optimized,and the boric acid grafted magnetic microsphere prepared by the formula first adsorbs and enriches the cis-diols substance in the food,and then enriches the glycated hemoglobin in the blood sample.Results: 1.The method used in this paper successfully prepared a highly efficient porous silica gel coated boric acid grafted solid phase microextraction capillary column.The modified boron affinity capillary column has a maximum adsorption capacity of cis-diols of 170 ?g/m.Simultaneous sample loading and recovery experiments were carried out on four cis-diol molecules and one non-cis-diol in beverages.The recoveries of the four cis-diols were all above 80%,and the error coefficient less than 8%,and the recovery rate of the non-cis-diols is not more than 3%.2.In this paper,boron affinity magnetic microspheres with specific adsorption capacity were successfully prepared by experimental optimization.The prepared magnetic microspheres simultaneously carry out sample loading and recovery experiments on seven cis-diol molecules and two non-cis-diols in food.The experimental results show that they are different in different actual sample systems.The adsorption capacity of alcohol molecules is different.Under better actual conditions,the recovery rate can be greater than 80%,the error coefficient is less than 8%,and the recovery rate of the non-cis-diol substance ferulic acid is less than 30%.Kaempferol can be completely adsorbed and recovered.When it is used together with ion exchange method to enrich glycated hemoglobin in blood samples,the buffer salt solution is used much less than the ion exchange method,but the purity of pure glycated hemoglobin is less than that of ion exchange.Conclusion: This paper can prove that the boron affinity principle has a good specific adsorption effect on cis-diol molecules,and its adsorption performance on small molecules is stronger than that on biological macromolecules.The boron affinity capillary column has strong adsorption specificity and large adsorption amount for the cis-diol small molecules,and the extraction and enrichment of the target substance is better in the actual sample.By introducing boron affinity magnetic nano-microspheres of the "teamed boronate affinity" molecular group,the adsorption of most of the cis-diol small molecules in the actual sample can be realized,and the specific adsorption of the biomacromolecular glycated hemoglobin can be realized.
Keywords/Search Tags:Boron affinity, Cis-dihydroxyl, In-tube solid phase microextraction, Magnetic nanoparticles, Glycated hemoglobin
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