磁性固相萃
发布时间：2019-05-15 03:06
【摘要】：在化学分析工作中,样品前处理是一个最常见且十分重要的问题。作为出现于21世纪分离富集领域的革命性技术,磁性固相萃取(Magnetic solid-phase extraction,MSPE)受到了社会的广泛关注。MSPE技术,是以磁性或可磁化的材料作为吸附剂的一种新型样品前处理技术,它是将磁性吸附剂分散到样品溶液中进行吸附,使样品能够与吸附剂接触,萃取过程简单,避免了繁琐的操作程序,可在短时间内实现大体积样品中待测组分的吸附和萃取,同时,操作过程中有机溶剂的使用量减少,也避免对环境的污染,此外在加磁场作用下,待测组分可以随磁性吸附剂快速分离,不仅避免了繁琐的后处理操作,也有效的避免了样品基质中杂质的干扰。作为MSPE技术的核心,磁性固相萃取材料的开发与制备一直是研究者关注的重点,尝试并进一步拓展MSPE技术的应用范围,近年来,针对于新型磁性固相萃取的开发和制备,受到了越来越多科研工作者的关注,特别是在食品检测、环境污染等方面。在本论文中,采用自由基聚合的方法,以氨基酸衍生物为主要功能单体,我们设计并合成了针对于食品复杂基质中有害目标物的新型磁性固相萃取材料,即食品防腐剂和植物激素苯氧乙酸类化合物,并考察了其吸附性能,具体的研究内容如下所述:1.制备了聚(苯乙烯-co-L-苯丙氨酸甲基丙烯酰氯)修饰的磁性纳米颗粒,并将其作为磁性固相萃取吸附剂用于复杂样品饮料中防腐剂苯甲酸钠的分离分析。在材料制备过程中,通过自由基聚合,将功能单体L-苯丙氨酸甲基丙烯酰氯和苯乙烯修饰于磁性纳米颗粒表面。与其他两种防腐剂尼泊金丙酯和山梨酸钾相比,所合成吸附材料对苯甲酸钠具有较好的选择性,其中,吸附剂对目标物的吸附容量为6.08±0.31 mg/g。此外,所制备的吸附材料对于苯甲酸钠表现出较快的键合速率:5分钟之内即可达到最大吸附容量的85%。进一步,我们将所制备的吸附材料应用于饮料中防腐剂苯甲酸钠的分析中,在接下来的工作中,通过进一步的单体比例优化,所发展材料具有较好的应用前景。2.采用自由基聚合的方法,以聚氨基酸为功能单体,偶氮二异丁腈为引发剂,磁性纳米颗粒为基质,制备了对复杂样品豆芽中两种常见植物激素,2,4-二氯苯氧乙酸(2,4-D),4-氯苯氧乙酸(4-CPA),有吸附效能的新型磁性固相吸附材料。考察了其对2,4-D和4-CPA的吸附性能,探讨了其吸附动力学、吸附等温线及选择性,并将其应用于豆芽中2,4-D和4-CPA的分离富集研究中。结果表明:所制备的聚氨基酸功能化的磁性纳米颗粒对2,4-D和4-CPA具有较高的吸附容量(吸附量分别为39.82 mg/g,29.02mg/g),以及较好的选择吸附性能;作为吸附剂,能够实现对实际复杂样品豆芽中2,4-D和4-CPA的分离分析。
[Abstract]:Sample pretreatment is one of the most common and important problems in chemical analysis. As a revolutionary technology in the field of separation and enrichment in the 21st century, magnetic solid phase extraction (Magnetic solid-phase extraction,MSPE) has been widely concerned by the society. It is a new sample pretreatment technology, which uses magnetic or magnetized materials as adsorbents. It distributes magnetic adsorbents into the sample solution for adsorption, so that the samples can be in contact with the adsorbents, and the extraction process is simple. The tedious operation procedure can be avoided, and the adsorption and extraction of the components to be tested in the large volume sample can be realized in a short period of time. At the same time, the use of organic solvents in the operation process is reduced, and the pollution to the environment is also avoided. In addition, under the action of adding magnetic field, The components to be tested can be separated rapidly with magnetic adsorbents, which not only avoids the tedious post-treatment operation, but also effectively avoids the interference of impurities in the sample matrix. As the core of MSPE technology, the development and preparation of magnetic solid phase extraction materials have always been the focus of researchers. Try and further expand the application range of MSPE technology. In recent years, the development and preparation of new magnetic solid phase extraction. It has been paid more and more attention by more and more researchers, especially in food detection, environmental pollution and so on. In this paper, a new magnetic solid phase extraction material for harmful targets in complex food matrix was designed and synthesized by free radical polymerization with amino acid derivatives as the main functional monomer. That is, food preservatives and plant hormones phenoxyacetic acid compounds, and their adsorption properties were investigated. The specific research contents are as follows: 1. Poly (styrene-co-L- phenylalanine methacrylic chloride) modified magnetic nanoparticles were prepared and used as magnetic solid phase extraction adsorbents for the separation and analysis of sodium benzoate, a preservative in drinks with complex samples. In the process of material preparation, the functional monomers L-phenylalanine methacrylic chloride and styrene were modified on the surface of magnetic nanoparticles by free radical polymerization. Compared with the other two preservatives, Nipagin propyl ester and potassium sorbate, the synthesized adsorption materials have better selectivity to sodium benzoate, in which the adsorption capacity of the adsorbents for the target is 6.08 卤0.31 mg/g.. In addition, the prepared adsorption material shows a faster bonding rate for sodium benzoate: 85% of the maximum adsorption capacity can be reached within 5 minutes. Furthermore, we applied the prepared adsorption material to the analysis of sodium benzoate, a preservative in beverage. In the next work, through further optimization of monomer ratio, the developed material has a good application prospect. 2. Using polyamino acid as functional monomer, azodiisobutyrile as initiator and magnetic nanoparticles as matrix, two common plant hormones, 2, 4-dichlorophenoxyacetic acid (2, 4 脳 D), were prepared by free radical polymerization with polyamino acid as functional monomer, azodiisobutyrile as initiator and magnetic nanoparticles as matrix. 4-chlorophenoxyacetic acid (4-CPA), a new magnetic solid phase adsorption material with adsorption efficiency. The adsorption properties of 2, 4 脳 D and 4-CPA were investigated, and their adsorption kinetics, adsorption isotherm and selectivity were discussed. The adsorption kinetics, adsorption isotherm and selectivity were discussed and applied to the separation and enrichment of 2, 4 脳 D and 4-CPA in soybean sprouts. The results show that the prepared polyamino acid functionalized magnetic nanoparticles have higher adsorption capacity (adsorption capacity 39.82 mg/g,29.02mg/g) and better selective adsorption performance for 2, 4 脳 D and 4-CPA, respectively. As an absorbent, the separation and analysis of 2, 4 D and 4-CPA in complex bean sprouts can be realized.
【学位授予单位】：山东农业大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O657.72;TS207.3
[Abstract]:Sample pretreatment is one of the most common and important problems in chemical analysis. As a revolutionary technology in the field of separation and enrichment in the 21st century, magnetic solid phase extraction (Magnetic solid-phase extraction,MSPE) has been widely concerned by the society. It is a new sample pretreatment technology, which uses magnetic or magnetized materials as adsorbents. It distributes magnetic adsorbents into the sample solution for adsorption, so that the samples can be in contact with the adsorbents, and the extraction process is simple. The tedious operation procedure can be avoided, and the adsorption and extraction of the components to be tested in the large volume sample can be realized in a short period of time. At the same time, the use of organic solvents in the operation process is reduced, and the pollution to the environment is also avoided. In addition, under the action of adding magnetic field, The components to be tested can be separated rapidly with magnetic adsorbents, which not only avoids the tedious post-treatment operation, but also effectively avoids the interference of impurities in the sample matrix. As the core of MSPE technology, the development and preparation of magnetic solid phase extraction materials have always been the focus of researchers. Try and further expand the application range of MSPE technology. In recent years, the development and preparation of new magnetic solid phase extraction. It has been paid more and more attention by more and more researchers, especially in food detection, environmental pollution and so on. In this paper, a new magnetic solid phase extraction material for harmful targets in complex food matrix was designed and synthesized by free radical polymerization with amino acid derivatives as the main functional monomer. That is, food preservatives and plant hormones phenoxyacetic acid compounds, and their adsorption properties were investigated. The specific research contents are as follows: 1. Poly (styrene-co-L- phenylalanine methacrylic chloride) modified magnetic nanoparticles were prepared and used as magnetic solid phase extraction adsorbents for the separation and analysis of sodium benzoate, a preservative in drinks with complex samples. In the process of material preparation, the functional monomers L-phenylalanine methacrylic chloride and styrene were modified on the surface of magnetic nanoparticles by free radical polymerization. Compared with the other two preservatives, Nipagin propyl ester and potassium sorbate, the synthesized adsorption materials have better selectivity to sodium benzoate, in which the adsorption capacity of the adsorbents for the target is 6.08 卤0.31 mg/g.. In addition, the prepared adsorption material shows a faster bonding rate for sodium benzoate: 85% of the maximum adsorption capacity can be reached within 5 minutes. Furthermore, we applied the prepared adsorption material to the analysis of sodium benzoate, a preservative in beverage. In the next work, through further optimization of monomer ratio, the developed material has a good application prospect. 2. Using polyamino acid as functional monomer, azodiisobutyrile as initiator and magnetic nanoparticles as matrix, two common plant hormones, 2, 4-dichlorophenoxyacetic acid (2, 4 脳 D), were prepared by free radical polymerization with polyamino acid as functional monomer, azodiisobutyrile as initiator and magnetic nanoparticles as matrix. 4-chlorophenoxyacetic acid (4-CPA), a new magnetic solid phase adsorption material with adsorption efficiency. The adsorption properties of 2, 4 脳 D and 4-CPA were investigated, and their adsorption kinetics, adsorption isotherm and selectivity were discussed. The adsorption kinetics, adsorption isotherm and selectivity were discussed and applied to the separation and enrichment of 2, 4 脳 D and 4-CPA in soybean sprouts. The results show that the prepared polyamino acid functionalized magnetic nanoparticles have higher adsorption capacity (adsorption capacity 39.82 mg/g,29.02mg/g) and better selective adsorption performance for 2, 4 脳 D and 4-CPA, respectively. As an absorbent, the separation and analysis of 2, 4 D and 4-CPA in complex bean sprouts can be realized.
【学位授予单位】：山东农业大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O657.72;TS207.3
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