【摘要】：在化學分析工作中,樣品前處理是一個最常見且十分重要的問題。作為出現(xiàn)于21世紀分離富集領域的革命性技術(shù),磁性固相萃取(Magnetic solid-phase extraction,MSPE)受到了社會的廣泛關(guān)注。MSPE技術(shù),是以磁性或可磁化的材料作為吸附劑的一種新型樣品前處理技術(shù),它是將磁性吸附劑分散到樣品溶液中進行吸附,使樣品能夠與吸附劑接觸,萃取過程簡單,避免了繁瑣的操作程序,可在短時間內(nèi)實現(xiàn)大體積樣品中待測組分的吸附和萃取,同時,操作過程中有機溶劑的使用量減少,也避免對環(huán)境的污染,此外在加磁場作用下,待測組分可以隨磁性吸附劑快速分離,不僅避免了繁瑣的后處理操作,也有效的避免了樣品基質(zhì)中雜質(zhì)的干擾。作為MSPE技術(shù)的核心,磁性固相萃取材料的開發(fā)與制備一直是研究者關(guān)注的重點,嘗試并進一步拓展MSPE技術(shù)的應用范圍,近年來,針對于新型磁性固相萃取的開發(fā)和制備,受到了越來越多科研工作者的關(guān)注,特別是在食品檢測、環(huán)境污染等方面。在本論文中,采用自由基聚合的方法,以氨基酸衍生物為主要功能單體,我們設計并合成了針對于食品復雜基質(zhì)中有害目標物的新型磁性固相萃取材料,即食品防腐劑和植物激素苯氧乙酸類化合物,并考察了其吸附性能,具體的研究內(nèi)容如下所述:1.制備了聚(苯乙烯-co-L-苯丙氨酸甲基丙烯酰氯)修飾的磁性納米顆粒,并將其作為磁性固相萃取吸附劑用于復雜樣品飲料中防腐劑苯甲酸鈉的分離分析。在材料制備過程中,通過自由基聚合,將功能單體L-苯丙氨酸甲基丙烯酰氯和苯乙烯修飾于磁性納米顆粒表面。與其他兩種防腐劑尼泊金丙酯和山梨酸鉀相比,所合成吸附材料對苯甲酸鈉具有較好的選擇性,其中,吸附劑對目標物的吸附容量為6.08±0.31 mg/g。此外,所制備的吸附材料對于苯甲酸鈉表現(xiàn)出較快的鍵合速率:5分鐘之內(nèi)即可達到最大吸附容量的85%。進一步,我們將所制備的吸附材料應用于飲料中防腐劑苯甲酸鈉的分析中,在接下來的工作中,通過進一步的單體比例優(yōu)化,所發(fā)展材料具有較好的應用前景。2.采用自由基聚合的方法,以聚氨基酸為功能單體,偶氮二異丁腈為引發(fā)劑,磁性納米顆粒為基質(zhì),制備了對復雜樣品豆芽中兩種常見植物激素,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。考察了其對2,4-D和4-CPA的吸附性能,探討了其吸附動力學、吸附等溫線及選擇性,并將其應用于豆芽中2,4-D和4-CPA的分離富集研究中。結(jié)果表明:所制備的聚氨基酸功能化的磁性納米顆粒對2,4-D和4-CPA具有較高的吸附容量(吸附量分別為39.82 mg/g,29.02mg/g),以及較好的選擇吸附性能;作為吸附劑,能夠?qū)崿F(xiàn)對實際復雜樣品豆芽中2,4-D和4-CPA的分離分析。
[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 鹵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.
【學位授予單位】：山東農(nóng)業(yè)大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：O657.72;TS207.3

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