本文選題：樣品前處理 + 固相萃取　； 參考：《湖南大學》2015年碩士論文

【摘要】：多環(huán)芳烴由于其穩(wěn)定的結構而長期存在于我們的環(huán)境中,能夠引起生物體的DNA損傷和它帶來的致畸、致癌、致突變作用。因此這類化合物已引起廣泛關注并被認證為最重要的一類持久性有機污染物,開發(fā)有效的分析檢測方法是十分有必要的。但是帶強疏水基團的多環(huán)芳烴在環(huán)境樣品中往往是痕量存在的,而且環(huán)境樣品的基質往往都很復雜,其對目標物的檢測干擾很嚴重。因此不能對多環(huán)芳烴進行直接檢測,實際樣品進樣前的預處理非常重要。目前,多種樣品預處理技術已被開發(fā),其中,固相萃取因具有消耗有機溶劑少、回收率高、操作簡便等優(yōu)點,備受科學研究者的關注。本工作重點在于開發(fā)新型固相萃取吸附劑,用于富集濃縮環(huán)境水樣中的多環(huán)芳烴,并與高效液相色譜-熒光檢測聯(lián)用進行分析檢測。研究內容如下:1.室溫下,通過簡單的磁力攪拌合成出粒徑均一、對水穩(wěn)定的微米級類沸石咪唑酯骨架材料ZIF-7,建立一種基于該種材料的固相萃取方法,聯(lián)合HPLC-FLD應用于環(huán)境水樣中多環(huán)芳烴的分析。這種材料原料易得、合成簡便且對環(huán)境友好,通過優(yōu)化一些實驗條件,新方法對七種多環(huán)芳烴的檢測限在0.13-2.66 ng L-1范圍內,相對標準偏差RSD均在10%以內,展現了良好的重現性。在加入標準混合物的環(huán)境樣品中,PAHs的回收率為78.8-90.3%,RSD≤9.4。2.利用相同的原料,在不同的有機溶劑中合成出兩種拓撲結構不同的類沸石咪唑酯骨架材料ZIF-7和ZIF-11。通過傅里葉紅外光譜、X射線衍射、掃描電鏡以及接觸角測量儀等表征,確定了兩種材料成功合成且適用于固相萃取。經過比較,相同條件下,ZIF-11對多環(huán)芳烴的萃取效果比ZIF-7更好。因而,我們選擇ZIF-11晶體作為吸附劑建立固相萃取的方法,用于環(huán)境水樣中多環(huán)芳烴的分析。通過優(yōu)化各種可能影響萃取的因素,包括萃取時間、洗脫溶劑、洗脫溶劑體積、有機改性劑的量和鹽濃度,在最佳條件下水樣中多環(huán)芳烴的回收率在82.4%至112.7%之間,相對標準偏差小于9%。3.室溫下用一鍋法合成了核殼結構的納米-微米硅球,以此為支持材料,在其表面修飾了氨基后,用溶劑熱法在其表面原位生長納米Ui O-66。并以此復合材料為吸附劑建立新的固相萃取方法,用于環(huán)境水樣中多環(huán)芳烴的前處理,通過HPLC-FLD進行檢測。通過優(yōu)化吸附劑的用量、有機改性劑的種類及用量、萃取時間和鹽濃度,在最佳條件下,水樣中多環(huán)芳烴的檢測限在0.04-0.40 ng L-1范圍內,回收率為88.0-105.1%,相對標準偏差小于7%。
[Abstract]:Polycyclic aromatic hydrocarbons (PAHs) exist in our environment for a long time because of their stable structure, which can cause DNA damage and teratogenic, carcinogenic and mutagenic effects of PAHs. Therefore, these compounds have attracted widespread attention and have been recognized as the most important class of persistent organic pollutants. It is necessary to develop an effective analytical method for detection of these compounds. However, polycyclic aromatic hydrocarbons (PAHs) with strong hydrophobic groups often exist in trace amounts in environmental samples, and the matrix of environmental samples is often very complex. Therefore, PAHs can not be directly detected, and the pretreatment of actual samples before injection is very important. At present, a variety of sample pretreatment techniques have been developed. Among them, solid phase extraction (SPE) has attracted the attention of scientific researchers for its advantages of less organic solvent consumption, high recovery rate and easy operation. This work focuses on the development of a novel solid phase extraction adsorbent for the enrichment of PAHs in environmental water samples and the analysis and detection of PAHs with high performance liquid chromatography-fluorescence detection. The research is as follows: 1. At room temperature, a homogeneous particle size was synthesized by simple magnetic stirring. A solid phase extraction method based on ZIF-7 was established, and the HPLC-FLD was used in the analysis of polycyclic aromatic hydrocarbons (PAHs) in environmental water samples. This material is easy to obtain, easy to synthesize and environmentally friendly. By optimizing some experimental conditions, the detection limit of the new method for seven PAHs is within 0.13-2.66 ng L-1, and the relative standard deviation (RSD) is within 10%, showing a good reproducibility. The recoveries of PAHs in environmental samples with standard mixtures were 78.8-90.3 and RSD 鈮，

本文編號：2089192