本文關(guān)鍵詞： 銻 水楊基熒光酮 熒光光譜 高效液相色譜-熒光法 丙烯酰胺　出處：《南華大學(xué)》2013年碩士論文　論文類(lèi)型：學(xué)位論文

【摘要】：銻（antimony；Sb）和丙烯酰胺（acrylamide；AM）都是對(duì)環(huán)境和人體健康具有潛在危害的物質(zhì)。銻是一種微量元素，也是一種重金屬。長(zhǎng)期接觸銻可破壞人體內(nèi)臟功能，吸入后容易發(fā)生銻中毒，并具有潛在的致癌風(fēng)險(xiǎn)。AM是一種高水溶性的α, β-不飽和羰基化合物，易被人體吸收，無(wú)論經(jīng)口、皮膚或呼吸道進(jìn)入人體均可導(dǎo)致中毒。AM引起的慢性中毒主要以周?chē)窠?jīng)損害為主。長(zhǎng)期攝入過(guò)量的丙烯酰胺可導(dǎo)致基因損傷，誘發(fā)癌變，還可損害遺傳物質(zhì)。因此，進(jìn)行環(huán)境中銻和食品中丙烯酰胺的檢測(cè)研究具有十分重要的意義。 本文第二部分應(yīng)用光譜學(xué)技術(shù)建立了環(huán)境中銻的檢測(cè)新方法。研究了SAF-Sb~(3+)的光譜特性和反應(yīng)的適宜條件。①在HCl提供的強(qiáng)酸性介質(zhì)中，水楊基熒光酮與Sb~(3+)陽(yáng)離子發(fā)生配合反應(yīng)，形成配合物，導(dǎo)致水楊基熒光酮的熒光強(qiáng)度明顯降低。在優(yōu)化的實(shí)驗(yàn)條件下，銻質(zhì)量濃度為0.2~3.0μg/25ml時(shí)，水楊基熒光酮在520nm處的熒光猝滅程度（ΔF）與ρ（Sb~(3+)）之間存在良好的線(xiàn)性關(guān)系（r=0.9991）。該方法銻的檢出限為2.4ng/ml，環(huán)境中水樣分析的相對(duì)標(biāo)準(zhǔn)偏差為2.5%～3.1%，加標(biāo)回收率范圍是96.0%～105.0%。據(jù)此建立水楊基熒光酮熒光分光光度法測(cè)定水樣中痕量銻的新方法。結(jié)果表明采用熒光光譜法測(cè)定銻簡(jiǎn)便快捷，試劑用量少，準(zhǔn)確性好，，方法靈敏，測(cè)定結(jié)果滿(mǎn)意。 本文第三部分應(yīng)用高效液相色譜-熒光法建立了水體中痕量銻的測(cè)定新方法�；跓晒馓结�?lè)肿铀畻罨鶡晒馔臒晒馓匦蚤g接測(cè)定水樣中的銻。采用AgilentTC-C18色譜柱分離，流動(dòng)相為乙醇-水溶液（v/v=70∶30），流速為1.0ml/min，柱溫為30℃，熒光檢測(cè)器激發(fā)波長(zhǎng)為494nm，發(fā)射波長(zhǎng)為520nm。色譜測(cè)定結(jié)果表明，當(dāng)銻的質(zhì)量濃度在0.005μg/ml～0.1μg/ml時(shí)，峰面積（A）對(duì)質(zhì)量濃度（ρ）成良好的線(xiàn)性關(guān)系。熒光檢測(cè)銻的檢出限為3.0ng/ml，樣品相對(duì)標(biāo)準(zhǔn)偏差為0.90%～1.50%（n=6），加標(biāo)回收率98.6%～107.0%。用于水樣分析，結(jié)果滿(mǎn)意。 本文第四部分基于將速溶咖啡樣品處理后，用二極管陣列-高效液相色譜法測(cè)定提取液中的丙烯酰胺。確定丙烯酰胺的紫外吸收波長(zhǎng)由二極管陣列檢測(cè)器來(lái)確定，經(jīng)C18色譜柱分離，流動(dòng)相為5%的甲醇水溶液，流速為1.0ml/min，在210nm波長(zhǎng)出測(cè)定丙烯酰胺。在優(yōu)化的實(shí)驗(yàn)條件下，丙烯酰胺濃度為0.11～100μg/ml時(shí)，色譜峰面積與濃度呈現(xiàn)良好線(xiàn)性關(guān)系，相關(guān)系數(shù)為0.9999，檢出限為60ng/ml。測(cè)定咖啡樣品加標(biāo)溶液的回收率為97.60%～104.50%，相對(duì)標(biāo)準(zhǔn)偏差0.29%～0.50%。該方法具有簡(jiǎn)便、快速、靈敏度高等特點(diǎn)，用于速溶咖啡中丙烯酰胺測(cè)定，結(jié)果滿(mǎn)意。
[Abstract]:Antimony (SB) and acrylamide (AM) are both potentially harmful substances to the environment and human health. Antimony is a trace element and a heavy metal. Long-term exposure to antimony can damage the visceral function of the human body and lead to antimony poisoning after inhalation. And potentially carcinogenic risk. AM is a highly water-soluble 偽, 尾-unsaturated carbonyl compound, easily absorbed by the human body, regardless of the mouth, The chronic poisoning caused by skin or respiratory tract can be mainly caused by peripheral nerve damage. Long-term intake of acrylamide can cause gene damage, carcinogenesis, and genetic material damage. It is very important to study the detection of antimony in environment and acrylamide in food. In the second part of this paper, a new method for the detection of antimony in the environment was established by using spectroscopic technique. The spectral characteristics and reaction conditions of SAF-Sb~(3) were studied in the strong acidic medium provided by HCl. Salicylidene fluoresceone reacted with Sb~(3 cations to form complexes, which resulted in a significant decrease in the fluorescence intensity of salicylfluorone. Under the optimized experimental conditions, the concentration of antimony was 0.2 渭 g / 25ml. There is a good linear relationship between fluorescence quenching degree of salicylfluorone at 520 nm (螖 F) and 蟻 ~ (2 +) SbBX ~ (3 +). The detection limit of antimony is 2.4 ng / ml, the relative standard deviation of water sample analysis in environment is 2.5 ng / ml, and the recovery range is 96.0 ~ 105.0. A new method for the determination of trace antimony in water samples by fluorescence spectrophotometry with salicylidene fluorone. The results show that the method of fluorescence spectrometry is simple and convenient for the determination of antimony. The method is sensitive and satisfactory. In the third part of this paper, a new method for the determination of trace antimony in water was established by high performance liquid chromatography-fluorescence method. Based on the fluorescence characteristics of fluorescence probe molecule salicylfluorone, the antimony in water sample was indirectly determined. The method was separated by AgilentTC-C18 column. The mobile phase is ethanol-aqueous solution v / v / v: 30, the flow rate is 1.0ml / min, the column temperature is 30 鈩

本文編號(hào)：1550342