环境中锑和丙烯酰胺的谱学检测研究

发布时间：2018-03-01 04:18

  本文关键词： 锑 水杨基荧光酮 荧光光谱 高效液相色谱-荧光法 丙烯酰胺　出处：《南华大学》2013年硕士论文　论文类型：学位论文

【摘要】：锑（antimony；Sb）和丙烯酰胺（acrylamide；AM）都是对环境和人体健康具有潜在危害的物质。锑是一种微量元素，也是一种重金属。长期接触锑可破坏人体内脏功能，吸入后容易发生锑中毒，并具有潜在的致癌风险。AM是一种高水溶性的α, β-不饱和羰基化合物，易被人体吸收，无论经口、皮肤或呼吸道进入人体均可导致中毒。AM引起的慢性中毒主要以周围神经损害为主。长期摄入过量的丙烯酰胺可导致基因损伤，诱发癌变，还可损害遗传物质。因此，进行环境中锑和食品中丙烯酰胺的检测研究具有十分重要的意义。 本文第二部分应用光谱学技术建立了环境中锑的检测新方法。研究了SAF-Sb~(3+)的光谱特性和反应的适宜条件。①在HCl提供的强酸性介质中，水杨基荧光酮与Sb~(3+)阳离子发生配合反应，形成配合物，导致水杨基荧光酮的荧光强度明显降低。在优化的实验条件下，锑质量浓度为0.2~3.0μg/25ml时，水杨基荧光酮在520nm处的荧光猝灭程度（ΔF）与ρ（Sb~(3+)）之间存在良好的线性关系（r=0.9991）。该方法锑的检出限为2.4ng/ml，环境中水样分析的相对标准偏差为2.5%～3.1%，加标回收率范围是96.0%～105.0%。据此建立水杨基荧光酮荧光分光光度法测定水样中痕量锑的新方法。结果表明采用荧光光谱法测定锑简便快捷，试剂用量少，准确性好，，方法灵敏，测定结果满意。 本文第三部分应用高效液相色谱-荧光法建立了水体中痕量锑的测定新方法。基于荧光探针分子水杨基荧光酮的荧光特性间接测定水样中的锑。采用AgilentTC-C18色谱柱分离，流动相为乙醇-水溶液（v/v=70∶30），流速为1.0ml/min，柱温为30℃，荧光检测器激发波长为494nm，发射波长为520nm。色谱测定结果表明，当锑的质量浓度在0.005μg/ml～0.1μg/ml时，峰面积（A）对质量浓度（ρ）成良好的线性关系。荧光检测锑的检出限为3.0ng/ml，样品相对标准偏差为0.90%～1.50%（n=6），加标回收率98.6%～107.0%。用于水样分析，结果满意。 本文第四部分基于将速溶咖啡样品处理后，用二极管阵列-高效液相色谱法测定提取液中的丙烯酰胺。确定丙烯酰胺的紫外吸收波长由二极管阵列检测器来确定，经C18色谱柱分离，流动相为5%的甲醇水溶液，流速为1.0ml/min，在210nm波长出测定丙烯酰胺。在优化的实验条件下，丙烯酰胺浓度为0.11～100μg/ml时，色谱峰面积与浓度呈现良好线性关系，相关系数为0.9999，检出限为60ng/ml。测定咖啡样品加标溶液的回收率为97.60%～104.50%，相对标准偏差0.29%～0.50%。该方法具有简便、快速、灵敏度高等特点，用于速溶咖啡中丙烯酰胺测定，结果满意。
[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 伪, 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

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