石墨炉原子吸收光谱技术在生物样品测定中的应用研究

【作者】 梁冬松；

【导师】 林琳；

【作者基本信息】 郑州大学 ， 分析化学， 2005， 硕士

【摘要】 在已成为历史的20世纪,贵金属材料曾起到重要作用,被誉为“现代工业维他命”。这主要是贵金属在人类赖以生存的环境、能源和生命科学中显示的重要作用所决定的。但随着对贵金属研究的深入,发现金、银、钯等贵金属元素在人体中积累后会对人体健康造成危害。随着工业的发展及贵金属应用的日益广泛,它们对环境的污染已不容忽视。铍是一种有害元素,我国已经制订了饮用水中铍含量的卫生标准,但人体内铍含量的卫生标准还未见到。为了研究金、银、钯和铍这几种金属在人体中的背景值,我们分别建立了新的石墨炉原子吸收测定体系,并应用到生物样品和药品的实际测定中。人体中污染元素的背景值反映了它们在环境中的污染程度,此项工作可为环境污染研究及环境治理提供依据。 本论文主要围绕着上述主题开展工作,具体包括: 1.建立了以乙酸乙酯作萃取剂,钇涂层石墨管原子吸收法测定金的方法,有效地避免了碳化物的生成及一些常见元素的干扰,测定了人发样品中金的含量。方法的检出限为2.4×10^-11g,对于10ng/mL金的相对标准偏差为3.3%。 2.比较了多种萃取剂和基体改进剂对GFAAS法测定人发中银的影响,建立了MIBK作萃取剂,KI作络合剂,EDTA作基体改进剂的新方法。生物样品中常见元素的干扰得到抑制。方法的线性范围为0～25ng/mL,检出限为1.0×10^-10g,相对标准偏差为3.3% 3.比较了多种涂层金属处理石墨管和多种基体改进剂对GFAAS法测定微量铍的影响。建立了涂钼石墨管硝酸锂作基体改进剂测定铍的新方法,提高了灰化温度,降低了原子化温度,增强了抗干扰能力。对土壤标样中的铍进行了测定,结果与推荐值相符。并测定人发样品中的铍,结果满意。方法的相对标准偏差为4.8%,检出限为1.4×10^-11g。 4.本文采用涂钼热解石墨管,硝酸锂作基体改进剂,石墨炉原子吸收法测定了用新合成路线合成的1-脱氧野尻毒素中钯催化剂残留量。该法的线性范围和检出限分别为0～50ng/mL,3.5×10^-11g。对于5ng/mL钯的测定表明,方法的相对标准偏差为4.7%。更多还原

【Abstract】 In the past 20th century, precious metal materials have played an important part in most aspects of the society, and they have been honored as "modern industrial vitamin". The honor is mainly because of the important effects they have brought to the environment, the energy and the science that human beings rely on, However, as the research on precious metals moves on, elements such as Au, Ag and Pd are found to do harm to the human body if their contents are over amounted. Along with this, with the development of industry and the wide use of the precious metals, the pollutions they have brought to the environment cannot be overlooked. Beryllium is a harmful element, our nation has laid down hygienic standard for Be in drinking water, it is still not known about the hygienic standard for its content in human body. In order to research the background value of the four elements which accumulate in human body, we have respectively set up new graphite furnace atomic absorption systems to conduct detecting research on their contents in biological samples and chemical reagents. Metals’ background value in human bodies reflects the extent that they have produced the environmental pollution. This research is also helpful in providing evidence for the environmental pollutions produced by these metal elements and also helpful in removing the environmental pollution.The content of this paper is as follows:1. A method was established for the determination of gold in human hair by GFAAS.In the presence of extractant acetic ester, the matrix interference was eliminated efficiently and when the graphite tube was coated with Yttrium the sensitivity was improved .The method could be used for the determination of trace gold in biological samples or ore samples. The detection limit is 2.4×10-11g, and the relative standard deviation is 3.3%.2. Different kinds of extractants and matrix modifiers have been tested for the determination of trace silver in human hair by GFAAS. A simple method was developed after preconcentration with methyl isobutylketone, KI and EDTA were added in the sample solution as complex agent and matrix modifier, the optimized content of KI and EDTA in sample solution were 0.8%. The matrix interference of elements which were common inbiological samples was eliminated efficiently, additionally, the recovery of this method is much better. Calibration curves for silver were linear across the rang of 0~25ng/mL. The relative standard deviation is 3.3%, and the detection limit is 1.0× 10-10g.3. Different kinds of coating layers and matrix modifiers have been tested for the determination of trace beryllium in biological samples by GFAAS. A new method using molybdenum coated graphite tube with lithium nitrate as matrix modifier was established.The result shows that ashing temperature increased while atomization temperature decreased. Meanwhile the method has strong ability to resist interference,This method has been used for the determination of trace beryllium in standard reference soil sample and human hair. The detection limit is 1.4× 10-11g, and the relative standard deviation is 4.8%.4. A new method for the determination of trace palladium in 1-deoxynojirimycin synthesized by new means. The graphite tube coated with molybdenum and the matrix modifier of lithium nitrate were used in this method, then, the matrix interference was eliminated efficiently in determining actual samples. The calibration curve is linear over the range of 0~50 ng/g with detection limit of 3.5 × 10-11g and RSD of 4.7%.更多还原