【作者】 王萍；

【导师】 倪永年；

【作者基本信息】 南昌大学 ， 分析化学， 2013， 硕士

【摘要】 基于化学动力学原理的分析方法具有操作简单、灵敏度高、测定时间短等特点,因此常被用于食品、环境、药物等复杂体系中的多组分分析测定；对测量数据进行前处理,如求导或平滑方法,能消除或减少由于光源噪声和温度漂移等因素对分析测定结果的影响。在较复杂的体系分析中,由于许多组分的性质比较相似,它们的动力学测量数据会有重叠,影响复杂混合物中各单一成分的测定,化学计量学-多元校正方法的引入使得动力学反应体系的定量解析成为可能。本文的主要研究内容是采用动力学分光光度法并藉助分析化学计量学的帮助,快速定量分析环境样中的农药残留,工业废水中的污染物,以及动物源食品中的兽药残留。为了研究化学计量学-动力学方法在环境水样中农药残留的应用,我们以环境水样中的两种常见农药(抗蚜威和杀线威)作为分析对象；探讨了反应体系中可能的机理,考察了可能反应进程的条件；在化学计量学的帮助下,我们构建了一个动力学方法测定环境样中农药残留的成功模型。我们还对环境水样中的氨基酚类物质进行了多组分定量分析,建立了校准曲线,得到其相关参数(线性范围、检测限、斜率和截距的相对标准偏差等),用文中提出方法对合成样分析测定的数据构建校正模型,然后对未知样进行预报,所得的结果与HPLC比较,结果满意。另外我们还利用食品抗氧化剂合成了纳米银,考察了合成纳米银合成的动力学过程及应用于食品中抗氧化剂分析的可能性,并建立了四种常见抗氧化剂的校正曲线。我们也尝试定量测定动物组织和牛奶中阿维菌素类抗寄生虫药,对实验条件及可能干扰因素进行了考察,建立相关标准曲线,构建定量校正模型并预报合成样品,并用于实际分析。更多还原

【Abstract】 Differential spectrophotometric method for dynamics determination is a fast, simple and sensitive analytical approach, commonly applied in simple analysis for two or three components. However, in complex systems, even if some substances are masked by some agent, it is still difficult for quantitatively analysis, such as food and environment samples. In order to resolve the problem, appropriate chemometrics mathematical statistic methods are introduced, then the effective analysis is implemented for complex multi-component system. The basic principle of the proposed method is as follows:the same reagent act with a variety of analytes. Their nature are different because of the different structure, the reaction rate has a certain different degree. When the added substance is excessed, the reaction can be regarded as pseudo-first-order reaction. In this case, the reaction rate is only linearly related to the concentration of added analytes, then quantitative methods was implemented based on the measured data. In most cases, due to the analytes with similar chemical properties, the differences of the reaction rate between these analytes is relatively small. Thus, some suitable chemometrics method can be used to resolve this problem. The quantitative analysis can be realized by building a multivariate calibration model for multi-component complex systems.In this paper, different kinetics-chemometrics-UV spectrophotometric method was applied to analyze for multi-component systems. The main applications of chemometrics methods were partial least squares (PLS), principal component regression (PCR) and artificial neural networks (ANN); The analytical complex systems, including environment and food objects, were selected as the analytical systems in this research work. In the thesis, four complex systerms were determined, including chemometrics-inhibition kinetic determination of pirimicarb and oxamyl in environmental water samples, silver anoparticles preparation using zntioxidant propyl gallate and its analytical application, kinetic spectrophotometric simultaneous determination of aminophenol isomers by partial least squares, and kinetic-chemometrics determination of avermectins in animal tissues and milk samples. At the same time, the mechanism of kinetic reaction was investigated and discussed, the parameters that could affect the experiment results were optimized, the calibration curve at different concentrations were examined for analytes, the calibration-prediction models were built to determine the synthetic samples, and the related models were established and used for determination of real samples. The feasibility of the method (kinetic spectrophotometric combined with chemometrics for determination multi-components in complex systems) was explored, and the results resolved by built calibration model were compared.更多还原