【作者】 王晓军；

【导师】 周瑛；

【作者基本信息】 浙江工业大学 ， 农药学， 2015， 硕士

【摘要】 随着现代工业的快速发展,镉、镍、铜、钴和锌等重金属不可避免地释放进入环境之中。此外,食品与水是大多数人重金属暴露的主要来源,重金属可以通过食物链对人体产生蓄积作用,最终危害人体健康。因此,对公共卫生安全而言,食品、环境水样中重金属的痕量检测具有十分重要的意义。本论文研究目的是,将分散液液微萃取与电感耦合等离子体质谱联用建立痕量分析新方法,并将其应用于实际样品中痕量金属元素与人工纳米材料的分析检测。本论文首次建立了分散液液微萃取-分散固相微萃取与电感耦合等离子体质谱联用技术同时分离富集复杂基质中痕量重金属的分析方法。具体内容如下:(1)建立了以DDTC为螯合剂、四氯化碳(CCl4)为萃取剂的分散液液微萃取-分散固相微萃取-电感耦合等离子体质谱法(DLLME/D-μ-SPE-ICP-MS)快速测定食品、环境水样中镉、镍和铜的新方法。对萃取剂种类及用量、溶液p H值、螯合剂浓度、Fe3O4用量、盐效应、超声时间、基质效应等影响萃取效率的实验因素进行了优化。本方法应用于食品及环境水样中镉、镍和铜的检测,结果令人满意。(2)建立了超声辅助-液液分散微萃取(USA-DLLME)技术测定环境水样中痕量纳米氧化锌的新方法,并对萃取剂种类及用量、溶液p H值、盐效应、萃取时间、萃取温度等影响萃取效率的因素进行了优化。本方法应用于实际水样中纳米氧化锌的分析,测定结果令人满意。(3)以APDC为螯合剂,甲苯为萃取剂,采用超声辅助-分散液液微萃取技术,以ICP-MS为检测手段,优化了萃取剂用量、溶液p H值、螯合剂浓度、超声时间、盐效应等影响萃取的各种因素,并对自来水、湖水、河水等环境水样中的痕量镉、钴和锌进行了分析,测定结果令人满意。更多还原

【Abstract】 With the developing of modern industry, heavy metals such as cadmium, nickel, copper, cobalt and zinc are inevitably released into the environment as a result of human activities and rapid industrialization. Moreover, food and water are the main sources of exposure to Cd, Ni, Cu, Co and Zn for the general population; these heavy metals could enter food chain gradually accumulate in living organisms even at a very low concentration levels and finally cause damage to human health. Therefore, the determination of heavy metal ions at trace levels in real samples including food and environmental water is a very important task for the public health safety.The objective of this work aims to develop new methods for analysis of trace metal elements and engineered nanomaterials in real samples by the combination of dispersive liquid-liquid microextraction with inductively coupled plasma-mass spectrometry. Herein, in this paper, dispersive liquid-liquid microextraction combined with dispersive micro-solid phase extraction for separation, enrichment and analysis of trace heavy metals in complex matrices by ICP-MS was established for the first time. The details were as follows:(1)A rapid and innovative two-step microextraction technique, combining dispersive liquid-liquid microextraction and dispersive micro-solid phase extraction, was developed for the preconcentration and extraction of cadmium, nickel and copper in food and environmental water samples, prior to analyzed by inductively coupled plasma-mass spectrometry(ICP-MS). In the proposed approach, DDTC was used as chelating agent and carbon tetrachloride was selected as extraction solvent. Several parameters that influencing the extraction efficiency, such as the kind and volume of the extraction solvent, p H of sample solution, concentration of the chelating agent, amount of Fe3O4 magnetic nanoparticles, salt effect, sonication time and matrix effect were optimized in details. The method was successfully applied to the determination of Cd, Ni and Cu ions in food and environmental water samples with satisfactory results.(2)A simple and powerful microextraction technique was used for the detection of the nano-Zn O trace amounts in environmental water samples using the ultrasound-assisted dispersive liquid-liquid microextraction (USA-DLLME), followed by the inductively coupled plasma-mass spectrometry(ICP-MS). Several parameters that affect the extraction efficiency, such as the volume of the extraction solvent, p H of sample solution, salt effect, extraction time and extraction temperature were investigated and optimized. The proposed method was successfully applied to the extraction and determination of nano-Zn O in nature water samples.(3)The method based on ultrasound-assisted dispersive liquid-liquid microextraction(USA-DLLME) preconcentration and inductively coupled plasma-mass spectrometry(ICP-MS) detection was successfully proposed for the determination of trace Cd, Co and Zn in environmental water samples. In the proposed approach, APDC and toluene were selected as the chelating agent and extraction solvent. Several parameters that affect the extraction efficiency, such as the volume of the extraction solvent, p H of sample solution, concentration of the chelating agent, salt effect, and sonication time were investigated and optimized. The method was successfully applied to determination of Cd, Co and Zn in tap, river and lake water samples.更多还原