离子液体在样品前处理及化学发光在色谱分析中的应用研究
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摘要
近些年来,由于色谱分析的样品往往具有很复杂的基质,同时待测物质的含量又极少,因此发展新型的、绿色环保并且高效的色谱样品前处理方法和灵敏的检测手段对于提高整个色谱分析的选择性和灵敏度有着非常重要的意义。
本论文正是基于以上考虑,建立了利用离子液体与现代萃取仪器相结合的新型、高效色谱样品前处理方法,同时利用化学发光检测的高灵敏度和一定的选择性,研究了其与离子色谱相结合测定复杂基体中痕量有机物,极大的扩宽了离子色谱的应用范围,提高了检测的灵敏度。
第一章介绍了离子液体的基本特性并综述了其作为新型萃取剂在分离分析和色谱样品前处理中的应用；对化学发光的基本原理、仪器结构、典型的化学发光体系以及其与高效液相色谱的联用技术应用和发展做了概述,指出利用离子色谱与化学发光检测联用,不仅发光条件与离子色谱分离条件可以很好匹配,而且发光检测灵敏度也较高。
第二章利用亲水性离子液体作为萃取剂,结合现代加压溶剂萃取技术,快速萃取4种传统中药中的芦丁和槲皮素。萃取物经高效液相色谱分离后利用化学发光检测。首次将离子液体-加压溶剂萃取与化学发光检测结合起来,研究了加压溶剂萃取与离子液体结合的萃取机理,对离子液体的种类、浓度、萃取时间、循环次数等影响萃取效率的因素做了考察。同时也与常用的紫外检测法进行了对比。
第三章首次将微波辅助离子液体分散微萃取技术应用于固体样品中痕量组分的提取。利用疏水性离子液体[C4mim][PF6]作为萃取剂,对影响萃取效率的因素例如萃取时间、温度、离子液体用量等进行了优化,同时也对萃取机理和速率控制类型进行了初步探讨。以中药当归和蒲公英中阿魏酸的提取为例验证方法,将萃取与浓缩步骤合二为一。实验表明,本方法简单高效,有较广泛的应用前景。
第四章研究了碱性鲁米诺化学发光体系与阴离子交换色谱联用测定水中痕量酚类物质。由于阴离子交换色谱流动相为碱性,与高效液相色谱常用的酸性流动相相比更匹配柱后发光体系,而且离子色谱流动相不含有机改进剂,避免了甲醇、乙腈等对发光的猝灭作用,不仅方法绿色环保,检测灵敏度也大大提高。
第五章研究了酸性高锰酸钾体系与阳离子交换色谱联用技术,对高锰酸钾的浓度,介质pH值、增敏剂的种类和浓度等进行了优化,用于测定复杂生物样品中痕量的儿茶酚胺类物质,取得较为满意的结果。
In recent years, because of the complex matrix and low analyte content of sample of HPLC analysis, it is very important to develop new types of sample pretreatment methods and sensitive detection methods.
In this work, the application of ionic liquid-based extraction techniques in sample pretreatment of different chromatographic methods was investigated. The combination of ion chromatography and chemiluminescence was also studied.
Chapter one comprised a brief introduction of ionic liquid and its application in analytical chemistry and a comprehensive review of the application of ionic liquid extraction methods in sample pretreatment of chromatography. The information of chemiluminescence such as principle, apparatus structure, typical chemical luminescence system and combination of HPLC were summarized.
In chapter two, a novel ionic liquid-based pressurized liquid extraction (IL-PLE) procedure coupled to high performance liquid chromatography (HPLC) tandem chemiluminescence (CL) detection capable of quantifying trace amounts of rutin and quercetin in four Chinese medicine plants was described. The effect of ILs with different cation on extraction efficiency was systematically investigated. In addition, the extraction performance of IL-PLE was compared with HRE and UAE for the extraction of rutin and quercetin in real samples. What is more, the selectivity of the proposed method was investigated by comparing the chromatograms of real sample obtained with CL detector and UV detector.
In chapter three, the ionic liquid-based microwave-assisted dispersive microextraction (IL-based MADME) was firstly used to solid sample. The aim of this work is to simplify the analytical step, reduce the extraction time and improve the sensitivity. The effects of various experimental parameters were studied and the possible extraction mechanism was also discussed. The developed method was successfully applied to the analysis of real samples.
In chapter four, a novel method was established for the simultaneous determination of resorcinol and phloroglucinol in environmental water samples by ion chromatography with chemiluminescence detection. The absence of methanol and acetonitrile in mobile phase made the proposed method more sensitive.
In chapter five, without complicated derivative process and gradient elution, a simple, fast, sensitive, highly selective and eco-friendly analytical method for the determination of catecholamines in human urine was established originally in this paper, based on the combination technique of IC with the CL detection. Parameters related to IC separation and acidic potassium permanganate chemiluminescence system were optimized systematically.
本论文正是基于以上考虑,建立了利用离子液体与现代萃取仪器相结合的新型、高效色谱样品前处理方法,同时利用化学发光检测的高灵敏度和一定的选择性,研究了其与离子色谱相结合测定复杂基体中痕量有机物,极大的扩宽了离子色谱的应用范围,提高了检测的灵敏度。
第一章介绍了离子液体的基本特性并综述了其作为新型萃取剂在分离分析和色谱样品前处理中的应用；对化学发光的基本原理、仪器结构、典型的化学发光体系以及其与高效液相色谱的联用技术应用和发展做了概述,指出利用离子色谱与化学发光检测联用,不仅发光条件与离子色谱分离条件可以很好匹配,而且发光检测灵敏度也较高。
第二章利用亲水性离子液体作为萃取剂,结合现代加压溶剂萃取技术,快速萃取4种传统中药中的芦丁和槲皮素。萃取物经高效液相色谱分离后利用化学发光检测。首次将离子液体-加压溶剂萃取与化学发光检测结合起来,研究了加压溶剂萃取与离子液体结合的萃取机理,对离子液体的种类、浓度、萃取时间、循环次数等影响萃取效率的因素做了考察。同时也与常用的紫外检测法进行了对比。
第三章首次将微波辅助离子液体分散微萃取技术应用于固体样品中痕量组分的提取。利用疏水性离子液体[C4mim][PF6]作为萃取剂,对影响萃取效率的因素例如萃取时间、温度、离子液体用量等进行了优化,同时也对萃取机理和速率控制类型进行了初步探讨。以中药当归和蒲公英中阿魏酸的提取为例验证方法,将萃取与浓缩步骤合二为一。实验表明,本方法简单高效,有较广泛的应用前景。
第四章研究了碱性鲁米诺化学发光体系与阴离子交换色谱联用测定水中痕量酚类物质。由于阴离子交换色谱流动相为碱性,与高效液相色谱常用的酸性流动相相比更匹配柱后发光体系,而且离子色谱流动相不含有机改进剂,避免了甲醇、乙腈等对发光的猝灭作用,不仅方法绿色环保,检测灵敏度也大大提高。
第五章研究了酸性高锰酸钾体系与阳离子交换色谱联用技术,对高锰酸钾的浓度,介质pH值、增敏剂的种类和浓度等进行了优化,用于测定复杂生物样品中痕量的儿茶酚胺类物质,取得较为满意的结果。
In recent years, because of the complex matrix and low analyte content of sample of HPLC analysis, it is very important to develop new types of sample pretreatment methods and sensitive detection methods.
In this work, the application of ionic liquid-based extraction techniques in sample pretreatment of different chromatographic methods was investigated. The combination of ion chromatography and chemiluminescence was also studied.
Chapter one comprised a brief introduction of ionic liquid and its application in analytical chemistry and a comprehensive review of the application of ionic liquid extraction methods in sample pretreatment of chromatography. The information of chemiluminescence such as principle, apparatus structure, typical chemical luminescence system and combination of HPLC were summarized.
In chapter two, a novel ionic liquid-based pressurized liquid extraction (IL-PLE) procedure coupled to high performance liquid chromatography (HPLC) tandem chemiluminescence (CL) detection capable of quantifying trace amounts of rutin and quercetin in four Chinese medicine plants was described. The effect of ILs with different cation on extraction efficiency was systematically investigated. In addition, the extraction performance of IL-PLE was compared with HRE and UAE for the extraction of rutin and quercetin in real samples. What is more, the selectivity of the proposed method was investigated by comparing the chromatograms of real sample obtained with CL detector and UV detector.
In chapter three, the ionic liquid-based microwave-assisted dispersive microextraction (IL-based MADME) was firstly used to solid sample. The aim of this work is to simplify the analytical step, reduce the extraction time and improve the sensitivity. The effects of various experimental parameters were studied and the possible extraction mechanism was also discussed. The developed method was successfully applied to the analysis of real samples.
In chapter four, a novel method was established for the simultaneous determination of resorcinol and phloroglucinol in environmental water samples by ion chromatography with chemiluminescence detection. The absence of methanol and acetonitrile in mobile phase made the proposed method more sensitive.
In chapter five, without complicated derivative process and gradient elution, a simple, fast, sensitive, highly selective and eco-friendly analytical method for the determination of catecholamines in human urine was established originally in this paper, based on the combination technique of IC with the CL detection. Parameters related to IC separation and acidic potassium permanganate chemiluminescence system were optimized systematically.
引文
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