Development Of Capillary Electrophoresis And Inductively Coupled Plasma Atomic Emission Spectrometry And Its Application To Element Speciation In Chinese Traditional Medicine

The high-efficient capillary electrophoresis (CE) is developed rapidly in the eighties of the 20th century as a novel separation and analysis technology. It is considered to be one of the strongest influence branches of separate and analysis field at the end of last century, as well as the front of this field. It has many advantages : high efficiency , quick analysis speed , many analysis modes, little reagent consumption, wide application, easy automation, etc. Thus it shows extremely important application to life sciences, biotechnology, clinical medicine, medicine analysis and environmental science and so on. Inductively Coupled Plasma Atomic Emission Spectrometry(ICP-AES)offers extending good advantages in terms of low detection limit, high precision, wide linear range and simultaneous multi-elements determination, widely used in trace-element analysis fields in recent years. With individual advantages of capillary electrophoresis and inductively coupling plasma spectrometry, it realized the combination of efficient separation and element alternative measurement. With the application of that capillary electrophoresis and inductively coupling plasma spectrometry to element speciation analysis, it has become a kind of rising separation and detection method. It can be applied to environmental protection, food, biology, clinic and Chinese Traditional Medicine(CTM) ,etc. The trace elements will play an important role to the health in the traditional Chinese medicine. We should pay much attention to elemental speciation when determining the total amount of trace elements. It is well known that the physiology, toxicity, biogeochemical behavior, environmental behavior and transformation of trace toxic elements are highly depended on their chemical speciation to some great extent .Speciation analysis has already become an active front subject in environmental sciences, biochemistry and life sciences at present .The speciation analysis methodology will help to disclose the essence of trace amount elements in CTM. In this paper, the research has been carried on foundation of capillary electrophoresis and inductively coupling plasma atomic emission spectrometry and its application to the traditional Chinese medicine, mainly shown in the following several aspects: 1 Sampling device of capillary electrophoresis is designed and made, which adopts nitrogen pressure to inject.The advantage of this sampling device is simple operation and easy use, and good reproducibility. 2 The interface of capillary electrophoresis and inductively coupling plasma atomic emission spectrometry is made, which has good stability, high efficiency of nebulization, easy unpick and wash.. The analysis performance of the interface has been studied, such as voltage, nebulizer flow rate, detection limit, precision, efficiency of nebulization , work condition of the electrophoresis and condition of work of ICP-AES,etc. 3 The method, which combines capillary electrophoresis and inductively coupling plasma atomic emission spectrometry, is established. The speciation of the iron was examined by CE-ICP-AES.With 0.02mol·L-1 Potassium Hydrogen Phthalate (pH 4.05 ) as buffer solution for electrophoresis , the speciation separation of Fe3+ and Fe2+ is studied in O-phenanthroline solution. With 0.1mol·L-1 Sodium Acetate (pH 5.0) as buffer solution for electrophoresis, speciation separation of Fe3+and Fe2+ is stuied in the mixture complexing reagent EDTA and O-Phenanthroline. The influences of pH, electrophoresis electrolyte and the voltage of electrophoresis on the separatation of Fe3+ and Fe2+ are investigated. The satisfactory analysis results are obtained. 4 The new method for microwave extraction and capillary electrophoresis and inductively coupling plasma atomic emission spectrometry was developed. The aqueous solution in the ginkgo leaves and ginkgo fruits with the microwave extraction were filetered .through 0.45μm membrane. Choosing 0.05 mol·L-1 Sodium Tetraborate-Hydrochloric Acid as buffer solution for the electrophoresis (pH7.0), speciation of Ca, Mg, Zn and Cu is researched by CE-ICP-AES in extraction solution of ginkgo leaves and ginkgo fruits. The content of these elements in the ginkgo leaves and ginkgo fruits was determined, as well as the extraction efficiency of water solution. These results have important reference value to the comprehensive research of the ginkgo. 5 With 0.05mol·L-1 Sodium Acetate -Acetic Acid (pH 5.5) as buffer solution for electrophoresis, the speciation of trace elements in the pseudo-ginseng ,such as Mg, Cu and Fe , is studied by microwave extraction and capillary electrophoresis and inductively coupling plasma atomic emission spectrometry.The total content of these trace elements in pseudo-ginseng was determined, and extraction efficiency of water solution of Mg, Cu and Fe was obtained in pseudo-ginseng. This paper is divided into five chapters. Chapter One briefly introduces the history , current situation and combination of capillary electrophoresis and inductively coupling plasma atomic emission spectrometry / mass spectrometry , and their electrical connecting interface and its application, and the meaning of speciation analysis in the traditional Chinese medicine. From Chapter two to five, they are the making sampler and interface of CE-ICP-AES, The speciation of simple metal ions and the metal complex compounds, and the element speciation in the pseudo-ginseng and ginkgo, respectively..