Study On The Element Speciation With Plasma Spectrometry Hyphenating Techniques And Its Application

Inductively coupled plasma Spectrometry (ICP-AES/MS) is a advanced multi-elements trace analysis technology.It offers extending good advantages in terms of low detection limit, high precision, good selectivity, little matrix effect, wide linear range and simultaneous multi-elements determination, so it is widely used. But the routine determination of ICP-AES/MS couldn't meet the research demand with scientific development. The hyphenating of ICP-AES/MS with analytical instruments else would combine strongpoints of them to a certain extent and so much as improves analytical capability for conquering their shortcomings so that it meets analytical demand to the best.Hydride Generation-Inductively Coupled Plasma Atomic Emission Spectrometry (HG-ICP-AES) enhance detection power of ICP-AES to hydride-forming elements. The detection limits of hydride-forming elements can be improved by one or two orders of magnitude over conventional nebulizer, and nearly eliminated matrix spectrum interference. Therefore, it provides a new way to solve complex matrix interference and speciation analysis .Capillary electrophoresis (CE) 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. The hyphenating of capillary electrophoresis and inductively coupling plasma spectrometry applying to element speciation analysis is a kind of rising separation and detection method. It can be widely applied to environmental protection, food, biology, clinic and Chinese Traditional Medicine (CTM), etc. We should be conscious of that the physiology, toxicity effect, biogeochemical behavior, environmental behavior and transformation of a element are highly depended on their chemical speciation to some great extent when determining the total amount of trace elements. Speciation analysis has already become an active frontier in environmental sciences, biochemistry and life sciences at present. When HG coupled with CE-ICP, the detection limits of analytical method can be improved.In this paper, the research has been carried on foundation of hyphenating of inductively coupling plasma atomic emission spectrometry with hydride generation and capillary electrophoresis. The application of coupling method to determination and speciation analysis of elements has been studied, too. The dominating contents and researching results of the paper are as follows:1:Using ultrasonic wave to bread red blood cell, the speciation of calcium in red blood cell was studied by capillary electrophoresis-inductively coupled plasma atomic emission spectrometry. The speciation of free calcium in red blood cell was identified using free standard Ca2+.Comparing the breading effect of SDS with ultrasonic wave, the ultrasonic method is more efficient than that of SDS. The effects of running buffer concentration and pH was researched, separation voltage and injection time on the CE-ICP-AES determination were optimized. The forms of calcium in rat red blood cells have seven different species, and quantification of free calcium concentration by peak height which was 0.25 mmol/L. The precisions (relative standard deviation, RSD, n=11) was 2.34%. The recoveries of the free calcium species in red blood cells were 83.2% to 89.6%.2:The separation of DNA and RNA using on-line coupling capillary electrophoresis (CE) with inductively coupled plasma atomic emission spectrometry(ICP-AES) was reported in the paper for the first time. The wavelength of P detected using ICP-AES was researched. The effects of running buffer, separation voltage and injection time on the CE-ICP-AES determination were investigated. The optimal condition was received. The relative standard deviation (RSD) of peak height of RNA and DNA was 2.03% and 2.21%, RSD of migration time for 1.61% and 1.94%, Detection limit RNA and DNA for 53.68mg/L and 79.80mg/L, respectively.3:An interface for CE- on-line redox-HG-ICP-AES has been designed. It was applied to determination of selenomethionine in rat plasma. The effects of separation buffer pH, the acidity of HCl, NaBH4 concentration and nebulizer flow rate on Se hydride signal intensity were discussed. The optimal condition has been gained. The relative standard deviation (RSD) was 5.3%, Detection limit of selenomethionine was 6.71μg/L.4:A new method was proposed for simultaneous determination of trace arsenic and selenium in milk by microwave-assisted digestion-HG-ICP-AES. The operation condition of hydride generation and inductively coupled plasma atomic emission spectrometry was investigated and optimized. The effects of acid concentration, NaBH4 concentration, nebulizer flow rate and sample volume was discussed. Under the optimal condition, the detection limits of arsenic and selenium are 0.61μg·L-1 and 0.50μg·L-1,respectively. The relative standard deviations are 1.35% and 1.33%, respectively. The recovery are 98% and 101%, respectively.