Development of total "down sizing" analytical system following high-speed and high-powered concentration method

本研究的目的是将样品溶液的细微性与分析仪器的“小型化”相结合。研究了均相液-液萃取作为一种高速、高效的浓缩方法，建立了全规模化的分析体系。两年内所取得的成果如下：均相液-液萃取色谱法的发展。(1)高效液相色谱分析体系：在水/吡啶/氯乙酸乙酯三元组分溶剂体系中，利用pH依赖的相分离现象，建立了新型的均相液-液萃取体系。该方法采用水溶性卟啉分光光度-高效液相色谱法同时测定金属离子。(2)气相色谱/质谱分析系统：上述均相液-液萃取也可作为气相色谱/质谱的前处理。结果，对12种怀疑为内分泌干扰物的氯酚类化合物进行了同时快速的测定。滤纸上微滴和全氟表面活性剂均相液-液萃取后的一些光谱测定方法的发展。(1)荧光光谱法：采用全氟表面活性剂作为预富集法，研究了pH依赖性相分离。在22种氨基酸中，色氨酸采用荧光法选择性测定。(2) x射线荧光光谱法：同时测定了15种含高价金属的元素。提出了三种螯合剂在同一工艺中同时使用的新概念。综上所述，本工程按原计划取得了满意的效果。在不久的将来，这种有用的方法将广泛应用于实际样本。

The aim of this study is that fuses together with the minuteness of sample solution and the analytical apparatus which directs toward "Down Sizing". The homogeneous liquid-liquid extraction was studied in detail as a high-speed and high-powered concentration method, in order to create the total down sizing analytical system.The produced fruits during the term of two years are as follows :1.Development of some chromatographies following homogeneous liquid-liquid extraction.(1)HPLC analytical system : New homogeneous liquid-liquid extraction was developed using pH dependent phase separation phenomenon in water/pyridine/ethyl chloroacetate ternary component solvent system. In this method, the simultaneous determination of metal ions was performed by spectrophotometric detection-HPLC with water-soluble porphyrin.(2)GC/MS analytical system : Above homogeneous liquid-liquid extraction was also applied as pretreatment of GC/MS.As results, twelve kinds of chlorophenol compounds which are doubted as endocrine disrupting chemicals, were simultaneously and rapidly determined.2.Development of some spectrometries following a microdroplet on filter-paper and a homo-geneous liquid-liquid extraction with perfluorosurfactant.(1)Flurescence spectrometry : The pH dependent phase separation using perfluorosurfactant was studied as preconcentration method. Among 22 kinds of amino acid, tryptophan was selectively determined by the fluorometry.(2)X-ray fluorescence spectrometry : Fifteen kinds of element containing high valence metals were simultaneously determined. Moreover, new concept which uses together three kinds of chelating reagents in the same process, was proposed.In conclusion, the satisfactory results were obtained in this project according to the original plan. In the near future, this useful method will be applied to wide range of practical sample.