Preparation,Evaluation And Application Of Metal Tetraphenylporphyrin For Open Tubular Capillary Electrochromatography

Open-tubular Capillary Electrochromatography(OTCEC) is an emerging micro column electroseparation technique which combines the high selectivity of HPLC and the high efficiency of HPCE, The stationary phase is coated or eroded on the wall of capillary, whereas the mobile phase moves through the column propelled by electroosmosis. It is used to analysis the complicated medicines. Porphyrin was widely used in analytical chemistry. We collected a lot of literatures on these themes and analyzed it seriously and synthesized series of porphyrin compounds and provide the application in amino-acids separation. The paper is consisted by five paragraphs as follows:Chapter I IntroductionThis part give a review in detail about Open-tubular Capillary Electrochromatography (OTCEC) in the process of development, basic characteristic, principle of separation, progress of column preparation and the application in pharmaceutical analysis. The structure of porphyrins and its application in spectrophotometry, electrochemical analysis, molecular recognition, probe, HPLC and CE were discussed.Chapter II Determination of Zinc in Zinc Gluconate Tablets and human serum by HPLCTo determine the Zinc of Zinc Gluconate Tablets and human serum and study the optimal condition for the reaction of tetraphenylporphyrin with Copper and Zinc. A method for determination of Zinc in human serum and Zinc Gluconate Tablets by HPLC was established by tetraphenylporphyrin as pre-column derivatization regent and the ultraviolet spectrum of chelates was studied. The mobile consists of methanol, tetrahydroruran and HBO₃-NaBO₃ and the determination wave was 417 nm. The linearity of Zinc was good from 6.5-65 μg·ml^-1. The RSD of inter-day and intra-day was inferior to 4% and 13%, respectively. The method is simple and quick and suitable for the assay of Zinc Gluconate Tablets and useful for pharmacokinetic studies.Chapter III Preparation and evaluation of metal tetraphenylporphyrin for opentubular capillary electrochromatographyA series of novel open-tubular capillary electrochromatography columns were prepared coated with tetraphenylporphyrin Zinc, tetraphenylporphyrin ferrum and tetraphenylporphyrin Nickel respectively and evaluated by mixtures containing L-Arginine and DL-Tyrosine. The results showed that the metal tetraphenylporphyrin was better bonded inner wall of capillary. The highest efficiency reached 5.3 ×10⁴. The RSD of migration time is less than 3%. Under the optimum conditions, L-Arginine, L-asparagines, DL-Tyrosine, and L-asparagic acid were separated successfully.Chapter IV preparation of capillary column of metal tetraphenylporphyrin and application for dl-cystine enantiomer tion separationA series of novel open-tubular capillary electrochromatography columns coating tetraphenylporphyrin Zinc, tetraphenylporphyrin ferrum and tetraphenylporphyrin Nickel were prepared respectively. Under the optimum condition, dl-cystine enantiomer could be separated better with capillary electrochromatography columns coating tetraphenylporphyrin ferrum and tetraphenylporphyrin Nickel than tetraphenylporphyrin Zinc. The resolution of dl-cystine enantiomer could be affected by pH.Chapter V Application in amino acids separation of different open-tubular capillary electrochromatography porphyrins columnsThe five amino acid were separated by seven open-tubular capillary electrochromatography columns coating tetraphenylporphyrin, tetraphenylporphyrin Zinc, tetraphenylporphyrin ferrum and tetraphenylporphyrin Nickel, 5-(m-propylsulfydryloxyphenyl)-10,15,20-phenyl porphyrinate 5-(m-decylsulfydryl-oxyphenyl)-10,15,20-phenyl porphyrinate, 5-(m-hydroxylphenyl)- 10,15,20-phenyl porphyrinate respectively. The different pH conditions were investigated in tetraphenylporphyrin ferrum column, 18 amino acids injections was separated at the pH 2.25 conditions by the columns of the tetraphenylporphyrin ferrum or tetraphenylporphyrin Nickel coating and blank.