Separation And Analysis Of Some Amine Drugs By Using Capillary Electrophoresis With A Ternary Ionic Association Gel As The Separation Additive

In this thesis,because formaldehyde is used as a main N-methylation derivatization reagent for two amine drugs,tranexamic acid and amantadine hydrochloride,those reaction products can produce a very strong electrochemiluminescence signal when coexisting with tris（2,2’-bipyridine）ruthenium（II）.Based on this principle,a new method has established for the separation and analysis of two amine drugs by capillary electrophoresis coupled with chemiluminescence detection（CE-ECL）.In the electrophoretic analysis experiments,a ternary ionic association gel,Mg²⁺-trehalose-SiO₃^2-（MTS-gel）,has been used as a separation additive for the first time,which can greatly improves the electrophoretic separation efficiency.In addition,under the premise of using MTS-gel as the separation additive,when a mixture standard sample containing four amino acids is accepted to be the probe sample,the separation efficiency of the quartz capillary column coating with single-walled hydroxylation carbon nanotube/chitosan composite has been evaluated by pre-column derivatization CE-ECL method.The main research contents are as follows:Chapter one:The overview on this research fields is presented.In this chapter,the related knowledge of capillary electrophoresis technology,which includes the development trend,separation principle and separation additives about capillary electrophoresis technology,was introduced in detail.Especially,the several main detection methods that can be coupled to capillary electrophoresis are also reviewed.Additionally,the concept and principles of electrogenerated chemiluminescence and development of capillary electrophoresis coupled with electrochemiluminescence detection technique（CE-ECL）are briefly summarized,and some application examples of CE-ECL method in the field of analytical chemistry have been outlined.Chapter two:Determination of tranexamic acid content in essential cosmetics by pre-column derivatization capillary electrophoresis coupled with electrogenerated chemiluminescence detection.In this chapter,N-methylation of tranexamic acid yields an unique derivative,which generate strong co-luminescence signals in the presence of an electrochemiluminescence reagent such as Ru（bpy）₃²⁺.Using this principle,we established a highly selective analytical method based on pre-column derivatization capillary electrophoresis coupled with electrogenerated chemiluminescence detection for determining the tranexamic acid content in essential cosmetics.The addition of a ternary ionic association gel,Mg²⁺-trehalose-SiO₃^2-,in the components of background electrolyte greatly improved the electrophoretic separation efficiency.Under the optimized assay conditions,two electrophoretic peaks attributed to the derivatives of tranexamic acid and its internal standard（sarcosine）were completely separated in 500 s,and their electrophoretic peak intensities ratio showed a good linear relationship with the initial concentration of tranexamic acid in the range of 10-750μmol/L（correlation coefficient R²=0.9993）.The limit of detection was estimated to be 3.6μmol/L（S/N=3）.Moreover,the internal standard method was further applied to the quantitative determination of tranexamic acid content in three kinds of toothpaste and two kinds of nutrient solutions in facial masks.The results showed that the average tranexamic acid content in three toothpaste samples was 4.05,0.24,and 6.06 mg/g,while that in two facial masks was 51.30 and 7.98 mg/mL.The recoveries for the above-mentioned samples were within the range 92.5%to 104.0%,implying satisfactory results.Chapter three:Determination of amantadine hydrochloride in drug samples by capillary electrophoresis using a modified column coated with the single-walled hydroxylation carbon nanotube/chitosan composite.In this chapter,applied a modified quartz capillary coated with the single-walled hydroxylation carbon nanotube/chitosan composite as separation column and the MTS-gel as a separation additive,we had studied the quantitative assay methodology of amantadine hydrochloride by using pre-column derivatization capillary electrophoresis coupled with electrogenerated chemiluminescence detection（CE-ECL）.In the experiments,the many influencing factors that include the critical reaction conditions in pre-column derivatization process of amantadine hydrochloride,the working conditions of electrophoretic separations and detection parameters relating to the electrogenerated chemiluminescence signal were investigated.Under the optimal experimental conditions,the electrophoretic peaks of amantadine hydrochloride and the internal standard substance（sarcosine）added to the sample at a fixed concentration level could completely reach baseline separation within 450 s,and their peaks area ratio(A_AH/A_Sar)showed a good linear relationship to the initial concentration value of amantadine hydrochloride in the two segment range of 10-250μmol/L(A_AH/A_Sar=-0.1509+0.0942C_AH,R²=0.9995)and 400-750μmol/L(A_AH/A_Sar=-30.1729+0.1133 C_AH,R²=0.9991),respectively.The detection limit was also estimated to be 2.4μmol/L（S/N=3）.In addition,the new analytical method had been applied to the determination of amantadine hydrochloride content in several anti-cold medicaments.The recoveries for the real samples were between 90.2%and 102.9%,and the results were satisfactory.Chapter four:Evaluation of electrophoretic separation efficiency of modified quartz capillaries coated with several nano-materials/chitosan composite.In this chapter,with a mixed standard amino acid sample containing arginine,alanine,glycine and phenylalanine as an indicating sample and the ternary ionic association gel（MTS-gel）as the separation additive,we investigated the electrophoretic separation behavior of an indicating sample by pre-column derivatization CE-ECL method.When Mg²⁺ion in the the process of synthesis reaction of MTS-gel was replaced Ca²⁺and Sr²⁺belonging to the same main group of elements,the two ternary ionic association gels had also been synthesized as the separation additives,and their action contributing to the electrophoretic separation efficiency of a mixed standard amino acid sample had been comparatively studied.From experimental results,the four amino acid derivatives in the indicating sample could be effectively separated by the modified quartz capillary column coated with the single-walled hydroxylation carbon nanotube/chitosan composite.In particular,when using the MTS-gel gel as a separation additive simultaneously,the total separation efficiency of electrophoretic separation for a mixed standard amino acid sample would be significantly enhanced by the mutual promotion mode.