Separation And Determination Of Some Amine Drugs By Using High Performance Capillary Electrophoresis With Ionic Liquid As A Separation Additive

The ternary mixtures of sorbitol-trehalose-ionic liquid(1-hexyl-3-methyl imidazolium tetrafluoroborate) was added in the borax running buffer as a separation additives. A new method for effective separation of three kinds of aconitum alkaloids of aconitine, mesaconitine, hypaconitine by capillary electrophoresis electrochemiluminescence(CE-ECL) was established in this paper. With this separation additive, an efficiency baseline separation between aconitine and adjacent interfering substances was achieved in Yunnan Baiyao aerosol samples.Especially, the Eu-PBAs chemically modified electrode was used as ECL detection electrode, the aconitine components in external Yunnan Baiyao aerosol samples can be high sensitive quantitative determined by the CE-ECL method. At the same time, the CE-ECL method was applied to quantitative determination of diclofenac diethylamine in the real drugs sample.The dissertation includes following four chapters:Chapter 1: The reviewFirst of all, A brief review of properties, structure and classification of ionic liquids(IL) was summarized, and it’s application in electroanalytical chemistry, extraction chemistry, liquid chromatography analysis, capillary electrophoresis analysis(CE) was introduced briefly. Then, the capillary electrophoresis separation modes and signal detection methods were introduced, meanwhile, the choice of capillary electrophoresis running buffer and it’s application examples in pharmaceutical analysis was summarized. At last, the quantitative determination methods of capillary electrophoresis which applied to medicinal alkaloids and some other amine drugs were concluded, and some applications in amine drugs analysis by using ionic liquids, polyol, non reducing sugar as high performance capillary electrophoresis additives were especially reviewed.Chapter 2: Determination and separation of aconitine by high performance capillary electrophoresis with ionic liquid-sorbitol-trehalose ternary mixtures as separation additives in the external Yunnan Baiyao preparationsUsing ionic liquid-sorbitol-trehalose ternary mixtures as separation additives, a simple and novel method for separation and determination of aconitine in Yunnan Baiyao aerosol samples has been developed by capillary electrophoresis coupled with electrochemiluminescence(CE-ECL) with the Eu-PBAs chemically modified electrode as working electrode. In this work, the effect of electrophoresis separation conditions on the separation ability and detection sensitivity, such as detection potential, concentration and acidity of the running buffer solution, separation voltage and the addition amount of separation additives were examined. Under the optimal experimental conditions, aconitine was baseline separated within 9 min, and the ECL intensity has good linear correlation with aconitine concentration from 1.0×10-7 to1.0×10-5mol/L(r2=0.9998), with the detection limit was 5.4×10-8mol/L. This method was successfully applied to determine the contents of aconitine in Yunnan Baiyao aerosol samples with recoveries between 93% and 104.5%.Chapter 3: Separation of three kinds of aconitum alkaloids mixture by high performance capillary electrophoresis with ionic liquid-sorbitol-trehalose ternary mixtures as separation additivesBase on the Eu-PBAs chemically modified platinum electrode as working electrode, the separation conditions of three kinds of aconitum alkaloids(aconitine,mesaconitine, hypaconitine) was developed by CE-ECL method with separation additives(1-hexyl-3-methyl imidazolium tetrafluoroborate ionic liquid-sorbitoltrehalose ternary mixtures). Under the optimal experimental conditions: borax and boric acid as buffer system, capillary column length 42 cm, electrokinetic injection 10 s, 12 KV, three kinds of aconitum alkaloids were separated within 7min.Chapter 4: Determination and separation of diclofenac diethylamine content in pharmaceutical preparations by high performance capillary electrophoresis with ionic liquid as separation additivesUsing ionic liquid as separation additive, a method for separation and determination of diclofenac diethylamine in diclofenac diethylamine emulgel was developed by CE-ECL method, the Eu-PBAs chemically modified electrode was choosen as working electrode. In this experiment, the effect of some electrophoresisseparation conditions such as the detection potential, concentration and acidity of the running buffer solution, separation voltage, the addition amount of separation additives on the separation ability and detection sensitivity were examined,. Under the optimal experimental conditions, diclofenac diethylamine was separated within 4 min,and the ECL intensity was in proportion diclofenac diethylamine concentration in range of 5.0×10-7 to 1.0×10-5 mol/L(r2=0.9999) with the detection limit was2.6×10-7mol/L. The relative standard deviations of the ECL intensity and the migration time about 5.0×10-6mol/L diclofenac diethylamine were 2.26% and 0.05%,respectively. This method is simple and rapid, it can determine the content of diclofenac diethylamine in diclofenac diethylamine emulgel accurately, the recoveries of method are between 95.9% and 98.9%.