| Studies on the application of flow-injection chemiluminescence method and microdialysis sampling technique in pharmaceutical analysis were carried out in this work. The dissertation is divided into two parts.Part 1 describes pharmaceutical analysis using flow-injection chemiluminescence system. This part consists of four chapters. Chapter 1 reviews the development of the application of chemiluminescence in pharmaceutical analysis since 1990 especially since 1998. The chemiluminescence analysis of 8 kinds of Pharmaceuticals is also concluded in this chapter.Chapter 2 describes the flow-injection chemiluminescence analysis of Paracetamol. The determination of Paracetamol based on its repression on the chemiluminescence emission produced upon mixing a K.3Fe(CN)6 solution with an alkaline luminol solution. The system responds linearly to Paracetamol concentration in the range of 4.0x10-8-1.0xl0-6g/mL with a detection limit of 2.4x10-9g/mL and the relative standard deviation is 2.3% for 8.0x10-7g/mL Paracetamol (n=ll). The method has been applied to determine Paracetamol in tablets, and the results agree well with that by standard method. In addition, the possible reaction mechanism has been discussed as well.Chapter 3 develops a new method for determination of Metronidazole using flow-injection chemiluminescence analysis based on its enhancement on the emission intensity of the chemiluminescence reaction of K3Fe(CN)6 and alkaline luminol solution in basic medium in the presence of K4Fe(CN)e as suppressor. The chemiluminescence intensity is proportional to Metronidazole concentration over the range 2.0x10-6-4.0x10-4mol/L with a detection limit of 1.5x10-7mol/L. The relative standard deviation is 3.6% for 1.0x10-5mol/L Metronidazole (n=ll). The recovery for tablet and injection is 101.6% and 99.9%, respectively. The method has been successfully applied to the determination of Metronidazole in preparations with satisfactory results.Chapter 4 describes the development of a flow-injection chemiluminescencesystem for determination of Thiamazole. The method is based on the chemi-luminescence produced during the oxidation of Thiamazole by KMnO4 in sulphuric acid in the presence of a sensitizer, HCHO. The proposed method is simple, sensitive and inexpensive. The response to the concentration of Thiamazole is linear in the range of 2.0x10-8-8.0x10-6g/mL with a detection limit of 1.8x10-9g/mL. The relative standard deviation is 2.7% for 1.0xlO'7g/mL Thiamazole (n=ll) and the recovery is 98.5%. The method has been successfully applied to assay of Thiamazole in tablets with satisfactory results.In part 2, studies on the application of microdialysis sampling technique combined with optical detection system in pharmaceutical and clinically important biochemical substances were carried out. This part is composed of 5 chapters. The first one is a review concerning the principle of microdialysis, microdialysis instruments and experiment, advantages and limitations of microdialysis, analytical consideration and methodologies, probe calibration methods and status of microdialysis since 1990.Chapter 2 describes the development of a microdialysis-flow injection-chemiluminescence detection system for studying the drug-protein interaction, which has been successfully applied to the study of interaction between Metronidazole and human serum album (HSA). The microdialysis probe was calibrated and its recoveries at different perfusion rates and two different temperatures were measured. Under 5uL/min of perfusion rate and 37 of temperature, the recovery was 25.2% for Metronidazole. The interaction parameters of studied drug to HSA were in vitro estimated by Scatchard method and Klotz analysis. The result compared well with that in literature, which means that the proposed system was valid for determination of interaction between drug and protein using relatively simple instrument.Chapter 3 describes the development of a microdialysis-flow injection-fluorescence detection system for in vivo on-line monitoring of calcium...
|
PDF Full Text Request