| Chemiluminescence method has been widely used in the analysis of food, medicine, biology, and agriculture due to its characteristics of high sensitivity, wide linear range, simple equipment, convenient operation, rapid analysis and easy automation. This thesis consists of two parts. In the first part, the development history and basic principle of chemiluminescence, main determination systems including Fenton and analogous Fenton reaction systems are briefly reviewed. In the second part, the development of Fe3+-H2O2-calcein system for chemiluminescence determination of pharmaceuticals is presented, the optimal conditions and mechanism of chemiluminescence reaction are reported. The main work done is as follows:1. A novel chemiluminescence (CL) system was established for the determination of inosine in pharmaceutical preparations. It was shown that a weak CL signal was observed when Fe3+-H2O2mixed with calcein solution. The CL intensity was increased significantly when inosine was added to the reaction system. The extent of increase in the CL intensity had a good stoichiometrical relationship with inosine concentration. Based on this, we developed a new method for the determination of inosine using a flow injection chemiluminescence (FI-CL)technique. Under the optimal conditions, the linear range of inosine concentration was8.0×10-7-2.0±10-5mol·L-1with a detection limit of2.4×10-7mol·L-1, and the RSD was2.9%for2.0×10-6mol·L-1inosine (n=11). This method was successfully used in the determination of inosine in tablets and injection with satisfactory results. The possible reaction mechanism of the CL system was discussed.2. In an acidic medium, the chemiluminescence intensity of Fe3+-H2O2-calcein system was significantly enhanced when gentamycin sulfate was added. Based on this, a method for determination of gentamycin sulfate using flow-injection chemiluminescence technique was established. Under the optimal conditions, the linear range of CL intensity and the concentration of gentamycin sulfate was in the range of4.6×10-1～4.6×10-6mol·L-1with a detection limit of3.6×10-6mol·L-1. The relative standard deviation was1.7%for3.6×10-6mol·L-1gentamycin sulfate (n=11). This proposed method had been successfully used for the determination of gentamycin sulfate in injection, the results had no significant difference with that obtained by ultra-violet spectrophotometry. The mechanism of gentamycin sulfate enhancing the CL intensity of Fe3+-H2O2-calcein system was also investigated.3. It was observed that ribavirin could enhance the CL intensity of Fe3+-H2O2-calcein chemiluminescence system in acidic medium. Based on this phenomenon, a new chemiluminescence method for determination of ribavirin was established. The reaction mechanism was investigated. Under the optimal condition, the linear range of ribavirin was4.1×10-7～2.0×10-5mol·L-1with a detection limit of3.1×10-7mol·L-1, the relative standard deviation was1.4%for1.0×10-6mol·L-1ribavirin (n=11). This method had been used for determination of ribavirin in tablet and injection with satisfied results.4. In acidic medium, a weak chemiluminescence (CL) was observed in Fe3+-H2O2-calcein system and1,10-Phenanthroline could enhance the CL intensity. It was showed that a significantly inhibitory effect in CL signal was observed when L-dopa was added to the reaction system. The decrease extent of the CL intensity was of a good stoichiometrical relationship with L-dopa concentration. Based on this, a new method for determination of L-dopa using flow injection chemiluminescence technique was developed. Various factors influencing the CL signal were investigated and the possible mechanism was also discussed. Under the optimal conditions, the linear range of L-dopa concentration was2.0×10-8～2.0×10-6mol/L with a detection limit of1.2×10-8mol/L, the relative standard deviation was1.1%for2.0×10-7mol/L L-dopa (n=11). This method was successfully used in the determination of L-dopa in injection and tablet, with satisfactory results. |
PDF Full Text Request