Investigation Of Aerodynamic Force Capillary Microdrop-injection-Chemiluminescence System And Its Applications

This thesis consists of two parts. The first part is review. And the second one is research reports.The review includes the history, principle and its applications of chemiluminescence(CL). And the major development of CL analyzer, especially the two basic sampling-injection modes for CL analysis is emphasized. The two basic sampling-injection modes, traditionally, batch and flow methods have both of the advantages and the intrinsic disadvantages. We combine the advantages in the two basic sampling-injection modes so as to eliminate the phenomena of sample zone dilution and spreading in flow method and avoid the poor precision due to variations in mixing in batch method. So a novel aerodynamic force capillary microdrop-injection-chemilurninescence(AFCM-CL) system is proposed. The proposed method in comparison with known batch and flow methods is very sensitive, precise, simple, rapid and miniature with the evaluation of the new system according to using several known chemiluminescence systems.In part two, the AFCM-CL system has been applied satisfactorily to the determination of the ethamsylate, omethoate, benzoyl peroxide, capreomycin sulfate and ampicillin respectively.1. The ethamsylate is directly oxidized by dissolved oxygen in the presence of hexacyanoferrate(III) to generate a CL signal in sodium hydroxide medium. With the AFCM-CL system the ethamsylate has been determinated. The analysis sample volume is only about 7-8@L. The system shows that the ethamsylate is detected linearly in the concentration range from 5.0×10-10 to 1.0×10-6 g/mL. The detection limit is 1.4×10-10 g/mL(mass concentration is 1.1 pg). The relative standard deviation is 3.1% at 2.5×10-8 g/mL (n = 7).2. A novel aerodynamic force capillary microdrop-injection-chemiluminescence system for the determination of omethoate is proposed based on the florophoruscompound produced from omethoate reacted with sodium fluoride and using mercury ion as the catalyst oxidize luminol-H2O2 to generate a CL signal. The system shows that the omethoate is detected linearly in the concentration range from 1.0×10-7 to 5.0×10 g/mL. The detection limit is 4.0×10-8 g/mL(mass concentration is 320 pg). The relative standard deviation is 3.7% at 3.0×10-6 g/mL (n = 11). It has been successfully applied to determination of trace omethoate residue in vegetable.3. A novel aerodynamic force capillary microdrop-injection-chemiluminescence system is proposed. In this system, the volume of sample is only several microlitres. To evaluate the applicability of the proposed method, a determination of benzoyl peroxide(BPO) is examined based on the directly oxidation of luminol by BPO. The system shows that the BPO is detected linearly in the concentration range from 5.0×10-10 to 1.0×10-6 g/mL. The detection limit (signal-to-noise ratio = 3) is 1.4×10-10 g/mL for BPO(mass concentration is 1.1 pg), which is the best result reported so far. The relative standard deviation (n = 11) is 1.5% for 2.0×10-8 g/mL BPO.4. The weak chemiluminescence(CL) is produced from the reaction of capreomycin sulfate with the potassium ferricynide in the alkaline solution. The CL intensity is enhanced in the presence of potassium ferroyanide. The proposed method has a linear range of 4.0×10-8 -2.0×10-6 g/mL, 4.0×10-6 g/mL~3.5×10-5 g/mL, with a RSD of 2.0% (n = 11, C = l.0×10-7 g/mL), 3.1% (n = 11, C = 1.01×10-5 g/mL)respectively. The detection limit is 2.0×10-8 g/mL. The method has been successfully applied to the determination of capreomycin sulfate in capreomycin sulfate for injection.5. The ampicillin is directly oxidized by hexacyanoferrate(III) to generate a CL signal in sodium hydroxide medium. With the AFCM-CL system the ampicillin has been detected linearly in the concentration range from 1.0×10-6 to 2.0×10-4 g/mL. The detection limit is 5.0×10-7 g/mL(mass concentration is 400 pg). The relative standard deviation is 3.3% at 3.0×10-5 g/mL (n = 7). This method has been successfully applied to the determination of ampicillin in urine sam...