Application Of HPLC With Post-column Chemiluminescence Detection To Environmental And Pharmaceutical Samples

At present, high performance liquid chromatography (HPLC) has mostly been used to enhance the selectivity of analytical methods, because of its high efficiency for separation of analytes from various interfering substances. One of the major research areas about HPLC involves the development of sensitive detection methods. Significantly more sensitive detection can be realized by HPLC when the analytes are subjected to the use of chemiluminescence (CL) detection. The chemiluminescence (CL) detection system combined with HPLC separation method can offer excellent analytical selectivity and sensitivity. No doubtably, chemiluminescence linked to HPLC will be widely applied in environmental science, biological science, pharmaceutical science and clinical science.The thesis consists of two parts. One is a review related to the application of HPLC with post-column chemiluminescence detection to environmental and pharmaceutical samples. Emphasis is taken on the development in the recent ten years.The other is research reports which is composed of 4 components as follows. 1) simultaneous determination of N, N-Dimethylaniline and phenol in wastewater by high-performance liquid chromatography with chemiluminescence detection; 2) rapid determination of rudimental trace aniline in indigotine by reverse phase HPLC; 3) determination of the levels of tetracycline and oxytetracycline residues in liver tissue by HPLC-CL; 4) rapid determination of Shikimic acid in taxodium distichum by ion-suppression reversed-phase HPLC. 1. Simultaneous Determination of N, N-Dimethylaniline and Phenol inWastewater by High-Performance Liquid Chromatography with Chemilumineseence DetectionA method using HPLC-CL linkage was developed for simultaneous determination of N, Af-dimethylaniline and phenol in wastewater, based on the strong sensitive chemilumineseence of the luminol-K3Fe (CN) 6 systems in alkaline medium. The separation was carried out on a Hypersil ODS column with a mobDe phase of ethanol-0.01% triethylamine (2:1,V/V). The linear ranges for N, W-dimethylaniline determinations were 2.0 X 10~7 g/mL~2.5 X10"5 g/mL and 4.0 X10'5 g/mL~ 1.5 X10"4 g/mL with a detection limit (3a) of 1.20 X10"* g/mL. The relative standard deviation for 5.0 X lO^g/mL A^W-dimethylaniline was 1.4% (n = 6).The range for phenol was from 5.1X10'7g/mLtol.3X10^ g/mL, and a detection limit (3a) of^SXlO^g/mL could be obtained. The method can be useful for the determination of N, AT-dimethylaniline and phenol in some environmental samples.2. Rapid Determination of Rudimental Trace Aniline in Indigotine by Reverse Phase HPLCAn accurate and reliable reverse phase HPLC method was established for the determination of rudimental trace aniline in indigotine. Aniline can be separated on YWG-C18 (5um,300mmx5mm ID) column by using methanol: water=70:30 as mobile phase with UV detector at a wavelength of 285nm.The standard curve was linear in the concentration range 6.92 X 10"8gAnL~ 3.59 X lO^g/mL and the correlation coefficient was 0.999 7. The recovery and RSD was 98.34%~98.36% and 1.84%~3.03%(n = 5)respectively. The detection limit was 2.02X lO*g/mUS/N= 3). The method has been successfully applied to the determination of rudimental trace aniline in indigotine, which proved to be simple and rapid.3. Determination of the Levels of Tetracycline and Oxytetracycline Residues in Liver Tissue by HPLC-CLAn HPLC-CL linkage method was developed for simultaneous determination of Oxytetracycline and tetracycline in animal liver tissues, based on the strong sensitive chemilumineseence of the CH3CN-H2O2 system in alkaline medium. The separation was carried out on a Hypersil ODS column with a mobile phase of CH3CN: HCON...