The Application Of Flow Injection Chemiluminescence And Its Combination Of PLS In Pharmaceutical Analysis

Flow injection chemiluminescence makes a feature of fast development and wide application because of its high sensitivity, fast analysis, low cost, wide linear responserange, and simplified operation for trace analysis. Up to now, the FICL analysis has been widely applied in drug analysis, environment and life sciences examination, clinical, mineralogical analysis and immunoassay fields and is becoming one of the most powerful techniques for use in analytical chemistry. It is not only of great theoretical meaning but also of application and guide value for drug clinical authentication and use that chemiluminescence is applied in the pharmac-eutical analysis.In recent years, chemometrics methods and flow injection chemiluminescence method unifies, keeps chemiluminescence high sensitivity, instrument, the equipment is simple, fast advantages, through mathematical processing of data measured by the complex and is not the separation process and draw all the content of coexistence components. In a certain extent traditional chemiluminescence solved the problem of poor selectivity and widening the application range of chemical luminescence, for chemiluminescence detection pioneering a new research direction.This thesis include the following two parts. The first part is the literature revie w, this paper expounds the flow injection chemiluminescence in recent years and che mometrics methods combining chemiluminescence advances in analytical chemistry. The second part was the research reports, Firstly, further research has been done the to improve the sensitivity of existing system, established the determination of two drugs flow injection chemiluminescence analysis. Secondly, against former proce ssing technology applied to complex system chemiluminescence detection was inves tigated. Finally, combing chemometrics multivariate calibrat ion method of chem iluminescence analysis, the separation and pretreatment without realizing complex system of simultaneous determination components. Specific research content as following:PartⅠflow injection chemiluminescence analysis1. Based on the fact salbutamol sulfate could enhance the CL reaction of Luminol-KIO4 and gold nanoparticles(AuNPs) could greatly enhance the chemiluminesen-ce(CL) of this system in alkaline solution, a novel chemiluminescence method for the determination of salbutamol sulfate was developed. The linear range of the wor king curves was 6.0×10-7～1.0×10-5g/ml and the detection limit was 9.1×10-8g/ml. The method was successfully applied to the determination of salbutamol sulfate in tablets.2. A novel chemiluminescence method for the determination of Apomorphini Hydroc-hloridum was developed. It was based on the fact that Apomorphini Hydroc-hloridum could enhance the chemiluminescence intensity from the reaction of luminol with potassium periodate in alkaline medium. The detection limit was 4.4x10"3mg/L. The method has been successfully applied to the determination of Apomorphini Hydrochloridum in urine sample and blood sample with the recov-eries of 97.32%-104.69% and 106.30%～110.57%.3. In hemoglobin (Hb) of catalytic Luminol - H2O2, puerarin chemiluminescence systems have significant inhibition, and inhibition rate Y and the logarithm of puera-rin concentration in certain concentration range lgC linear relationship. According to this phenomenon, this paper establishes a simple, sensitive flow injection chemilu-minescence new methods of determination of puerarin, this method for linear range of 8×10-8g/mL～1×10-5g/mL, method for detection limit 5×10-8g/mL (3a),1×10 "6 g/mL puerarin grain standard solution 11 straight parallel determination, the relati-ve standard deviation is 1.4%. This method have been successfully used in the three clinical pue preparations determination. In addition, combining solid phaseextracti-on technology, this method can also be applied to the determination of puerarin in urine and rat body pharmacokinetic study.PartⅡchemometrics multivariate calibration methods in the application of chemiluminescence analysis1. In this paper, a flow injection chemiluminescence (CL) system has been proposed for the simultaneous determination of metronidazole(MET) and ciprofloxacin(CPLX) using partial least squares (PLS) calibration. This method is based on the kinetic distinction of the CL reactions rates of MET and CPLX. The CL intensity of luminol- KIO4-MET-CPLX was measured and recorder at different reaction times, and the obtained data were processed by the chemometric approach of partial least squares. Under the optimum conditions,the calibration graph of emission intensity was linear in the range of 1×10-6g/ml～8×10-5g/ml and 6×10-6g/ml～8×10-5/gml, and the detection limit of 4.3×10-7g/ml and 9.2×10-7g/ml for individual analysis of MET and CPLX, respectively. The proposed method was successfully applied to the simultaneous determination of both analytes in tablets.2. In this paper, a flow injection chemiluminescence(CL) syetem has been proposed for the simultaneous determination of vitamin C (AA) and Rutin (Rutin) using partial least squares(PLS) calibration. This method is based on the kinetic distinction of the CL reactions of AA and rutin can quantitatively reduce Fe3+ to Fe2+, and that the reaction rates of AA and rutin with Fe3+ are different. The reduced product Fe2+was detected with the luminol-Fe2+-NaOH CL system. The CL intensity was measured and recorded at different reaction times of Fe3+with AA and rutin, and the obtained data was processed by the chemometric approach of PLS. Under the optimum conditions, the calibration graph of CL intensity was linear in the range 0.02～0.6 mg/L and 0.1～20mg/L, and the detection limit of 0.045 mg/L and 8.90 ug/L for individual analysis of rutin and vitamin C, respectively. The relative standard deviations for ten replicate determinations were calculated as2.80% and 1.42% for 0.1mg/L of rutin and 1.0 mg/L vitamin C concentrations, respectively. The proposed method was successfully applied to the simultaneous determination of both analytes in tablets and human urine samples.