Studies On The Method Of Determination Of Pharmaceuticals By Flow Injection-Atomic Absorption Spectrscopy And Flow Injection- Chemiluminescence

This thesis has studied the analytical methods of determination of captopril, reserpine, analgin, urapdil and leucoge by flow injection-atomic absorption spectrscopy (FI-AAS) and flow injection- chemiluminescence(FI-CL). The methods have been applied to the analysis of the samples with satisfactory results. The thesis is divided into seven parts:Part I: Review. A review of the application of flow injection-atomic absorption spectrscopy and flow injection- chemiluminescence in pharmaceutical analsis is given.Part II: Determination of captopril by flow-injection on-line filtration-dilution AAS. A simple, rapid and accurate method for the assay of captopril has been developed. The method is based on the reaction in aqueous solution of captopril with Cu2+ and SCN" to form precipitate quantitatively. The amount of residual Cu2+ can be determined by flow injection on-line filtration-dilution-atomic absorption spectrometry, then the content of captopril can be determined indirectly. The linear range is 2~100ng/mL, the recovery is 97.1%~99.5%, the sampling frequency is lOOh"1. The method has been applied to determine captopril with good results.Part III: Determination of reserpine by flow-injection on-line filtration-dilution AAS. A new method for the assay of reserpine has been developed. It is based on the reaction in aqueous solution of reserpine with Reinecke'salt to form precipitate quantitatively, the amount of residual Cr5* can be determined by flow injection on-line filtration-dilution-atomic absorption, then the content of reserpine can be determined indirectly. The linear range is 25~200ug/mL, the recovery is 97.2 %~102.6%, and the sampling frequency is lOOh'1. The method has been applied to determine reserpine with good results.Part IV: Determination of analgin by flow-injection on-line filtration-dilutionAAS. A simple, rapid and accurate method for the assay of analgin has been developed. It is based on the reaction in aqueous solution of analgin with Cu2+ and SCN" to form precipitate quantitatively, the amount of residual Cu2+ can be determined by flow injection on-line filtration-dilution-atomic absorption spectrometry, then the content of analgin can be determined indirectly. The linear range is 2~100ug/mL, the recovery is 97.0 %~102.5%, the sampling frequency is lOOh"1. The method has been applied to determine analgin with good results.Part V: Ion-pair formation of Bi(III)-iodide with urapidil and its application. A new method for the assay of urapidil has been developed by studying on ion-pair formation of Bi(III)-iodide and urapidil. It is based on the reaction in aqueous solution of urapidil with Bi(III)-iodide to form precipitate quantitatively, the amount of residual Bi3+ can be determined by flow injection on-line filtration-dilution atomic absorption, then the content of urapidil can be determined indirectly. The linear range is 5-100 ug/mL, the recovery is 97.8 %~101.4 %, and the sampling frequency is lOOh"1. The method has been applied to determine reserpine with good result.Part VI: Determination of leucoge by flow injection chemiluminescence. A new flow injection chemiluminescence method for the determination of leucoge was described. The method was based on chemiluminescence reaction of the product degraded from leucoge with cerium(IV) in sulphuric acid medium sensitized by rhodamine B. The CL emission allows quantitation of leucoge concentrations in 0.1~100jig/mL with detection limit of 0.07ug/mL and relative standard deviation was 1.1% (c=10(jg/mL, w=ll) , a sampling frequency of 150 h"'was attained. The method was applied to determination of leucoge in pharmaceutical preparations with recovery of 97.6% and 98.1%.Part VII: Determination of urapidil by flow injection chemiluminescence. A reverse flow injection chemiluminescence method for the determination of urapidil was firstly described. It was found that the CL intensity from the luminol-CIO" system could be enhanced in the presence of urapidil. The increase of CL emission was correlated withurapidi...