Determination of some sulphonamides by sequential injection analysis with chemiluminescence detection

Determination of a group of sulphonamides (sulphanilamide, sulphacetamide, sulphathiazole, sulphadimidine, sulphafurazole, sulphamethoxypyridazine, su lphaguanidine) using sequential injection analysis (SIA) technique with che miluminescence (CL) detection has been devised. The CL signal was emitted d uring the oxidation of sulphonamides by potassium permanganate in sulphuric acid medium. The lab-made SIA system consisted of a 2.5 mi Cavro syringe p ump, eight-port Vici Valco selection valve and a lab-modified Spectra-Physi cs FS 970 fluorescence detector. It was controlled by a PC with use of orig inally compiled LabVIEW((R))-suppotted software. Concentration, volume of r eagents and Row rate were optimised by a simplex method. A number of enhanc ers was tested to increase the CL signal. The optimum conditions and sequen ce of injected zones for sulphanilamide (model substance) were: 0.1 M gluta raldehyde 45 mul, sample 50 mul; 0.5 M H2SO4 45 mul; 1 mM KMnO4 46 mul and 100 mul s(-1) Row rate. The transient CL signal (lambda greater than or equ al to 390 nm) was recorded after a single reversal of the flow. Calibration curves relating the intensity of CL (peak heights) to the concentration of the analytes were curvilinear (of the second polynomial order) with rectil inear sections typically in the range approximate to0.01-0.5 mM sulphonamid e. The sample throughput was 120 h(-1). The proposed method has been applie d for the assay of sulphacetamide and sulphafurazole in pharmaceutical dosa ge forms. The SIA results did not show any statistically significant differ ence from those obtained by titrimetry according to USP XXIV. (C) 2001 Else vier Science B.V. All rights reserved.