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Potentiometric and atomic absorption spectrometric (AAS) methods are described for the determination of various sulfonamides in tablets, suspensions, and injections, based on reactions with silver and copper ions. The methods involve direct titration at pH 8, using either a graphite electrode in which silver and copper sulfides have been precipitated, or ion selective electrodes to monitor the potential change. AAS measurements of the excess metal ions after metalsulfonamide reaction are also reported. Results compare favorably with those obtained using USP XIX procedures. The methods described are selective, simple, and precise.

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Simple, rapid, and accurate methods have been developed for determining vitamin Bx in pharmaceutical preparations without prior separation of the vitamin. The methods are based on the desulfurization reaction with potassium plumbite and measurement of the unreacted lead (II) ions at 217 nm using atomic absorption spectroscopy (AAS), or by titration with EDTA at pH 4.5 with the lead ion selective electrode and Gran's plot. The results compare favorably with those obtained using the USP fluorometric method. Recoveries of pure vitamin Bx averaged 99.1%, with a standard deviation of 0.8%, and 99.0%, with a standard deviation of 0.7%, for the AAS and ion selective electrode procedures, respectively.