The determination of certain sulphonamides

Abstract

A new titrimetric method is described for determining certain sulphonamides. The proposed method is based on the fact that N-bromosuccinimide readily and quantitatively brominates an aqueous acidic solution of the sulphonamide and is itself irreversibly reduced to succinimide. The mechanism of the reaction is illustrated. The experimental error is within 5 1 per cent.CEKTAIS sulphonamides, such as sulphanilamide, sulphaguanidine and sulphacet amide, cannot be determined by the silver nitrate meth0d.l Further, sulphanilamide and sulphaguanidine cannot be estimated by the recent complexometric method,2 whose error in case of sulphacetamide sodium amounts to more than 20 per cent.This paper describes a new method for determining these sulphonamides. The proposed method is based on the fact that N-bromosuccinimide readily and quantitatively brominates an aqueous acidic solution of sulphanilamide, sulphaguanidine or sulphacetamide to the corresponding 3,5-dibromo derivative and is itself irreversibly reduced to succinimide, as repreGnted 6v the equation-CHZ-CO, >NBr + H,NH-~SO,-NH.R 2 C I_ HZ-CO'

Determination of sulfa drugs with chloramine-T

“…1-4,6, and 7. For the determination of compound I (Tables IV and V) an aliquot of mixture is analyzed by method B, the following equation being used: compound I (mg) = (mol wt)MVA (1) where VA is volume (mL) for "alone" titration using CAT of molarity M. Thereafter, an equal but separate aliquot of mixture is analyzed by method A to yield a total of two sulfonamides. The second substance is found by difference compound II (mg) of mixt no.…”

“…After cooling, the solution is determined by method A (titer Vn). A third equal aliquot is again hydrolyzed and titrated by method B (titer Vm) ríVii -V,) 1 M---…”

“…The mixture is titrated first by method A to yield titer V:; thereafter, an equal but second aliquot is hydrolyzed by mixing with 10 mL of 10% sulfuric acid and heating in a boiling water bath for 15 min and titrated after cooling by method A (titer Vn). Equation 4is used to determine phthalylsulfathiazole while the other compound is calculated by following sulfamerazine or sulfadiazine (mg) = ~|~M[Vn -)1.5(Vn -V^)] (7) RESULTS AND DISCUSSION A number of reagents can be employed to liberate bromine from acidified potassium bromide (1,12,(14)(15)(16)(17). CAT, however, excells in its ready availability, stability, and easy applicability (18)(19)(20).…”

“…Humans may be exposed to IV-nitroso compounds in a variety of ways, such as ingestion of food, water, or alcoholic beverages, from the consumption of smoking of tobacco, absorption from the air or consumer products, occupational exposure, and in vivo formation within the human digestive system. In vivo formation of iV-nitroso compounds from nitrite and amine percursors has been dem- 1 Present address: Radian Corp., Austin, TX 78766. onstrated (6-8).…”

Volumetric and Gravimetric Analytical Methods for Organic Compounds

“…Sulfonamides. Sulfonamide, sulfanilamide, sulfaguanidine, and so-dium sulfacetamide can be titrated to within ±1% using 1% Ar-bromosuccinimide as titrant (8).…”