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Since then, testing of a representative sample of each produced lot of these pharmaceuticals is required as a part of quality control processes. Hence, an interface\u2010free CE\u2010nanoESI system coupled with MS detection was employed for the development of a simple and economical method for quantitative detection of this contaminant in the valsartan drug substances and finished formulations used as model matrices. In this arrangement, a fused\u2010silica capillary was used as both a separation column and a nanoESI emitter providing high ionization efficiency and sensitivity. The optimized procedure was found to have sufficient selectivity, linearity, accuracy, and precision. The established LOD and LOQ values were 0.3 and 1.0\u00a0ng\/mL, respectively. The practical applicability of the method was tested by analyses of commercially available Valsacor<jats:sup>\u00ae<\/jats:sup> tablets. The results obtained prove that the developed procedure represents a promising alternative to currently available GC\u2010 and LC\u2010based methods. 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