Macroalgae are important source of biologically active compounds which helps in suppression of many harmful diseases. Indian brown macroalgae (Sargassum wightii) aqueous extract was prepared to quantify the polyphenols using LC-MS/MS. The aqueous extract of S. wightii showed special class of polyphenol, phloroglucinol (55.30 mg/kg dry weight) along with gallic acid (0.59 mg/kg dry weight), ferulic acid (12.7 mg/kg dry weight) and caffeic acid (0.59 mg/kg dry weight). Results signify the tremendous scope for the value addition of macroalgae for its potential utilization in the development of functional food and nutraceuticals.