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Development in the bioanalytical technology & the application of pharmacokinetic (PK) principles has created a synergistic partnership that plays a vital, influential role in the discovery and development of new medicines. In the bioanalytical investigation a fast, sensitive, accurate and reproducible high performance liquid chromatography-mass spectrometry method has been developed & validated for the quantitative estimation of DOXAZOSIN in human plasma using DOXAZOSIN D8 used as internal standard by solid phase extraction (SPE) technique.Doxazosin, is an oral drug used for treating high blood pressure and symptoms of benign prostatic hyperplasia, it belongs to the class of alpha -1 adrenergic blockers. It prevents Norepinephrine that is released by nerves from binding to alpha -1 receptors on smooth muscles surrounding blood vessels and in prostate and bladder by blocking the effect of norepinephrine, Doxazosin relaxes the smooth muscles, relaxation of smooth muscle surrounding blood vessels causes them to enlarge (dilate) and thereby reduces blood pressure.