The development of the pharmaceuticals brought a revolution in human health. These pharmaceuticals would serve their intent only if they are free from impurities and are administered in an appropriate amount. To make drugs serve their purpose various chemical and instrumental methods were developed at regular intervals which are involved in the estimation of drugs. These pharmaceuticals may develop impurities at various stages of their development, transportation and storage which makes the pharmaceutical risky to be administered thus they must be detected and quantitated. For this analytical instrumentation and methods play an important role. This review highlights the role of the analytical instrumentation and the analytical methods in assessing the quality of the drugs. The review highlights a variety of analytical techniques such as titrimetric, chromatographic, spectroscopic, electrophoretic, and electrochemical and their corresponding methods that have been applied in the analysis of pharmaceuticals. Guided by pharmacology and clinical sciences, and driven by chemistry, pharmaceutical research in the past has played a crucial role in the progress of development of pharmaceuticals. The contribution of chemistry, pharmacology, microbiology and biochemistry has set a standard in the drug discovery where new drugs are no longer generated only by the imagination of chemists but these new drugs are the outcome of exchange of ideas between biologists and chemists.