Pharmaceutical analysis is going through an expeditious progress as the perception of 'multivariate data analysis' (MVA) becomes gradually more assimilated. Pharmaceutical analysis comprises a range of processes that covers both chemical and physical assessment of drugs and their formulations employing different analytical techniques. With the revolution in instrumental analysis and the huge amount of information produced, there must be an up-to-date data processing tool. The role of chemometrics then comes up. Multivariate analysis (MVA) has the capability of effectively drawing a complete picture of the investigated process. Moreover, MVA reproduces the arithmetic influence of variables and their interactions through a smaller number of trials, keeping both efforts and capitals. Spectrophotometry is among the most extensively used techniques in pharmaceutical analysis either direct (single component) or derivative (multicomponent). In addition to these recognized benefits, using chemometrics in conjunction with spectrophotometry affects three vital characteristics: accuracy, precision and robustness. The impact of hyphenation of spectrophotometric analytical techniques to chemometrics (experimental design and support vector machines) on analytical laboratory will be revealed. A theoretical background on the different factorial designs and their relevance is provided. Readers will be able to use this chapter as a guide to select the appropriate design for a problem.