In the pharmaceutical field, quality control is a fundamental step to ensure the safety and efficacy of drugs. Quality control is based on reliable analytical procedures (APs) that can be developed according to the principles of Analytical Quality by Design (AQbD). AQbD derives from the risk-based strategy Quality by Design, whose application is strongly encouraged in the pharmaceutical field, where quality is essential to ensure the safety and efficacy of drugs. Through the definition of the AP target, called Analytical Target Profile (ATP), the critical factors for the procedure are identified and the hazard for the loss of ATP is minimized. Finally, a region in which the overall quality of the process can be guaranteed with a defined risk of failure, named Method Operable Design Region, is defined. Examples of development of APs dedicated to the quality control of monoclonal antibodies using Infliximab as a lead molecule will be presented. The advantages of an experimental planning based on Design of Experiments will also be shown. This approach allows to gain insight into the hidden aspects of experimental processes. DoE enables risk assessment and mitigation, and its use should be encouraged to achieve scientific goals, gain greater confidence in data, as well as valuable insights, even from negative results. Finally, a workflow for the application of AQbD in the development of APs will be presented.