A Procedure for Developing Quantitative Near Infrared (NIR) Methods for Pharmaceutical Products

Abstract

The pharmaceutical industry uses procedures to describe all the instructions needed to perform a process in a consistent manner. Procedures are based on process knowledge and the desire to consistently meet desired specifications. This chapter proposes a procedure for the development of NIR partial least squares (PLS) calibration models for pharmaceutical applications. The chapter captures the lessons learned for more than a decade in studies where NIR spectroscopy has been used for quantitative determinations of drug concentration, moisture, polymorphs, and other important applications. Two examples of recent initiatives to develop NIR calibration models in a more efficient manner reducing the number of calibration samples are also discussed. The procedure differs from previously published guidelines since it is based on specific examples of method validations for pharmaceutical processes and provides clear instructions for method development and validation. The procedure and tutorial should advance the implementation of near infrared spectroscopic (NIRS) quantitative methods in the pharmaceutical industry.