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SPECTROSCOPY


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Independence and Dependence in Calibration: A Discussion of FDA and EMA Guidelines


Rodolfo J. Romañach, PhD


Engineering Research Center for Structured Organic Particulate Systems (C-SOPS) Department of Chemistry, University of Puerto Rico, Mayaguez Campus, Mayaguez


Introduction


Two recently published FDA and EMA documents describe expectations for the submission of spectroscopic methods to the regulatory agencies and are important advancements for the implementation of modern non-destructive analytical methods in the pharmaceutical industry.1,2


Both documents are focused on the description of near


infrared spectroscopic methods. However, the FDA Draft Guidance indicates that the same fundamental concepts of validation may be applied to Raman, X-ray, and other Process Analytical Technology (PAT) analytical techniques. These expectations must become part of the plans or procedures for the development of PAT spectroscopic methods.


The FDA and EMA documents should not be considered a checklist for the validation of methods to be submitted to regulatory agencies. Regulatory submission must include justifications of the strategies followed for the development of calibration models; strategies that define how scientists work. The documents encompass chemometrics; a scientific discipline that is based on careful planning and observation of data to extract the maximum information. The documents describe the information needed to demonstrate the validation of the meth- ods. Validation requires evidence that prediction performance is valid, and a calibration model should be evaluated according to its purpose.3


The development of a calibration model for a pharmaceutical product requires extensive planning.4


learning phase where scientists study the composition of a formulation and the pharmaceutical process and define method requirements and performance criteria. This initial planning has been described as “general steps in an analytical Quality by Design strategy”.5


Validation requires thinking, planning and establishing clear


objectives. Thus, the FDA and EMA documents should not be viewed as checklists for the submission of PAT and spectroscopic methods.


Model development starts with a


Thus, the


planning entails the selection of an analytical technique and may also include a risk assessment to identify factors that may affect the method’s performance.5


calibration model that will be suitable to predict future production 48 | | May/June 2016 This planning stage is essential to obtain a


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