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. 2005 Oct 6;6(2):E284–E297. doi: 10.1208/pt060239

Process analytical technology case study, part III: Calibration monitoring and transfer

Robert P Cogdill 1, Carl A Anderson 1, James K Drennen 1,✉
PMCID: PMC2750542  PMID: 16353988

Abstract

This is the third of a series of articles detailing the development of near-infrared spectroscopy methods for solid dosage form analysis. Experiments were conducted at the Duquesne University Center for Pharmaceutical Technology to develop a system for continuous calibration monitoring and formulate an appropriate strategy for calibration transfer. Indcators of high-flux noise (noise factor level) and wave-length uncertainty were developed. These measurements, in combination with Hotelling’s T2 and Q residual, are used to continuously monitor instrument performance and model relevance. Four calibration transfer techniques were compared. Three established techniques, finite impulse response filtering, generalized least squares weighting, and piecewise direct standardization were evaluated. A fourth technique, baseline subtraction, was the most effective for calibration transfer. Using as few as 15 transfer samples, predictive capability of the analytical method was maintained across multiple instruments and major instrument maintenance.

Keywords: process analytical technology (PAT), near-infrared spectroscopy (NIR), tablet analysis, pharmaceutical analysis, calibration transfer

Full Text

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