Mass Spectrometry

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The authors describe implementation and performance of a miniaturized NIR analyzer and associated chemometric techniques applied to the monitoring of a drying process for active pharmaceutical ingredients (APIs).

The need to verify cleaning between manufacturing runs presents a special challenge to the analytical chemist. In this article, the principles of ion mobility spectrometry are described, its performance is compared to HPLC for the analysis of cleaning validation samples, and findings are presented from a study to establish the feasibility of using IMS in validating a cleaning verification method.

A paradigm shift is required for chemists and engineers to best utilize chemometrics in their processes. This change demands that one not be too fixated upon ideal textbook thermodynamic models but instead continually check these models using real-time data input and chemometric analysis. The author discusses implementation strategies and the benefits that chemometrics can bring to the process environment.

The authors describe the in-line moisture measurement of a pharmaceutical granulation of lactose, microcrystalline cellulose, and crospovidone in a fluid bed granulator-dryer using top sprayed granulating liquid. A near-infrared (NIR) prediction model was developed for moisture on spectra collected during a calibration run. Subsequent granulations were analyzed for moisture content real-time throughout the granulation and drying process using the NIR process instrument.

What does the accelerating adoption of PAT-based approaches to pharmaceutical manufacturing mean for the makers and users of spectroscopic systems?