Studies demonstrate utility of X-ray powder diffraction (XRPD) for determining process-induced phase transformations in pharmaceutical solids
Studies undertaken at the Department of Pharmaceutical Technology at the University of Bonn, using Panalytical's XPert Pro MPD system, have demonstrated the value of X-ray powder diffraction (XRPD) for detecting process-induced crystallinity changes in pharmaceutical solids.
For samples with a low crystalline content, detection limits were down to around 0.5%, while for samples with a low amorphous content detection limits were less than 1%.
Results were comparable with those using near infrared spectroscopy (NIRS) and significantly more accurate and reliable than those using differential scanning calorimetry.
Crystallinity changes are typically associated with a number of processing steps in the pharmaceutical industry.
Milling, granulation, compression, spray-drying or lyophilisation can all cause disruption of the crystalline structure, leading to the formation of amorphous regions.
The detection of such regions is an important factor in process control because their presence, in either excipients or active ingredients, can have a profound influence on processing behavior and the bioavailability of the active ingredient in the finished product.
This study found both XRPD and NIRS to be precise and accurate methods, each characterised by low detection limits, non-destructive analysis and rapid production of results.
XRPD proved more precise than NIRS for samples with a low crystalline content.
In addition, its high sensitivity for these samples makes it the preferred technique for monitoring crystallisation processes, offering detection of crystallisation at extremely low limits and direct determination of the crystallisation products.
Panalytical is a supplier of analytical instrumentation and software for X-ray diffraction (XRD) and X-ray fluorescence spectrometry (XRF), with more than half a century of experience.
The materials characterisation equipment is used for scientific research and development, for industrial process control applications and for semiconductor metrology.
Panalytical, formerly Philips Analytical, employs around 800 people worldwide.
Its headquarters are in Almelo, the Netherlands.
Fully equipped application laboratories are established in China, Japan, the USA, and the Netherlands.
Panalytical's research activities are based in Almelo (NL) and on the campus of the University of Sussex in Brighton (UK).
Supply and competence centres are located in Almelo and Eindhoven (NL).
A sales and service network is established in more than 60 countries.
The company is certified in accordance with ISO 9001:2000 and ISO 14001.
The product portfolio includes a broad range of XRD and XRF systems and software widely used for the analysis and materials characterisation of products such as cement, metals and steel, nanomaterials, plastics, polymers and petrochemicals, industrial minerals, glass, catalysts, semiconductors, thin films and advanced materials, pharmaceutical solids, recycled materials and environmental samples.
