A Special "Thank You" 
to our event sponsors

The ICDD is pleased to present the second symposium on Pharmaceutical Powder X-ray Diffraction, December 9-12, 2002 in Concordville, PA, U.S.A. PPXRD-2 focused on topics of interest to scientists and engineers in the pharmaceutical industry using powder x-ray diffraction. The ICDD hopes to create a forum for these two fields to discuss latest developments, exchange ideas and gain knowledge from valuable lectures all surrounding the XRD and pharmaceutical industries. 

PPXRD-2, December 9-12, 2002
By John Faber
ICDD Principal Scientist 

The International Centre for Diffraction Data (ICDD) organized the 2nd Pharmaceutical Powder X-ray Diffraction Symposium, PPXRD-2.  The Symposium was held in Concordville, Pennsylvania, USA on 9-12th December and had over 70 participants.  The focus of the Symposium was on high-throughput crystallization and screening, polymorph characterization, and  powder pattern indexing.  The attendance was truly international with half the participants coming  from 12 different countries. 

A companion workshop, held on December 12th , 2002 focused on practical guides to powder pattern indexing and a discussion on round robins that can be used to help researchers compare their instrument performance with others in the pharmaceutical industry.  There were 16 registrants for this hands-on Workshop.  The workshop focused on the steps in going from data collection through analysis to an indexed pattern. Examples and comparisons were made between conventional commercial X-ray equipment and synchrotron sources.

The first day was dedicated to acquisition and analysis of XRPD data.  Creative approaches in pre-formulation and formulation were discussed.  A comparative analysis between brand name drugs and generic drugs was given.  Several presentations discussed the advantages of capillary sample holders, especially with single characteristic wavelength monochromators and parallel beam geometries.  The second day focused on polymorph characterization.  Results from challenging problems, including for example, determining the dynamics of dehydration in indapamide hemihydrate, using ‘clustering’ of low-quality XRPD patterns for phase identification, characterization of four polymorphs of fananserine, and high-throughput crystallization techniques that allowed up to ~300 crystallizations per day for a single lead compound were also clearly explained.  The fananserine work showed the opportunity to connect structural results from X-ray powder diffraction with thermodynamic properties.  Studies using structure determination techniques were discussed on a wide range of examples including zopiclone, anhydrous caffeine (Z’=5) and a compositionally disordered form of ranitidine HCl form 2.  There were strong contributions from academia, pharmaceutical industry, analytical laboratories, equipment manufacturers and database organizations in all sessions. 

The third day session on regulatory and patent issues focused on a number of well-known litigation cases including cefadroxil and ranitidine hydrochloride.  The discussion focused on distinguishing differences between how courts interpret X-ray diffraction patents and how scientists interpret X-ray powder diffraction patterns.  This session ended with several tutorial talks on SAXS and SANS.  The focus was on contrast matching and other techniques to characterize length scale distributions up to several thousand Angstroms. 

The fourth day Workshop featured lectures and a hands-on computer work (using WINPLOTR and FULLPROF) by Prof. Daniel Louër on Indexing.  Able assistance and lectures were provided by Dr. Jim Kaduk, Dr. Arnt Kern, Dr. Peter Varlaskin, and Dr. Fangling Needham.    

The ICDD announced an exciting new relational database of organic materials targeted for pharmaceutical analyses.  This product called PDF-4/Organics 2003 is immediately available containing 24,385 experimental entries and 122,816 calculated patterns.  The database has more than 31 searchable fields,  provides fully digitized powder patterns for both experimental and calculated patterns and contains integrated display software. This new database results from collaborations with the Cambridge Crystallographic Data Centre. Integrated data analysis packages utilizing the PDF-4/Organics database are available from several vendors. 

I would like to acknowledge the excellent contributions and team effort from the PPXRD-2 Organizing Committee: 

Dr. Tomas Blanton, Eastman Kodak Company, Rochester, NY, USA
Dr. Harry G. Brittain, Center for Pharmaceutical Physics, Milford, NJ, USA
Prof. Noriaki Hirayama, Tokai University, Shizuoka, Japan
Dr. Arnt Kern, Bruker AXS GmbH, Karlsruhe, Germany
Prof. Daniel Louër, University of Rennes, Rennes cedex, France
Dr. Peter Munk, Panalytical, Almelo, The Netherlands
Dr. Fangling Needham, ICDD, Newtown Square, PA, USA
Dr. Richard Ortega, Rigaku, Inc., The Woodlands, TX, USA
Prof. Peter Stephens, SUNY Stony Brook, Stony Brook, NY, USA
Dr. Gregory Stephens, Eli Lilly and Company, Indianapolis, IN, USA
Dr. Peter Varlashkin, GlaxoSmithKline, Research Triangle Park, NC, USA
Dr. John Faber, Chairman of the PPXRD-2 Organizing Committee

PPXRD Coordinators: T. Maguire, L. Mooney, and D. Flaherty


For more information on future PPXRD events please email: ppxrd@icdd.com.