Spring Pharmaceutical Synchrotron X-Ray Powder Diffraction Workshop

6th - 8th May 2018

Purdue University
The SPS-XRPD 2018 workshop marked the inauguration of an annual series of events aimed at providing the pharmaceutical industry with up-to-date information on cutting-edge analytical tools and methodologies involving synchrotron radiation and related techniques. This initiative has been ongoing, with the exception of the years 2020 to 2022 due to pandemic-related restrictions. These workshops serve as a platform to address challenges that conventional laboratory instrumentation cannot effectively tackle.

The organizing committee for this workshop was composed of representatives from prominent institutions, including Excelsus Structural Solutions, Purdue University, Argonne National Laboratory and Improved Pharma.
Noteworthy aspects of the event included:
  • A dedicated session focused exclusively on the application of the emerging Pair Distribution Function method. This session delved into the structural characterization and quantification of amorphous and nano-crystalline solid formulations, a field that has garnered increasing interest in recent years.
  • To enhance the workshop experience, on the afternoon of May 6th, a complimentary "XRPD refreshers" session was provided. This session was tailored for industrial participants who may not be familiar with X-Ray Powder Diffraction and the advantages of using synchrotron radiation. Its goal was to make the two-day workshop more accessible and valuable to a wider audience.

DAY 1 - 7TH MAY 2018

8:30 am – 8:45 am Opening remarks: Mission and structure of the Spring Pharmaceutical Synchrotron XRPD workshop
  • S. Byrn - Purdue University, USA
  • F. Gozzo - Excelsus Structural Solutions, Switzerland & Belgium

8:45 am – 10:25 am Applications of XRPD for Phase Identification throughout Pharmaceutical Product Development
  • Patel - Bristol-Myers Squibb, USA
Compression induced phase transformation: a formulator's perspective
  • K. Thakral - Upsher-Smith Laboratories LLC & University of Minnesota, USA
The "Form Selection Process" in the Pharmaceutical Industry: The Importance of being Earnest
  • Daldosso – Aptuit, Italy
The Impact of qualitative and quantitative synchrotron-XRPD trace analyses on the characterization of pharmaceuticals
  • Gozzo - Excelsus Structural Solutions, Switzerland & Belgium
10:25 am – 10:55 am Coffee break
10:55 am – 12:20 pm Recent developments in PDF analysis of organics and pharmaceuticals
  • J. L. Billinge - Columbia University and Brookhaven National Laboratory, USA
PDF analysis of organic and molecular systems - quirks and peculiarities
  • Whitfield - Excelsus Structural Solutions, Switzerland
Synchrotron x-ray PDF from amorphous pharmaceuticals
  • Benmore - Advanced Photon Source, Argonne National Laboratory, USA
12:20 pm – 1:20 pm Lunch, coffee and networking
1:20 pm – 2:35 pm xINTERPDF: a GUI program for analyzing intermolecular pair distribution functions of organic compounds from X-ray total scattering data
  • Shi - Abbvie Inc, USA
Characterization of Mesomorphous Pharmaceuticals Using Pair Distribution Function
  • Atassi - Pulmatrix Inc, USA
Assessment of Processing Induced Structural Disorder in Pharmaceutical Solids by Synchrotron Total Scattering
  • S. Chen - Abbvie Inc, USA
2:35 pm – 3:50 pm Monitoring phase transformations in formulations
  • Suryanarayanan - College of Pharmacy, University of Minnesota, USA
Probing crystallization of drugs using synchrotron radiation
  • Taylor - Department of Industrial and Physical Pharmacy, Purdue University, USA
Parts per Million PXRD through Nonlinear Optically Guided Analysis
  • G. J. Simpson- Department of Chemistry, Purdue University, USA
3:50 pm – 4:20 pm Coffee break
4:20pm -6:00 pm Structure and Analysis of Amorphous Dispersions
  • S. Byrn Purdue University, USA

Polyamorphism of D-mannitol: Structural studies by Synchrotron X ray diffraction
  • Yu - Department of Chemistry, University of Wisconsin Madison, USA

Using Containerless Methods   to Synthesize and Characterize
Amorphous Pharmaceuticals
  • R. Weber - Materials Development, Inc. and Argonne National Laboratory, USA

Pharmaceutical amorphous solid dispersions characterized by Synchrotron X-ray diffraction and Pair Distribution Function method
  • G.L.B. de Araujo - University of Sao Paulo, BraziI
6:00 pm – 6:30 pm Flash presentations of posters
6:30 pm – 7:30 pm Standing dinner during poster session
7:30 pm - 9:30 pm or longer
Guidelines for generating  reliable experimental  PDF of pharmaceuticals ( PDF experts discussion, but open to Interested participants)


DAY 2 - 8TH MAY 2018

8:30 am - 8:45 am
Current treatment of crystalline forms under US and EP patent law
  • Weingarten - Finnegan, Henderson, Farabow, Garrett & Dunner, LLP, USA
8:55 am – 9:55 am The XPDF beamline at Diamond Light Source
  • Chater - Diamond Light Source, UK
X-ray Powder Diffraction Facilities available at the Advanced Photon Source
  • Toby - Advanced Photon Source, Argonne National Laboratory, USA
The ESRF powder diffraction beamlines
  • SIides provided by A. Fitch - European Synchrotron Radiatlon Facility, France
The MS beamline at the Swiss Light Source
  • SIides provided by N. Casati - Swiss Light Source, Switzerland
Powder Diffraction Capabilities at NSLS-II ( Brookhaven )
  • J. L. Billinge - Columbia University and Brookhaven National Laboratory, USA
10:10 am – 10:40 am Coffee break
10:40 am – 12:20 pm Advanced quantitative phase analysis methods to support the Industrial drug development process
  • Reinle-Schmitt - Excelsus Structural Solutions, Switzerland
Crystal Structures of Large-Volume Commercial Pharmaceuticals
  • A. Kaduk - North Central College, Illinois Institute of Technology and PolyCrystallography Inc. USA
Powder Diffraction FileTM Coverage of Polymers used in Pharmaceutical and Biomedical Applications
  • N. Blanton - International Centre for Diffraction Data, USA
The GSAS-II software package
  • R. Von Dreele & B.Toby - Advanced Photon Source, Argonne National Laboratory, USA
12:20 pm – 1:20 pm Lunch, coffee and networking
1:20 pm – 2:10 pm In house and synchrotron based atomic PDF studies on non­crystalline drugs: Is there room for both?
  • Petkov - Department of Physics, Central Michigan University, USA
X-Ray Total Scattering Analysis on Laboratory Instrumentation
  • Beckers - Malvern Panalytical B. V., The Netherlands
2:10 pm – 3:30 pm Meet the experts
3:30 pm – 4:00 pm Workshop wrap up (what pharma industry needs? what can we provide?)


Special session: 'XRPD Refreshers: an informal tutorial on X-Ray Powder Diffraction (XRPD) and Synchrotron X-Ray Powder Diffraction (S-XRPD)' 
Fabia Gozzo, Pamela Whitfield and Mathilde Reinle-Schmitt, Excelsus Structural Solutions
Robert von Dreele, Argonne National Laboratory, Chicago

Part1: Crystalline drugs and their diffraction patterns
  • Elements of crystallography & X-Ray Diffraction
  • Powder diffraction vs Single Crystal Diffraction
  • Specificities of organics & qualitative interpretation of their diffraction patterns
  • Structural analysis of drug substances and products
Part 2: The importance of powder sample preparation: how can it influence the output of our experiments/measurements?
  • Does a powder sample always behave as a powder?
  • The choice of the experiment configuration (transmission vs reflection)
  • The choice of the detectors: is high-resolution always the best choice?
  • How should we prepare samples? Tips
  • What if we cannot control all parameters?
Part 3: Laboratory versus synchrotron XRPD: when is lab-XRPD no longer the best choice?
  • What is a synchrotron? Why does it enable you to learn more about your sample?
  • Laboratory vs synchrotron source: are they complementary?
  • LOD & LOQ
  • Synchrotron-XRPD: measurements or experiments?
  • Synchrotron-based analytical techniques: how does a company access them?
Part 4: In practice – What does a diffraction pattern tell us at glance? What else can it tell us?
  • Indexation, Structure Solution and Refinement
  • Trace analysis & Quantitative Phase Analysis
  • Microstructure analysis of pharmaceuticals
  • Pair Distribution Function analysis of pharmaceuticals: definitions, aim of analyses, complexity
Part 5: Can XRPD analyze systems as complex as proteins?
  • The pioneer work of Robert von Dreele, Irene Margiolaki and Jonathan Wright

Upcoming Workshop Edition (SPS-XRPD-4):
10th - 11th June 2024 NOVARTIS Campus, FAB6 conference room
Fabrikstrasse 2, 4056 Basel - Switzerland