2018

1^st

Spring Pharmaceutical Synchrotron X-Ray Powder Diffraction Workshop

7^th - 8^th 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.

SCHEDULE

DAY 1 - 7^TH 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 - 8^TH 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