Spring Pharmaceutical Synchrotron X-Ray Powder Diffraction Workshop

9th - 12th May 2019

PSI Auditorium
The SPS-XRPD-2 workshop in 2019 was conducted in conjunction with the 16th Pharmaceutical Powder X-ray Diffraction (PPXRD-16) Symposium and was hosted at the Paul Scherrer Institute in Switzerland from May 9th to May 12th, 2019.
The organizing committee for this collaborative event included representatives from Excelsus Structural Solutions, Purdue University, Argonne National Laboratory, Improved Pharma, Park Innovaare, Paul Scherrer Institute, and the International Center for Diffraction Data (ICDD).

The technical program for PPXRD-16 & SPS-XRPD-2 commenced on Thursday, May 9th, featuring a half-day workshop on the advantages and disadvantages of Laboratory and Synchrotron XRPD. The program continued throughout Friday to Sunday with a series of technical sessions, concluding at 4:40 pm on Sunday, May 12th, followed by closing remarks.

The event commenced with a preliminary one-day workshop dedicated to exploring the advantages and disadvantages of Laboratory and Synchrotron XRPD.

DAY 1 - 9TH MAY 2019

8:30 am – 4:30 pm Half-day workshop on Laboratory and Synchrotron XRPD – Advantages and Disadvantages

8:30 Phil Willmott: “Synchrotron Radiation and SR based techniques”
  • General introduction to synchrotron radiation
  • Interaction of X-rays with matter, in particular at synchrotron sources
  • Overview of techniques that exploit synchrotron radiation for the characterization of matter
9:45 Coffee Break

10:00 Tom Blanton: “Laboratory X-ray Powder Diffraction and the Power of Crystallographic Database”
  • General introduction to lab-XRPD technique
  • Advantages of lab-XRPD for the pharma industry (user-friendliness, GMP certification) and limits
  • The power of crystallographic database and overview
11:00 Fabia Gozzo: “Synchrotron X-ray Powder Diffraction and Applications to Pharmaceuticals”
  • General introduction to Synchrotron-XRPD
  • Advantages and disadvantages for applications to pharmaceuticals
  • Enhanced Level of Detection (LOD) and Level of Quantification (LOQ)
11:45 Pamela Smith: “Pair Distribution Function and Applications to Pharmaceuticals”
  • General introduction to Pair Distribution Function (PDF)
  • PDF applied to pharmaceuticals
12:30 Lunch

1:30 Tour: Visit PSI Large Scale Facilities

4:30 pm – 5:00 pm Welcome to our Attendees
5:00 pm - 6:00 pm Opening Plenary: Industry Speaks to Academia
Invited presentation by Arnaud Grandeury, Novartis Pharma, Switzerland
6:00 pm - 7:30 pm Welcoming Reception
Please join us after the Plenary for light refreshments and cocktails.


DAY 2 - 10TH MAY 2019

8:30 am - 9:10 am
P25 Patenting Solid Forms: A Review of US Case Law Involving Dr. Joel Bernstein
Jill MacAlpine, Finnegan, USA
9:10 am – 9:50 am P26 Facts and Fictions about Polymorphism: Personal Recollections of our Good Friend, Joel Bernstein
Susan M. Reutzel-Edens, Eli Lilly and Company, USA
9:50 am - 10:30 am P24 Solid Form Patents in Pharmaceutical Development
Eyal Barash, Barash Law LLC, USA
10:30 am – 11:00 am Coffee break
11:00 am – 11:40 am P37 Invited – Role of Physical Form of the Active Pharmaceutical Ingredient (API) and Excipients
Raj Suryanarayanan, University of Minnesota, USA
11:40 am - 12:10 pm P5 High-Throughput Quantum Molecular Dynamics Constrained by Electron Diffraction Aimed at the Prediction of Amorphous Solid Dispersion Stability
Georgios Antipas, Molecular Modelling Laboratory (MML), Switzerland
12:10 pm – 1:15 pm Lunch
1:15 pm – 1:55 pm P11 Invited – The Direct Derivation (DD) Method for Quantitative Phase Analysis: A Practical Approach with the Direct-fitting of Observed Diffraction Patterns
Hideo Toraya, Rigaku Corporation, Japan
1:55 pm - 2:25 pm P8 Method Validation for Quantitative Determination of the (Pseudo) Polymorphs Ratio in DS and DP Samples: Performance and Compliance
Matteo Daldosso*, Silvia Lenzini, Brigida Allieri, Aptuit, an Evotec Company, Italy
Sarah Le Meur, Michel Wagneur, Luc Aerts, UCB Pharma, Belgium
2:25 pm - 2:55 pm P10 Using Portable X-ray Diffraction (XRD) with Pseudo-Thin-Film Type Analysis for API Verification and Counterfeit Formulation Investigations
Jose Brum, Olympus OSSA, USA
2:55 pm – 3:30 pm Coffee Break
3:30 pm - 4:10 pm P28 Invited – Overview of Synchrotron X-ray Powder Diffraction: Instruments and Case Studies
Peter Stephens, Stony Brook University, USA
4:10 pm - 4:30pm P36 Industrial Collaboration: How to make it happen at the Swiss Light Source?
Stefan Müller, Paul Scherrer Institut & SLS Techno Trans AG, Switzerland
4:30 pm - 5:10 pm P39 Invited – Time and Matter: The Material Science Beamline at the SLS
Nicola Casati, Paul Scherrer Institute, Switzerland
5:10 pm - 5:40 pm P35 – ID22 High Resolution Powder Diffraction Beamline at ESRF
Andy Fitch, ESRF, France
From 7:30 pm
Conference Dinner


DAY 3 - 11TH MAY 2019

9:00 am - 9:56 am
9:00 P15 Humidity Effects on Amorphous Pharmaceuticals
C.J. Benmore*, Argonne National Laboratory, USA
P. Smith, S.R. Byrn, Improved Pharma, USA
J.K.R. Weber, Argonne National Laboratory and Materials Development, Inc., USA

9:08 P18 Quantification of Multiple Amorphous and Crystalline Phases
Maria Orlova*, PANalytical B.V., Switzerland
Detlef Beckers, Thomas Degen, PANalytical B.V., The Netherlands

9:16 P22 Computed Tomography Analysis for Process Development and Quality Control of Formulations
Detlef Beckers*, Natalia Dadivanyan, Detlev J. Götz, Malvern Panalytical B.V.

9:24 P23 Atomic Pair Distribution Function (PDF) and X-ray Scattering Methods to Assess Amorphous Organic Compounds
Detlef Beckers*, Milen Gateshki, Malvern Panalytical B.V., The Netherlands

9:32 P27 Use of “Cleaning” Algorithm for Model-Free Correction of Instrumental Aberrations in XRPD Patterns
Vladimir Kogan*, Dannalab, The Netherlands
Detlef Beckers, Alexander Kharchenko, Malvern Panalytical B.V., Almelo, The Netherlands

9:40 P31 Total Pattern Analyses of Pharmaceutical Formulations
T.G. Fawcett, S. Gates-Rector, M. Rost, A.M. Gindhart, T.N. Blanton*, S.N. Kabekkodu, ICDD, USA

9:48 P34 Attempts and Approximations for a Background Modeling in Pharmaceutical Samples in Patterns of XRD and S-XRPD
Bárbara A. Ramírez Almaguer*, Lauro Bucio, Universidad Nacional Autónoma de México, México
Mathilde Reinle-Schmitt, Mickael Morin, Fabia Gozzo, Excelsus Structural Solutions, Switzerland
Antonio Cervellino, Paul Scherrer Institute, Switzerland

9:56 am – 10:30 am Coffee break
10:30 am – 11:10 am P20 Invited–Magnifying Nano-/Meso- Structural Information of Amorphous Pharmaceutical Solids through Small Angle X-Ray Scattering
Amrit Paudel*, Peter Laggner, Graz University of Technology and Research Center Pharmaceutical Engineering GmbH (RCPE), Austria
11:10 am - 11:50 pm P14 Invited–SAXS-WAXS Studies of Amorphous, Mesoporous and Nanomaterials
C.J. Benmore*, D. Robinson, G. Jennings, J. Ilavsky, S. Shastri, Argonne National Laboratory, USA
O.L.G. Alderman, A. Tamalonis, E. Clark, Materials Development Inc., USA
E. Soignard, J.L. Yarger, Arizona State University, USA
J.K.R. Weber, Argonne National Laboratory and Materials Development, Inc., USA
11:50 am - 12:30 pm P40 Invited–Understanding the Disordered State of Matter in Pharmaceutical Development
Vishal Koradia, Novartis Pharma AG, Switzerland
12:30 pm – 2:00 pm Lunch
2:00 pm – 2:40 pm P33 Invited–Macromolecular Powder Diffraction: Ready for Genuine Biological Problems
Irene Margiolaki, University of Patras, Greece
2:40 pm - 3:10 pm P13 Characterizing Proteins Using XRPD and SAXS Techniques on a Laboratory Diffractometer
N. Dadivanyan*, J. Bolze, D. Beckers, G. Nénert, T. Degen, Malvern Panalytical B.V., The Netherlands
S. Trampari, Kapodistrian University of Athens, Greece
S. Logotheti, A. Valmas, S. Saslis, F. Karavassili, I. Margiolaki, University of Patras, Greece
3:10 pm – 3:30 pm Coffee Break
3:30 pm - 5:30 pm Guidelines Discussion


DAY 4 - 12TH MAY 2019

8:30 am - 9:10 am
P29 Invited- How Many Ritonavir Cases are Still Out There?
Marcus A. Neumann*, Jacco van de Streek, Hanno Dietrich, Kiran Sasikumar, Asbjörn Burow, Avant-garde Materials Simulation Deutschland GmbH, Germany
9:10 am – 9:40 am P9 ICDD® Polymer Diffraction Data Project – 100+ PDF® Entries and Growing
Tom Blanton, Megan Rost, Stacy Gates-Rector, ICDD, USA
9:40 am – 10:10 am Coffee Break
10:10 am - 10:50 pm P7 Invited – Crystal Structures of Large-Volume Commercial Pharmaceuticals
Jim Kaduk, North Central College, Illinois Institute of Tech. and Poly Crystallography Inc., USA
10:50 am - 11:30 am P32 Invited – Structure Determination of Organic Materials from Powder X-ray Diffraction Data: Opportunities for Multi-technique Synergy
Kenneth Harris, Cardiff University, United Kingdom
11:30 am - 12:10 pm P30 Invited – Walking the Tightrope of Complexity – Assessing Probability of Success of Structure Solution from Powder Diffraction Data
Pamela Whitfield*, Michael Morin, Mathilde Reinle-Schmitt, Fabia Gozzo, Excelsus Structural Solutions, Switzerland and Belgium
12:10 pm - 12:40 pm P19 Structure Determination of Nanocrystalline Organic Compounds from Unindexed Powder Data by Real-Space and PDF methods
Martin U. Schmidt*, Stefan Habermehl, Carina Schlesinger, Dragica Prill, Goethe University, Germany
12:40 pm – 2:00 pm Lunch
2:00 pm – 2:40 pm P17 Invited – Micro to Nanometer Scale Characterization of Pharmaceutical Compounds by Electron Microscopy
Partha Pratim Das*, Alejandro Gómez Pérez, Stavros Nicolopoulos, NanoMEGAS SPRL, Belgium
2:40 pm - 3:10 pm P6 Extensive Polymorph Screening of the Nucleobase Adenine
Dubravka Sisak Jung*, DECTRIS, Switzerland
Ivan Halasz, Institute Rudjer Boskovic, Croatia
Graeme Day, David McDonagh, University of Southampton, UK
3:10 pm - 3:40 pm P21 Study Real Time Crystallization Process in Organic Crystals using Liquid Cell Transmission Electron Microscopy and Electron Crystallography Techniques on PDIs
Alejandro Gomez-Perez*, Partha Pratim Das, Stavros Nicolopoulos, NanoMEGAS, Belgium
Yael Tsarfati, Boris Rybtchinski, Weizmann Institute of Science, Israel
3:40 pm - 4:10 pm P38 Non-Standard Crystallization Methods of API´s & Electron Diffraction: The Future
Gustavo Santiso-Quiñones, Crystallise! AG, Switzerland
4:10 pm - 4:30 pm Closing Remarks

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