1st
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:
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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.
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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
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| 8:45 am – 10:25 am | Applications of XRPD for Phase Identification throughout Pharmaceutical Product Development
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| 10:25 am – 10:55 am | Coffee break |
| 10:55 am – 12:20 pm | Recent developments in PDF analysis of organics and pharmaceuticals
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| 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
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| 2:35 pm – 3:50 pm | Monitoring phase transformations in formulations
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| 3:50 pm – 4:20 pm | Coffee break |
| 4:20pm -6:00 pm | Structure and Analysis of Amorphous Dispersions
Polyamorphism of D-mannitol: Structural studies by Synchrotron X ray diffraction
Using Containerless Methods to Synthesize and Characterize Amorphous Pharmaceuticals
Pharmaceutical amorphous solid dispersions characterized by Synchrotron X-ray diffraction and Pair Distribution Function method
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| 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
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| 8:55 am – 9:55 am | The XPDF beamline at Diamond Light Source
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| 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
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| 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?
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| 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
Feedback
Very informative and useful to apply the information in my daily professional life’
Naveen K. Thakral, Upsher Smith Laboratories LLC
I’m very glad to attend this workshop. Excellent speakers and talks, fruitful discussions! It’s great to see some old friends and make some new. Thank you very much for organizing this wonderful workshop!
Tony Hu, NYU Department of Chemistry
An excellent mix of theory and practice and a great insight into how pharmaceutical research benefits from x-ray methods
Anonymous
I had the opportunity to interact with and listen to the experts in the field and emerging techniques in XRD and data analysis
Anonymous
The 1st SPS-XRPD workshop is a great success. The two-and-a-half workshop assembled x-ray experts from academia, industry and national labs. It is educational, informative and fun. A must-go event for all pharmaceutical scientists
Chenyang Shi, AbbVie Inc
I was pleasantly surprised that a gathering of highly qualified experts would make their presentations accessible for non-experts without compromising the depth of the subjects addressed
Arturo Araque, Excelsus Scientific Engineering
It has been an incredible experience, as a student it brings you the opportunity to meet the experts, share your work and even discuss it
Barbara Ramirez, UNAM Mexico
An excellent mix of x-ray synchrotron experts and pharma researchers
Anonymous
I was honored to join the SPS-XRPD workshop, hosted by Purdue University, Excelsus Structural Solutions, APS, and Improved Pharma. This collaborative event united industry leaders and synchrotron experts, fostering insightful discussions on Pharma R&D challenges and the benefits of Synchrotron-XRPD analysis. It's crucial for promoting awareness of synchrotron radiation's analytical prowess in pharmaceutical research. Excited for future workshops!
Gabriel L.B. Araujo, Associate Professor, School of Pharmaceutical Sciences, University of São Paulo, Brazil
